+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 15:56:51 on 09-May-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL DIRDIF output for 02SRC222 CELL 0.71073 9.3727 19.1440 20.2492 90.000 101.414 90.000 ZERR 8.00 0.0009 0.0015 0.0019 0.000 0.000 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O F PD UNIT 120 160 16 24 24 8 V = 3561.48 F(000) = 1768.0 Mu = 1.09 mm-1 Cell Wt = 3517.84 Rho = 1.640 MERG 2 OMIT -3.00 55.00 OMIT 1 8 5 OMIT -2 0 16 OMIT 4 2 12 EXTI 0.00025 ISOR 0.0001 $C $N $O FMAP 2 PLAN 10 SIZE 0.00 0.01 0.32 ACTA BOND $H WGHT 0.00000 44.84380 L.S. 4 TEMP -153.00 FVAR 0.08945 C1 1 0.181827 0.259046 0.331492 11.00000 0.01186 0.01191 = 0.01212 0.00002 0.00230 0.00005 AFIX 23 H1A 2 0.274794 0.233428 0.335055 11.00000 -1.20000 H1B 2 0.104164 0.224347 0.332893 11.00000 -1.20000 AFIX 0 C2 1 0.192836 0.307783 0.390588 11.00000 0.01639 0.01637 = 0.01629 0.00003 0.00311 0.00025 AFIX 23 H2A 2 0.218618 0.280919 0.433055 11.00000 -1.20000 H2B 2 0.270757 0.342464 0.389641 11.00000 -1.20000 AFIX 0 C3 1 0.024658 0.384185 0.326384 11.00000 0.01856 0.01842 = 0.01865 -0.00001 0.00354 -0.00004 AFIX 23 H3A 2 0.103146 0.418813 0.326475 11.00000 -1.20000 H3B 2 -0.067812 0.409935 0.324032 11.00000 -1.20000 AFIX 0 C4 1 0.012632 0.337102 0.264992 11.00000 0.01656 0.01647 = 0.01649 0.00003 0.00326 0.00007 AFIX 23 H4A 2 -0.069468 0.304251 0.263648 11.00000 -1.20000 H4B 2 -0.008364 0.365982 0.223647 11.00000 -1.20000 AFIX 0 C5 1 0.017327 0.118675 0.257813 11.00000 0.02201 0.02210 = 0.02222 0.00002 0.00425 -0.00007 C6 1 0.025803 0.048037 0.291793 11.00000 0.03368 0.03368 = 0.03384 0.00010 0.00675 0.00004 C7 1 0.233764 0.158522 0.073983 11.00000 0.02747 0.02771 = 0.02759 -0.00023 0.00559 -0.00005 AFIX 137 H7A 2 0.217668 0.134201 0.030553 11.00000 -1.50000 H7B 2 0.290481 0.128580 0.108822 11.00000 -1.50000 H7C 2 0.287176 0.201990 0.070744 11.00000 -1.50000 AFIX 0 C8 1 0.013190 0.106261 0.094374 11.00000 0.03577 0.03588 = 0.03584 -0.00001 0.00725 0.00011 AFIX 137 H8A 2 -0.074646 0.113663 0.112881 11.00000 -1.50000 H8B 2 0.077788 0.073408 0.123063 11.00000 -1.50000 H8C 2 -0.014002 0.087080 0.048741 11.00000 -1.50000 AFIX 0 C9 1 0.005329 0.221494 0.040454 11.00000 0.02266 0.02321 = 0.02284 -0.00012 0.00460 -0.00009 AFIX 23 H9A 2 0.013422 0.205137 -0.005040 11.00000 -1.20000 H9B 2 -0.098581 0.219817 0.043786 11.00000 -1.20000 AFIX 0 C10 1 0.057698 0.292386 0.049944 11.00000 0.01607 0.01629 = 0.01632 -0.00006 0.00368 0.00022 C11 1 0.051240 0.342217 -0.000453 11.00000 0.02161 0.02180 = 0.02149 -0.00007 0.00428 -0.00003 AFIX 43 H11 2 0.015307 0.329368 -0.046026 11.00000 -1.20000 AFIX 0 C12 1 0.094950 0.408299 0.014144 11.00000 0.02316 0.02325 = 0.02302 0.00014 0.00469 0.00025 AFIX 43 H12 2 0.086971 0.441693 -0.021101 11.00000 -1.20000 AFIX 0 C13 1 0.152433 0.428743 0.080976 11.00000 0.02080 0.02089 = 0.02090 -0.00011 0.00408 0.00012 AFIX 43 H13 2 0.181712 0.475711 0.090927 11.00000 -1.20000 AFIX 0 C14 1 0.165714 0.379581 0.131927 11.00000 0.01928 0.01934 = 0.01922 0.00006 0.00399 0.00007 AFIX 43 H14 2 0.207815 0.392348 0.176899 11.00000 -1.20000 AFIX 0 C15 1 0.117351 0.311195 0.117394 11.00000 0.00928 0.00951 = 0.00956 -0.00009 0.00213 0.00002 C16 1 -0.310757 0.256574 -0.167862 11.00000 0.01372 0.01363 = 0.01363 0.00002 0.00255 -0.00008 AFIX 23 H16A 2 -0.213312 0.234687 -0.161659 11.00000 -1.20000 H16B 2 -0.379082 0.221850 -0.155369 11.00000 -1.20000 AFIX 0 C17 1 -0.303938 0.319488 -0.122786 11.00000 0.02314 0.02326 = 0.02325 -0.00004 0.00458 -0.00007 AFIX 23 H17A 2 -0.269181 0.305018 -0.075393 11.00000 -1.20000 H17B 2 -0.233212 0.353437 -0.134485 11.00000 -1.20000 AFIX 0 C18 1 -0.491099 0.374378 -0.198330 11.00000 0.03083 0.03093 = 0.03076 0.00005 0.00605 0.00011 AFIX 23 H18A 2 -0.421178 0.409000 -0.209601 11.00000 -1.20000 H18B 2 -0.587302 0.397384 -0.203665 11.00000 -1.20000 AFIX 0 C19 1 -0.501905 0.313960 -0.246446 11.00000 0.01891 0.01894 = 0.01884 -0.00001 0.00378 0.00006 AFIX 23 H19A 2 -0.576929 0.280869 -0.237416 11.00000 -1.20000 H19B 2 -0.532438 0.331261 -0.293184 11.00000 -1.20000 AFIX 0 C20 1 -0.452969 0.098747 -0.206873 11.00000 0.01513 0.01513 = 0.01527 0.00006 0.00279 -0.00012 C21 1 -0.420951 0.033049 -0.161598 11.00000 0.03172 0.03155 = 0.03184 0.00005 0.00615 0.00000 C22 1 -0.248566 0.109622 -0.403920 11.00000 0.02208 0.02203 = 0.02208 -0.00002 0.00440 0.00007 AFIX 137 H22A 2 -0.257055 0.077100 -0.441873 11.00000 -1.50000 H22B 2 -0.181155 0.090440 -0.364913 11.00000 -1.50000 H22C 2 -0.211623 0.154602 -0.416441 11.00000 -1.50000 AFIX 0 C23 1 -0.449720 0.051272 -0.370908 11.00000 0.02502 0.02502 = 0.02496 -0.00013 0.00502 0.00012 AFIX 137 H23A 2 -0.544697 0.056925 -0.358236 11.00000 -1.50000 H23B 2 -0.381210 0.030001 -0.333461 11.00000 -1.50000 H23C 2 -0.460007 0.021082 -0.410656 11.00000 -1.50000 AFIX 0 C24 1 -0.492081 0.151628 -0.445112 11.00000 0.01741 0.01769 = 0.01753 0.00005 0.00347 -0.00006 AFIX 23 H24A 2 -0.479815 0.127639 -0.486941 11.00000 -1.20000 H24B 2 -0.594716 0.146353 -0.440479 11.00000 -1.20000 AFIX 0 C25 1 -0.456340 0.226338 -0.448933 11.00000 0.01713 0.01741 = 0.01745 -0.00021 0.00360 -0.00002 C26 1 -0.476334 0.264149 -0.508537 11.00000 0.02140 0.02172 = 0.02155 -0.00018 0.00432 -0.00002 AFIX 43 H26 2 -0.512563 0.241644 -0.550303 11.00000 -1.20000 AFIX 0 C27 1 -0.443919 0.333632 -0.507079 11.00000 0.01981 0.01997 = 0.01964 0.00037 0.00407 0.00013 AFIX 43 H27 2 -0.459641 0.358926 -0.548247 11.00000 -1.20000 AFIX 0 C28 1 -0.388966 0.368507 -0.447741 11.00000 0.02284 0.02274 = 0.02325 0.00007 0.00461 -0.00008 AFIX 43 H28 2 -0.368552 0.417129 -0.447355 11.00000 -1.20000 AFIX 0 C29 1 -0.364630 0.329318 -0.388291 11.00000 0.01604 0.01633 = 0.01602 -0.00022 0.00325 0.00000 AFIX 43 H29 2 -0.324217 0.351788 -0.346992 11.00000 -1.20000 AFIX 0 C30 1 -0.397125 0.259642 -0.387647 11.00000 0.01360 0.01367 = 0.01348 0.00012 0.00279 -0.00005 N1 3 0.149260 0.296630 0.266223 11.00000 0.00988 0.00949 = 0.00927 -0.00033 0.00181 0.00013 N2 3 0.090788 0.174935 0.091969 11.00000 0.01661 0.01669 = 0.01640 -0.00030 0.00348 0.00010 N3 3 -0.359904 0.276883 -0.239612 11.00000 0.01747 0.01760 = 0.01716 -0.00008 0.00337 0.00060 N4 3 -0.394677 0.119872 -0.386440 11.00000 0.01297 0.01286 = 0.01270 0.00018 0.00251 0.00006 O1 4 0.056031 0.343511 0.388372 11.00000 0.02174 0.02230 = 0.02180 0.00018 0.00458 0.00029 O2 4 0.131490 0.135838 0.239878 11.00000 0.01770 0.01774 = 0.01810 0.00059 0.00381 -0.00028 O3 4 -0.097647 0.152926 0.252942 11.00000 0.03139 0.03182 = 0.03197 -0.00021 0.00652 0.00015 O4 4 -0.444453 0.352749 -0.129261 11.00000 0.02452 0.02489 = 0.02460 -0.00004 0.00498 0.00028 O5 4 -0.350189 0.114866 -0.233641 11.00000 0.01902 0.01855 = 0.01885 0.00033 0.00418 -0.00013 O6 4 -0.573911 0.124389 -0.210101 11.00000 0.02935 0.02998 = 0.02975 0.00036 0.00624 0.00027 F1 5 0.068292 0.054261 0.355719 11.00000 0.25588 0.04176 = 0.01756 0.01883 0.02143 0.03249 F2 5 -0.107405 0.019769 0.282722 11.00000 0.07799 0.04097 = 0.16834 0.01580 0.07085 -0.00656 F3 5 0.106184 0.002654 0.268625 11.00000 0.05138 0.03632 = 0.04297 -0.00026 0.01548 0.01271 F4 5 -0.525582 0.014917 -0.131973 11.00000 0.07490 0.08474 = 0.13399 0.06599 0.06400 0.01918 F5 5 -0.309718 0.045404 -0.109683 11.00000 0.10220 0.04986 = 0.03610 0.01926 -0.00460 0.00705 F6 5 -0.377891 -0.021164 -0.191058 11.00000 0.12301 0.01364 = 0.05357 0.00235 0.02853 0.01991 PD1 6 0.123240 0.231361 0.181173 11.00000 0.01372 0.02325 = 0.01189 -0.00320 0.00391 -0.00043 PD2 6 -0.376050 0.194423 -0.309648 11.00000 0.01424 0.02346 = 0.01414 0.00233 0.00344 0.00058 HKLF 4 1.0 -1.00 0.00 0.00 0.00 -1.00 0.00 0.00 0.00 1.00 Covalent radii and connectivity table for DIRDIF output for 02SRC222 C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 PD 1.380 C1 - N1 C2 C2 - O1 C1 C3 - O1 C4 C4 - N1 C3 C5 - O2 O3 C6 C6 - F1 F3 F2 C5 C7 - N2 C8 - N2 C9 - C10 N2 C10 - C11 C15 C9 C11 - C12 C10 C12 - C11 C13 C13 - C14 C12 C14 - C13 C15 C15 - C14 C10 Pd1 C16 - N3 C17 C17 - O4 C16 C18 - O4 C19 C19 - N3 C18 C20 - O6 O5 C21 C21 - F4 F6 F5 C20 C22 - N4 C23 - N4 C24 - C25 N4 C25 - C26 C30 C24 C26 - C27 C25 C27 - C26 C28 C28 - C27 C29 C29 - C30 C28 C30 - C29 C25 Pd2 N1 - C1 C4 Pd1 N2 - C9 C7 C8 Pd1 N3 - C16 C19 Pd2 N4 - C23 C24 C22 Pd2 O1 - C2 C3 O2 - C5 Pd1 O3 - C5 O4 - C18 C17 O5 - C20 Pd2 O6 - C20 F1 - C6 F2 - C6 F3 - C6 F4 - C21 F5 - C21 F6 - C21 Pd1 - C15 N2 N1 O2 Pd2 - C30 N4 N3 O5 h k l Fo^2 Sigma Why rejected -1 0 3 4.32 1.08 observed but should be systematically absent 0 3 0 9.72 2.16 observed but should be systematically absent 0 3 0 6.48 1.08 observed but should be systematically absent 0 3 0 5.40 1.08 observed but should be systematically absent 0 3 0 9.72 2.16 observed but should be systematically absent 1 0 3 8.63 1.08 observed but should be systematically absent 2 0 3 4.33 1.08 observed but should be systematically absent 2 0 1 4.33 1.08 observed but should be systematically absent -2 0 3 4.32 1.08 observed but should be systematically absent 4 0 1 11.89 2.16 observed but should be systematically absent -4 0 3 7.58 1.08 observed but should be systematically absent -5 0 7 8.69 1.09 observed but should be systematically absent 9938 Reflections read, of which 295 rejected -9 =< h =< 9, -17 =< k =< 17, -18 =< l =< 18, Max. 2-theta = 46.07 12 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 6 2 0 6.04 0.63 4 8.46 8 2 0 120.95 4.70 2 36.62 6 1 1 8.61 0.69 5 3.58 -1 2 1 63.44 1.52 5 10.18 -6 3 1 5.77 1.08 2 5.95 -4 3 1 7.13 0.62 3 3.71 6 6 1 2.07 0.71 4 3.61 -5 1 3 60.63 1.58 3 14.62 7 1 3 4.86 0.96 2 5.35 -4 2 3 10.02 0.72 3 3.89 -6 3 3 6.95 0.76 3 10.83 -6 1 6 64.94 2.23 3 12.11 -4 6 14 13.33 2.14 2 26.39 -8 4 15 5.89 3.27 2 119.74 -8 3 16 22.33 5.42 2 134.14 15 Inconsistent equivalents 2323 Unique reflections, of which 0 suppressed R(int) = 0.0537 R(sigma) = 0.0509 Friedel opposites merged Maximum memory for data reduction = 4284 / 24640 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 = 5529 / 569692 wR2 = 0.1148 before cycle 1 for 2323 data and 438 / 438 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 240. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.285; Restrained GooF = 1.211 for 240 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 44.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08943 0.00027 -0.064 OSF 2 0.00024 0.00008 -0.152 EXTI Mean shift/esd = 0.063 Maximum = -0.288 for z O4 Max. shift = 0.013 A for H7A Max. dU =-0.001 for C29 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5529 / 569692 wR2 = 0.1147 before cycle 2 for 2323 data and 438 / 438 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 240. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.284; Restrained GooF = 1.210 for 240 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 44.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08942 0.00027 -0.039 OSF 2 0.00023 0.00008 -0.068 EXTI Mean shift/esd = 0.028 Maximum = -0.119 for U33 C29 Max. shift = 0.004 A for H22A Max. dU = 0.000 for C29 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5529 / 569692 wR2 = 0.1147 before cycle 3 for 2323 data and 438 / 438 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 240. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.284; Restrained GooF = 1.210 for 240 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 44.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08942 0.00027 -0.006 OSF 2 0.00023 0.00008 -0.008 EXTI Mean shift/esd = 0.004 Maximum = -0.023 for y C27 Max. shift = 0.001 A for H22A Max. dU = 0.000 for C29 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5529 / 569692 wR2 = 0.1147 before cycle 4 for 2323 data and 438 / 438 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 240. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.283; Restrained GooF = 1.210 for 240 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 44.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08942 0.00027 -0.001 OSF 2 0.00023 0.00008 -0.001 EXTI Mean shift/esd = 0.001 Maximum = 0.007 for y C14 Max. shift = 0.000 A for H22B Max. dU = 0.000 for C29 Largest correlation matrix elements 0.940 U33 C21 / U22 C21 0.938 U33 C8 / U11 C8 0.928 U22 C28 / U11 C28 0.940 U22 C21 / U11 C21 0.936 U33 C18 / U22 C18 0.928 U33 C28 / U11 C28 0.940 U33 C21 / U11 C21 0.936 U22 C18 / U11 C18 0.927 U33 C23 / U22 C23 0.939 U33 C6 / U22 C6 0.936 U33 C18 / U11 C18 0.927 U22 C23 / U11 C23 0.939 U33 C8 / U22 C8 0.929 U33 C7 / U22 C7 0.927 U33 C23 / U11 C23 0.938 U22 C6 / U11 C6 0.929 U22 C7 / U11 C7 0.926 U33 C13 / U22 C13 0.938 U22 C8 / U11 C8 0.929 U33 C7 / U11 C7 0.925 U33 C12 / U22 C12 0.938 U33 C6 / U11 C6 0.928 U33 C28 / U22 C28 0.925 U22 C13 / U11 C13 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.2748 0.2333 0.3350 23 0.990 0.000 C1 N1 C2 H1B 0.1042 0.2242 0.3328 23 0.990 0.000 C1 N1 C2 H2A 0.2187 0.2808 0.4330 23 0.990 0.000 C2 O1 C1 H2B 0.2708 0.3423 0.3895 23 0.990 0.000 C2 O1 C1 H3A 0.1030 0.4187 0.3266 23 0.990 0.000 C3 O1 C4 H3B -0.0679 0.4098 0.3241 23 0.990 0.000 C3 O1 C4 H4A -0.0693 0.3041 0.2638 23 0.990 0.000 C4 N1 C3 H4B -0.0086 0.3659 0.2238 23 0.990 0.000 C4 N1 C3 H7A 0.2173 0.1349 0.0301 137 0.980 0.000 C7 N2 H7A H7B 0.2900 0.1280 0.1082 137 0.980 0.000 C7 N2 H7A H7C 0.2877 0.2020 0.0712 137 0.980 0.000 C7 N2 H7A H8A -0.0745 0.1137 0.1130 137 0.980 0.000 C8 N2 H8A H8B 0.0780 0.0735 0.1231 137 0.980 0.000 C8 N2 H8A H8C -0.0140 0.0872 0.0488 137 0.980 0.000 C8 N2 H8A H9A 0.0134 0.2051 -0.0051 23 0.990 0.000 C9 C10 N2 H9B -0.0987 0.2199 0.0436 23 0.990 0.000 C9 C10 N2 H11 0.0151 0.3293 -0.0463 43 0.950 0.000 C11 C12 C10 H12 0.0869 0.4417 -0.0210 43 0.950 0.000 C12 C11 C13 H13 0.1816 0.4758 0.0908 43 0.950 0.000 C13 C14 C12 H14 0.2083 0.3921 0.1768 43 0.950 0.000 C14 C13 C15 H16A -0.2132 0.2347 -0.1618 23 0.990 0.000 C16 N3 C17 H16B -0.3789 0.2217 -0.1555 23 0.990 0.000 C16 N3 C17 H17A -0.2693 0.3049 -0.0755 23 0.990 0.000 C17 O4 C16 H17B -0.2332 0.3533 -0.1346 23 0.990 0.000 C17 O4 C16 H18A -0.4211 0.4089 -0.2098 23 0.990 0.000 C18 O4 C19 H18B -0.5873 0.3974 -0.2039 23 0.990 0.000 C18 O4 C19 H19A -0.5767 0.2807 -0.2371 23 0.990 0.000 C19 N3 C18 H19B -0.5330 0.3309 -0.2932 23 0.990 0.000 C19 N3 C18 H22A -0.2566 0.0765 -0.4415 137 0.980 0.000 C22 N4 H22A H22B -0.1809 0.0909 -0.3647 137 0.980 0.000 C22 N4 H22A H22C -0.2120 0.1544 -0.4169 137 0.980 0.000 C22 N4 H22A H23A -0.5447 0.0572 -0.3582 137 0.980 0.000 C23 N4 H23A H23B -0.3813 0.0301 -0.3335 137 0.980 0.000 C23 N4 H23A H23C -0.4605 0.0212 -0.4107 137 0.980 0.000 C23 N4 H23A H24A -0.4798 0.1277 -0.4870 23 0.990 0.000 C24 C25 N4 H24B -0.5946 0.1465 -0.4405 23 0.990 0.000 C24 C25 N4 H26 -0.5124 0.2414 -0.5503 43 0.950 0.000 C26 C27 C25 H27 -0.4597 0.3587 -0.5485 43 0.950 0.000 C27 C26 C28 H28 -0.3686 0.4172 -0.4475 43 0.950 0.000 C28 C27 C29 H29 -0.3243 0.3519 -0.3470 43 0.950 0.000 C29 C30 C28 DIRDIF output for 02SRC222 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.18187 0.25889 0.33143 1.00000 0.01279 0.01285 0.01311 0.00003 0.00249 0.00006 0.01292 0.02224 0.00131 0.00064 0.00057 0.00000 0.00345 0.00348 0.00348 0.00104 0.00121 0.00103 0.00336 H1A 0.27484 0.23328 0.33499 1.00000 0.01551 0.00000 0.00000 H1B 0.10420 0.22419 0.33282 1.00000 0.01551 0.00000 0.00000 C2 0.19285 0.30763 0.39049 1.00000 0.01696 0.01692 0.01690 0.00001 0.00321 0.00025 0.01694 0.02277 0.00127 0.00067 0.00062 0.00000 0.00362 0.00364 0.00364 0.00104 0.00123 0.00103 0.00353 H2A 0.21866 0.28076 0.43295 1.00000 0.02033 0.00000 0.00000 H2B 0.27082 0.34228 0.38953 1.00000 0.02033 0.00000 0.00000 C3 0.02460 0.38407 0.32648 1.00000 0.01921 0.01909 0.01930 -0.00003 0.00367 -0.00005 0.01922 0.02298 0.00135 0.00067 0.00060 0.00000 0.00367 0.00370 0.00370 0.00104 0.00123 0.00103 0.00359 H3A 0.10303 0.41872 0.32656 1.00000 0.02306 0.00000 0.00000 H3B -0.06791 0.40979 0.32410 1.00000 0.02306 0.00000 0.00000 C4 0.01267 0.33702 0.26514 1.00000 0.01718 0.01711 0.01712 0.00002 0.00341 0.00009 0.01713 0.02286 0.00128 0.00066 0.00062 0.00000 0.00357 0.00359 0.00359 0.00104 0.00123 0.00103 0.00348 H4A -0.06932 0.30412 0.26384 1.00000 0.02056 0.00000 0.00000 H4B -0.00857 0.36591 0.22380 1.00000 0.02056 0.00000 0.00000 C5 0.01726 0.11887 0.25783 1.00000 0.02252 0.02261 0.02276 0.00003 0.00435 -0.00008 0.02265 0.02408 0.00146 0.00070 0.00065 0.00000 0.00372 0.00374 0.00373 0.00104 0.00124 0.00104 0.00363 C6 0.02564 0.04806 0.29164 1.00000 0.03277 0.03274 0.03287 0.00011 0.00657 0.00006 0.03278 0.03124 0.00173 0.00085 0.00084 0.00000 0.00419 0.00422 0.00421 0.00104 0.00130 0.00104 0.00412 C7 0.23369 0.15855 0.07383 1.00000 0.02763 0.02789 0.02773 -0.00021 0.00563 -0.00006 0.02773 0.02457 0.00131 0.00070 0.00066 0.00000 0.00389 0.00391 0.00391 0.00104 0.00126 0.00104 0.00381 H7A 0.21733 0.13489 0.03006 1.00000 0.04159 0.00000 0.00000 H7B 0.28997 0.12801 0.10825 1.00000 0.04159 0.00000 0.00000 H7C 0.28769 0.20197 0.07122 1.00000 0.04159 0.00000 0.00000 C8 0.01330 0.10633 0.09445 1.00000 0.03542 0.03553 0.03544 -0.00003 0.00719 0.00010 0.03544 0.02511 0.00146 0.00070 0.00070 0.00000 0.00419 0.00421 0.00420 0.00104 0.00130 0.00104 0.00411 H8A -0.07447 0.11369 0.11302 1.00000 0.05316 0.00000 0.00000 H8B 0.07800 0.07348 0.12308 1.00000 0.05316 0.00000 0.00000 H8C -0.01401 0.08717 0.04881 1.00000 0.05316 0.00000 0.00000 C9 0.00523 0.22155 0.04031 1.00000 0.02324 0.02357 0.02316 -0.00012 0.00469 -0.00008 0.02331 0.02351 0.00138 0.00064 0.00065 0.00000 0.00375 0.00378 0.00377 0.00104 0.00125 0.00104 0.00367 H9A 0.01338 0.20511 -0.00515 1.00000 0.02797 0.00000 0.00000 H9B -0.09871 0.21995 0.04361 1.00000 0.02797 0.00000 0.00000 C10 0.05775 0.29232 0.04975 1.00000 0.01544 0.01566 0.01570 -0.00008 0.00355 0.00021 0.01554 0.02315 0.00129 0.00065 0.00065 0.00000 0.00358 0.00361 0.00360 0.00104 0.00123 0.00103 0.00349 C11 0.05103 0.34210 -0.00072 1.00000 0.02179 0.02198 0.02169 -0.00008 0.00430 -0.00002 0.02182 0.02489 0.00129 0.00068 0.00069 0.00000 0.00373 0.00376 0.00376 0.00104 0.00124 0.00103 0.00365 H11 0.01507 0.32933 -0.04631 1.00000 0.02619 0.00000 0.00000 C12 0.09490 0.40823 0.01422 1.00000 0.02302 0.02310 0.02289 0.00015 0.00464 0.00026 0.02299 0.02368 0.00129 0.00070 0.00067 0.00000 0.00378 0.00381 0.00380 0.00104 0.00125 0.00103 0.00370 H12 0.08687 0.44168 -0.02098 1.00000 0.02759 0.00000 0.00000 C13 0.15241 0.42881 0.08091 1.00000 0.02124 0.02141 0.02138 -0.00008 0.00415 0.00013 0.02135 0.02394 0.00127 0.00072 0.00063 0.00000 0.00379 0.00382 0.00381 0.00104 0.00125 0.00103 0.00371 H13 0.18156 0.47580 0.09085 1.00000 0.02562 0.00000 0.00000 C14 0.16585 0.37949 0.13185 1.00000 0.01965 0.01970 0.01959 0.00008 0.00406 0.00006 0.01962 0.02411 0.00126 0.00066 0.00068 0.00000 0.00368 0.00370 0.00370 0.00104 0.00124 0.00103 0.00359 H14 0.20826 0.39214 0.17682 1.00000 0.02355 0.00000 0.00000 C15 0.11724 0.31133 0.11724 1.00000 0.00895 0.00918 0.00936 -0.00010 0.00213 0.00003 0.00912 0.02210 0.00121 0.00063 0.00059 0.00000 0.00331 0.00333 0.00333 0.00104 0.00120 0.00103 0.00321 C16 -0.31068 0.25647 -0.16797 1.00000 0.01468 0.01457 0.01463 0.00002 0.00272 -0.00006 0.01465 0.02217 0.00131 0.00064 0.00057 0.00000 0.00350 0.00353 0.00352 0.00104 0.00122 0.00103 0.00341 H16A -0.21318 0.23466 -0.16181 1.00000 0.01758 0.00000 0.00000 H16B -0.37889 0.22170 -0.15545 1.00000 0.01758 0.00000 0.00000 C17 -0.30401 0.31940 -0.12295 1.00000 0.02315 0.02332 0.02325 -0.00007 0.00460 -0.00007 0.02324 0.02365 0.00133 0.00067 0.00066 0.00000 0.00378 0.00381 0.00380 0.00104 0.00125 0.00103 0.00369 H17A -0.26930 0.30495 -0.07554 1.00000 0.02789 0.00000 0.00000 H17B -0.23324 0.35333 -0.13463 1.00000 0.02789 0.00000 0.00000 C18 -0.49114 0.37435 -0.19848 1.00000 0.03098 0.03108 0.03091 0.00003 0.00607 0.00010 0.03100 0.02475 0.00145 0.00072 0.00064 0.00000 0.00410 0.00412 0.00411 0.00104 0.00129 0.00104 0.00402 H18A -0.42112 0.40889 -0.20981 1.00000 0.03720 0.00000 0.00000 H18B -0.58729 0.39741 -0.20386 1.00000 0.03720 0.00000 0.00000 C19 -0.50201 0.31380 -0.24638 1.00000 0.01939 0.01942 0.01936 -0.00002 0.00386 0.00007 0.01939 0.02325 0.00131 0.00065 0.00065 0.00000 0.00363 0.00366 0.00365 0.00104 0.00123 0.00103 0.00354 H19A -0.57673 0.28068 -0.23710 1.00000 0.02326 0.00000 0.00000 H19B -0.53303 0.33093 -0.29316 1.00000 0.02326 0.00000 0.00000 C20 -0.45280 0.09873 -0.20686 1.00000 0.01471 0.01472 0.01482 0.00004 0.00271 -0.00013 0.01478 0.02238 0.00139 0.00064 0.00060 0.00000 0.00352 0.00355 0.00354 0.00104 0.00122 0.00103 0.00343 C21 -0.42083 0.03307 -0.16130 1.00000 0.03246 0.03232 0.03259 0.00004 0.00634 0.00001 0.03247 0.03078 0.00171 0.00086 0.00081 0.00000 0.00424 0.00426 0.00426 0.00104 0.00131 0.00104 0.00417 C22 -0.24848 0.10953 -0.40389 1.00000 0.02229 0.02223 0.02234 -0.00003 0.00443 0.00007 0.02228 0.02318 0.00125 0.00068 0.00063 0.00000 0.00370 0.00372 0.00371 0.00104 0.00124 0.00103 0.00361 H22A -0.25662 0.07655 -0.44147 1.00000 0.03343 0.00000 0.00000 H22B -0.18086 0.09091 -0.36467 1.00000 0.03343 0.00000 0.00000 H22C -0.21203 0.15441 -0.41693 1.00000 0.03343 0.00000 0.00000 C23 -0.44987 0.05145 -0.37094 1.00000 0.02583 0.02585 0.02581 -0.00011 0.00517 0.00012 0.02582 0.02391 0.00137 0.00065 0.00066 0.00000 0.00384 0.00386 0.00385 0.00104 0.00126 0.00104 0.00375 H23A -0.54470 0.05725 -0.35815 1.00000 0.03873 0.00000 0.00000 H23B -0.38132 0.03012 -0.33354 1.00000 0.03873 0.00000 0.00000 H23C -0.46053 0.02123 -0.41068 1.00000 0.03873 0.00000 0.00000 C24 -0.49195 0.15169 -0.44516 1.00000 0.01733 0.01762 0.01747 0.00004 0.00343 -0.00005 0.01747 0.02259 0.00129 0.00062 0.00062 0.00000 0.00354 0.00357 0.00356 0.00104 0.00122 0.00103 0.00345 H24A -0.47980 0.12768 -0.48699 1.00000 0.02097 0.00000 0.00000 H24B -0.59458 0.14646 -0.44051 1.00000 0.02097 0.00000 0.00000 C25 -0.45628 0.22639 -0.44911 1.00000 0.01746 0.01776 0.01777 -0.00023 0.00367 -0.00003 0.01764 0.02399 0.00131 0.00067 0.00068 0.00000 0.00359 0.00362 0.00362 0.00104 0.00123 0.00103 0.00351 C26 -0.47623 0.26402 -0.50860 1.00000 0.02172 0.02203 0.02188 -0.00015 0.00439 -0.00001 0.02186 0.02524 0.00131 0.00068 0.00070 0.00000 0.00375 0.00378 0.00377 0.00104 0.00125 0.00103 0.00366 H26 -0.51240 0.24143 -0.55033 1.00000 0.02624 0.00000 0.00000 C27 -0.44397 0.33352 -0.50732 1.00000 0.01956 0.01971 0.01939 0.00036 0.00401 0.00014 0.01953 0.02398 0.00127 0.00067 0.00068 0.00000 0.00364 0.00367 0.00366 0.00104 0.00123 0.00103 0.00355 H27 -0.45971 0.35874 -0.54853 1.00000 0.02343 0.00000 0.00000 C28 -0.38894 0.36859 -0.44783 1.00000 0.02240 0.02231 0.02279 0.00006 0.00454 -0.00008 0.02249 0.02423 0.00126 0.00073 0.00063 0.00000 0.00386 0.00389 0.00389 0.00104 0.00126 0.00103 0.00378 H28 -0.36858 0.41721 -0.44749 1.00000 0.02699 0.00000 0.00000 C29 -0.36458 0.32940 -0.38827 1.00000 0.01468 0.01499 0.01460 -0.00024 0.00299 0.00001 0.01474 0.02336 0.00123 0.00063 0.00064 0.00000 0.00354 0.00358 0.00357 0.00104 0.00122 0.00103 0.00346 H29 -0.32426 0.35187 -0.34696 1.00000 0.01769 0.00000 0.00000 C30 -0.39719 0.25950 -0.38773 1.00000 0.01316 0.01323 0.01299 0.00011 0.00273 -0.00004 0.01311 0.02318 0.00125 0.00064 0.00062 0.00000 0.00348 0.00351 0.00350 0.00104 0.00122 0.00103 0.00339 N1 0.14928 0.29659 0.26615 1.00000 0.01026 0.00985 0.00972 -0.00033 0.00185 0.00015 0.00996 0.01708 0.00098 0.00048 0.00047 0.00000 0.00279 0.00282 0.00281 0.00103 0.00113 0.00102 0.00267 N2 0.09072 0.17497 0.09203 1.00000 0.01645 0.01651 0.01620 -0.00028 0.00346 0.00012 0.01636 0.01791 0.00102 0.00052 0.00049 0.00000 0.00286 0.00290 0.00288 0.00103 0.00114 0.00103 0.00275 N3 -0.36005 0.27688 -0.23973 1.00000 0.01767 0.01777 0.01721 -0.00009 0.00337 0.00060 0.01756 0.01812 0.00102 0.00051 0.00049 0.00000 0.00292 0.00294 0.00294 0.00103 0.00115 0.00103 0.00280 N4 -0.39468 0.11977 -0.38653 1.00000 0.01286 0.01271 0.01252 0.00016 0.00250 0.00003 0.01270 0.01730 0.00098 0.00050 0.00046 0.00000 0.00276 0.00279 0.00278 0.00103 0.00113 0.00102 0.00264 O1 0.05595 0.34353 0.38840 1.00000 0.02207 0.02262 0.02218 0.00019 0.00464 0.00031 0.02226 0.01486 0.00084 0.00043 0.00041 0.00000 0.00251 0.00254 0.00253 0.00103 0.00110 0.00102 0.00237 O2 0.13154 0.13588 0.23985 1.00000 0.01712 0.01716 0.01745 0.00058 0.00371 -0.00029 0.01720 0.01443 0.00084 0.00040 0.00039 0.00000 0.00237 0.00240 0.00239 0.00102 0.00109 0.00101 0.00223 O3 -0.09766 0.15297 0.25301 1.00000 0.03121 0.03166 0.03184 -0.00022 0.00648 0.00017 0.03154 0.01594 0.00095 0.00046 0.00043 0.00000 0.00263 0.00265 0.00264 0.00103 0.00112 0.00102 0.00250 O4 -0.44455 0.35274 -0.12943 1.00000 0.02448 0.02485 0.02461 -0.00003 0.00496 0.00028 0.02463 0.01518 0.00086 0.00043 0.00041 0.00000 0.00254 0.00257 0.00256 0.00103 0.00111 0.00102 0.00241 O5 -0.35014 0.11488 -0.23368 1.00000 0.01936 0.01888 0.01925 0.00030 0.00426 -0.00016 0.01910 0.01441 0.00084 0.00042 0.00039 0.00000 0.00237 0.00240 0.00239 0.00103 0.00109 0.00102 0.00223 O6 -0.57381 0.12447 -0.21011 1.00000 0.02946 0.03012 0.02991 0.00033 0.00625 0.00025 0.02978 0.01561 0.00092 0.00046 0.00041 0.00000 0.00263 0.00265 0.00264 0.00103 0.00111 0.00102 0.00250 F1 0.06832 0.05438 0.35565 1.00000 0.25637 0.04256 0.01630 0.01778 0.02284 0.03211 0.10565 0.02163 0.00147 0.00049 0.00044 0.00000 0.01503 0.00704 0.00638 0.00571 0.00727 0.00797 0.00457 F2 -0.10756 0.01984 0.28260 1.00000 0.07795 0.04020 0.16670 0.01502 0.06998 -0.00700 0.08867 0.02106 0.00109 0.00045 0.00059 0.00000 0.00801 0.00616 0.01143 0.00733 0.00759 0.00557 0.00377 F3 0.10612 0.00269 0.26863 1.00000 0.05069 0.03609 0.04426 -0.00158 0.01498 0.01232 0.04291 0.01475 0.00085 0.00039 0.00039 0.00000 0.00574 0.00536 0.00571 0.00504 0.00460 0.00457 0.00235 F4 -0.52562 0.01480 -0.13197 1.00000 0.07444 0.08530 0.13739 0.06723 0.06526 0.01938 0.09296 0.02209 0.00106 0.00052 0.00056 0.00000 0.00775 0.00785 0.00981 0.00811 0.00713 0.00617 0.00380 F5 -0.30957 0.04534 -0.10965 1.00000 0.10161 0.04874 0.03675 0.01869 -0.00605 0.00600 0.06508 0.01691 0.00104 0.00045 0.00041 0.00000 0.00803 0.00632 0.00596 0.00550 0.00570 0.00568 0.00289 F6 -0.37777 -0.02118 -0.19103 1.00000 0.12360 0.01273 0.05271 0.00222 0.02834 0.01929 0.06152 0.01729 0.00106 0.00040 0.00043 0.00000 0.00845 0.00506 0.00636 0.00531 0.00581 0.00527 0.00285 Pd1 0.12324 0.23137 0.18116 1.00000 0.01374 0.02330 0.01167 -0.00317 0.00397 -0.00038 0.01604 0.00188 0.00011 0.00005 0.00005 0.00000 0.00064 0.00075 0.00073 0.00066 0.00047 0.00055 0.00040 Pd2 -0.37605 0.19441 -0.30966 1.00000 0.01416 0.02338 0.01420 0.00223 0.00343 0.00050 0.01716 0.00192 0.00011 0.00005 0.00005 0.00000 0.00066 0.00076 0.00074 0.00066 0.00049 0.00054 0.00041 Final Structure Factor Calculation for DIRDIF output for 02SRC222 Total number of l.s. parameters = 438 Maximum vector length = 511 Memory required = 5091 / 25039 wR2 = 0.1147 before cycle 5 for 2323 data and 0 / 438 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 240. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.283; Restrained GooF = 1.210 for 240 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 44.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0535 for 1940 Fo > 4sig(Fo) and 0.0682 for all 2323 data wR2 = 0.1147, GooF = S = 1.283, Restrained GooF = 1.210 for all data Occupancy sum of asymmetric unit = 48.00 for non-hydrogen and 40.00 for hydrogen atoms Principal mean square atomic displacements U 0.0131 0.0129 0.0127 C1 0.0172 0.0169 0.0167 C2 0.0194 0.0192 0.0190 C3 0.0172 0.0171 0.0170 C4 0.0229 0.0226 0.0225 C5 0.0330 0.0327 0.0327 C6 0.0281 0.0277 0.0275 C7 0.0356 0.0355 0.0352 C8 0.0236 0.0232 0.0231 C9 0.0160 0.0157 0.0149 C10 0.0220 0.0218 0.0217 C11 0.0234 0.0228 0.0228 C12 0.0216 0.0213 0.0212 C13 0.0198 0.0196 0.0194 C14 0.0095 0.0092 0.0087 C15 0.0149 0.0146 0.0145 C16 0.0234 0.0232 0.0231 C17 0.0311 0.0310 0.0309 C18 0.0195 0.0194 0.0193 C19 0.0151 0.0147 0.0145 C20 0.0327 0.0324 0.0323 C21 0.0224 0.0223 0.0222 C22 0.0260 0.0259 0.0256 C23 0.0176 0.0175 0.0173 C24 0.0180 0.0176 0.0173 C25 0.0221 0.0218 0.0217 C26 0.0200 0.0195 0.0191 C27 0.0228 0.0224 0.0222 C28 0.0151 0.0147 0.0144 C29 0.0133 0.0132 0.0128 C30 0.0105 0.0100 0.0094 N1 0.0167 0.0165 0.0158 N2 0.0184 0.0172 0.0171 N3 0.0129 0.0128 0.0124 N4 0.0228 0.0222 0.0218 O1 0.0179 0.0174 0.0163 O2 0.0320 0.0317 0.0310 O3 0.0250 0.0246 0.0243 O4 0.0197 0.0192 0.0184 O5 0.0305 0.0297 0.0291 O6 0.2640 0.0458 0.0072 F1 may be split into 0.0923 0.0560 0.3544 and 0.0443 0.0527 0.3569 0.1795 0.0579 0.0285 F2 0.0581 0.0440 0.0266 F3 0.1928 0.0598 0.0263 F4 0.1122 0.0617 0.0214 F5 0.1270 0.0482 0.0093 F6 0.0241 0.0140 0.0100 Pd1 0.0239 0.0144 0.0132 Pd2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.026 0.041 0.055 0.070 0.090 0.114 0.148 0.207 1.000 Number in group 239. 235. 232. 227. 237. 230. 231. 226. 232. 234. GooF 1.879 1.687 1.581 1.125 1.344 0.972 0.907 0.921 0.946 0.953 K 7.554 1.868 1.391 1.094 1.088 1.012 0.994 0.997 0.993 1.002 Resolution(A) 0.91 1.07 1.20 1.28 1.36 1.46 1.57 1.74 1.98 2.49 inf Number in group 233. 232. 234. 233. 237. 232. 229. 228. 235. 230. GooF 1.120 1.335 1.326 1.191 1.419 1.278 1.098 1.159 1.311 1.527 K 1.056 1.029 1.030 1.004 1.012 1.005 1.003 1.004 1.005 1.008 R1 0.159 0.109 0.096 0.075 0.066 0.067 0.051 0.045 0.040 0.045 Recommended weighting scheme: WGHT 0.0000 44.3102 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 16 2216.67 178.26 5.30 0.020 1.19 4 0 12 4306.76 1555.73 5.22 0.060 1.23 2 2 0 1229.40 189.10 5.16 0.021 4.14 0 14 0 3769.58 1448.08 5.01 0.058 1.37 0 13 4 1288.38 11.69 4.91 0.005 1.41 0 5 8 1815.98 332.09 4.74 0.028 2.08 2 13 0 3531.57 1354.13 4.69 0.056 1.40 -1 2 2 590.84 10.25 4.61 0.005 5.92 2 2 8 727.23 21.72 4.47 0.007 1.98 1 6 5 1371.68 183.19 4.36 0.021 2.33 -2 14 2 1109.59 73.67 4.27 0.013 1.31 -2 14 4 2170.83 443.20 4.18 0.032 1.29 -8 11 4 3684.68 1624.54 4.17 0.061 0.97 0 1 3 535.27 23.25 4.17 0.007 6.25 0 1 16 3237.72 660.14 4.13 0.039 1.24 0 3 8 881.35 116.05 4.13 0.016 2.31 -4 14 2 990.49 2.98 4.04 0.003 1.18 5 2 0 820.40 0.93 4.03 0.001 1.80 -6 1 12 1274.82 150.63 3.93 0.019 1.25 0 3 1 780.99 159.19 3.90 0.019 6.08 0 14 2 1403.58 325.94 3.84 0.027 1.35 6 1 4 1132.09 302.27 3.80 0.026 1.38 3 3 13 1056.62 13.75 3.76 0.006 1.25 -4 13 2 1486.74 90.11 3.73 0.014 1.25 1 4 13 816.26 4.12 3.56 0.003 1.40 3 6 1 438.18 7.66 3.55 0.004 2.16 2 1 4 1060.52 346.49 3.54 0.028 3.04 0 5 6 5148.48 3213.29 3.53 0.086 2.50 0 13 2 743.18 7.57 3.53 0.004 1.46 -3 8 5 842.88 63.15 3.48 0.012 1.79 -1 1 4 714.70 164.63 3.43 0.020 4.64 1 1 3 1442.22 587.21 3.41 0.037 4.77 4 1 8 741.22 63.16 3.33 0.012 1.54 -2 12 2 1600.24 0.72 3.30 0.001 1.50 2 1 12 2784.68 831.55 3.29 0.044 1.46 0 12 6 675.69 27.10 3.29 0.008 1.44 5 5 1 3391.91 1997.30 3.24 0.068 1.63 -3 2 7 401.50 24.23 3.23 0.007 2.26 1 3 2 660.81 156.83 3.19 0.019 4.43 2 3 12 1411.34 594.21 3.18 0.037 1.43 1 9 3 587.63 58.65 3.16 0.012 1.95 2 12 0 544.10 28.76 3.09 0.008 1.51 -2 16 2 1317.36 477.67 3.08 0.033 1.16 0 13 10 951.13 35.70 3.07 0.009 1.18 -1 7 5 6327.98 4525.55 2.99 0.102 2.25 -8 13 2 1230.31 151.65 2.87 0.019 0.91 0 4 4 2370.14 1397.42 2.85 0.057 3.44 2 15 2 1400.69 573.25 2.84 0.036 1.21 2 0 2 65929.45 74016.59 2.80 0.414 3.89 -2 4 14 3037.53 1903.79 2.78 0.066 1.38 Bond lengths and angles C1 - Distance Angles N1 1.4839 (0.0134) C2 1.5042 (0.0149) 112.09 (0.93) H1A 0.9900 109.19 109.19 H1B 0.9900 109.19 109.19 107.89 C1 - N1 C2 H1A C2 - Distance Angles O1 1.4487 (0.0131) C1 1.5042 (0.0149) 110.50 (0.91) H2A 0.9900 109.55 109.55 H2B 0.9900 109.55 109.55 108.10 C2 - O1 C1 H2A C3 - Distance Angles O1 1.4543 (0.0130) C4 1.5204 (0.0154) 110.97 (0.95) H3A 0.9900 109.44 109.44 H3B 0.9900 109.44 109.44 108.04 C3 - O1 C4 H3A C4 - Distance Angles N1 1.4928 (0.0139) C3 1.5204 (0.0154) 111.82 (0.92) H4A 0.9900 109.25 109.25 H4B 0.9900 109.25 109.26 107.93 C4 - N1 C3 H4A C5 - Distance Angles O2 1.2411 (0.0133) O3 1.2466 (0.0135) 128.47 (1.26) C6 1.5137 (0.0188) 113.40 (1.19) 118.10 (1.22) C5 - O2 O3 C6 - Distance Angles F1 1.2843 (0.0165) F3 1.2960 (0.0158) 109.80 (1.39) F2 1.3392 (0.0159) 105.77 (1.39) 105.88 (1.31) C5 1.5137 (0.0188) 110.48 (1.39) 114.80 (1.27) 109.63 (1.24) C6 - F1 F3 F2 C7 - Distance Angles N2 1.4919 (0.0142) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - N2 H7A H7B C8 - Distance Angles N2 1.5065 (0.0153) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - N2 H8A H8B C9 - Distance Angles C10 1.4413 (0.0160) N2 1.4838 (0.0145) 110.41 (1.03) H9A 0.9900 109.57 109.57 H9B 0.9900 109.57 109.57 108.11 C9 - C10 N2 H9A C10 - Distance Angles C11 1.3898 (0.0154) C15 1.4175 (0.0158) 119.00 (1.12) C9 1.4413 (0.0160) 125.63 (1.18) 115.35 (1.21) C10 - C11 C15 C11 - Distance Angles C12 1.3469 (0.0162) C10 1.3898 (0.0153) 120.79 (1.27) H11 0.9500 119.60 119.60 C11 - C12 C10 C12 - Distance Angles C11 1.3469 (0.0162) C13 1.4076 (0.0165) 121.37 (1.37) H12 0.9500 119.32 119.31 C12 - C11 C13 C13 - Distance Angles C14 1.3855 (0.0153) C12 1.4076 (0.0165) 118.99 (1.22) H13 0.9500 120.50 120.51 C13 - C14 C12 C14 - Distance Angles C13 1.3855 (0.0153) C15 1.3944 (0.0159) 120.13 (1.19) H14 0.9500 119.94 119.93 C14 - C13 C15 C15 - Distance Angles C14 1.3944 (0.0159) C10 1.4175 (0.0158) 119.64 (1.20) Pd1 1.9982 (0.0120) 127.83 (0.95) 112.52 (0.89) C15 - C14 C10 C16 - Distance Angles N3 1.4874 (0.0141) C17 1.5045 (0.0155) 110.44 (0.99) H16A 0.9900 109.56 109.56 H16B 0.9900 109.56 109.56 108.11 C16 - N3 C17 H16A C17 - Distance Angles O4 1.4461 (0.0135) C16 1.5045 (0.0155) 111.75 (0.96) H17A 0.9900 109.27 109.27 H17B 0.9900 109.27 109.27 107.94 C17 - O4 C16 H17A C18 - Distance Angles O4 1.4406 (0.0139) C19 1.5019 (0.0162) 111.96 (1.07) H18A 0.9900 109.22 109.22 H18B 0.9900 109.22 109.22 107.91 C18 - O4 C19 H18A C19 - Distance Angles N3 1.4890 (0.0144) C18 1.5019 (0.0162) 111.27 (0.99) H19A 0.9900 109.38 109.38 H19B 0.9900 109.38 109.38 108.00 C19 - N3 C18 H19A C20 - Distance Angles O6 1.2263 (0.0127) O5 1.2341 (0.0125) 132.00 (1.22) C21 1.5530 (0.0183) 115.13 (1.13) 112.86 (1.13) C20 - O6 O5 C21 - Distance Angles F4 1.2924 (0.0154) F6 1.3038 (0.0160) 109.24 (1.34) F5 1.3434 (0.0159) 103.48 (1.30) 103.61 (1.29) C20 1.5530 (0.0183) 114.65 (1.27) 114.29 (1.21) 110.46 (1.22) C21 - F4 F6 F5 C22 - Distance Angles N4 1.4935 (0.0137) H22A 0.9800 109.47 H22B 0.9800 109.47 109.47 H22C 0.9800 109.47 109.47 109.47 C22 - N4 H22A H22B C23 - Distance Angles N4 1.4639 (0.0143) H23A 0.9800 109.47 H23B 0.9800 109.47 109.47 H23C 0.9800 109.47 109.47 109.47 C23 - N4 H23A H23B C24 - Distance Angles C25 1.4743 (0.0162) N4 1.4783 (0.0140) 109.52 (1.03) H24A 0.9900 109.77 109.77 H24B 0.9900 109.77 109.77 108.23 C24 - C25 N4 H24A C25 - Distance Angles C26 1.3843 (0.0154) C30 1.4074 (0.0155) 119.72 (1.13) C24 1.4743 (0.0162) 123.99 (1.17) 116.29 (1.16) C25 - C26 C30 C26 - Distance Angles C27 1.3635 (0.0165) C25 1.3843 (0.0155) 120.00 (1.28) H26 0.9500 120.00 120.00 C26 - C27 C25 C27 - Distance Angles C26 1.3635 (0.0165) C28 1.3863 (0.0155) 122.14 (1.31) H27 0.9500 118.93 118.93 C27 - C26 C28 C28 - Distance Angles C27 1.3863 (0.0156) C29 1.4001 (0.0153) 117.27 (1.20) H28 0.9500 121.36 121.36 C28 - C27 C29 C29 - Distance Angles C30 1.3732 (0.0161) C28 1.4001 (0.0153) 122.03 (1.20) H29 0.9500 118.98 118.98 C29 - C30 C28 C30 - Distance Angles C29 1.3732 (0.0161) C25 1.4074 (0.0155) 118.77 (1.15) Pd2 1.9918 (0.0121) 128.95 (1.00) 112.27 (0.88) C30 - C29 C25 N1 - Distance Angles C1 1.4839 (0.0134) C4 1.4928 (0.0139) 106.81 (0.87) Pd1 2.1011 (0.0094) 114.25 (0.67) 109.67 (0.68) N1 - C1 C4 N2 - Distance Angles C9 1.4838 (0.0145) C7 1.4919 (0.0142) 109.77 (0.94) C8 1.5065 (0.0153) 110.53 (0.93) 106.64 (0.96) Pd1 2.0732 (0.0097) 105.50 (0.71) 109.89 (0.73) 114.50 (0.76) N2 - C9 C7 C8 N3 - Distance Angles C16 1.4874 (0.0141) C19 1.4890 (0.0143) 108.22 (0.91) Pd2 2.1062 (0.0100) 115.28 (0.74) 110.58 (0.71) N3 - C16 C19 N4 - Distance Angles C23 1.4639 (0.0144) C24 1.4783 (0.0140) 110.76 (0.95) C22 1.4935 (0.0137) 108.26 (0.93) 108.30 (0.89) Pd2 2.0946 (0.0094) 115.49 (0.74) 105.20 (0.68) 108.60 (0.70) N4 - C23 C24 C22 O1 - Distance Angles C2 1.4487 (0.0131) C3 1.4543 (0.0130) 107.75 (0.84) O1 - C2 O2 - Distance Angles C5 1.2411 (0.0133) Pd1 2.1734 (0.0078) 116.20 (0.80) O2 - C5 O3 - Distance Angles C5 1.2466 (0.0135) O3 - O4 - Distance Angles C18 1.4406 (0.0139) C17 1.4461 (0.0135) 108.09 (0.91) O4 - C18 O5 - Distance Angles C20 1.2341 (0.0126) Pd2 2.1440 (0.0081) 120.41 (0.79) O5 - C20 O6 - Distance Angles C20 1.2263 (0.0127) O6 - F1 - Distance Angles C6 1.2843 (0.0165) F1 - F2 - Distance Angles C6 1.3392 (0.0160) F2 - F3 - Distance Angles C6 1.2960 (0.0158) F3 - F4 - Distance Angles C21 1.2924 (0.0154) F4 - F5 - Distance Angles C21 1.3434 (0.0160) F5 - F6 - Distance Angles C21 1.3038 (0.0160) F6 - Pd1 - Distance Angles C15 1.9982 (0.0120) N2 2.0732 (0.0097) 81.65 (0.45) N1 2.1011 (0.0094) 93.39 (0.43) 174.76 (0.38) O2 2.1734 (0.0078) 172.71 (0.40) 91.21 (0.35) 93.79 (0.33) Pd1 - C15 N2 N1 Pd2 - Distance Angles C30 1.9918 (0.0121) N4 2.0946 (0.0095) 81.74 (0.44) N3 2.1062 (0.0100) 92.71 (0.45) 174.45 (0.37) O5 2.1440 (0.0081) 173.33 (0.41) 91.71 (0.33) 93.84 (0.33) Pd2 - C30 N4 N3 FMAP and GRID set by program FMAP 2 1 21 GRID -2.778 -2 -1 2.778 2 1 R1 = 0.0673 for 2323 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.55 at 0.4492 0.6414 0.0635 [ 1.35 A from O4 ] Deepest hole -0.64 at 0.1286 0.2665 0.4567 [ 1.09 A from H2A ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 4957 / 30699 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.4492 0.3586 -0.0635 1.00000 0.05 0.55 1.35 O4 1.65 H24A 2.03 H17A 2.04 H26 Q2 1 -0.2801 0.3036 -0.2515 1.00000 0.05 0.49 0.98 N3 1.89 O3 1.99 C16 2.11 H29 Q3 1 0.1191 0.2843 -0.0783 1.00000 0.05 0.49 1.54 H11 1.55 H2A 1.79 H1B 2.04 C2 Q4 1 -0.5464 -0.0135 -0.1903 1.00000 0.05 0.47 1.28 F4 1.50 C21 1.59 F6 2.37 C20 Q5 1 0.2285 0.3271 0.2586 1.00000 0.05 0.46 0.98 N1 2.05 H14 2.06 O6 2.06 C4 Q6 1 0.0564 0.3595 0.4490 1.00000 0.05 0.41 1.26 O1 1.64 H9A 2.00 H7A 2.15 C2 Q7 1 -0.3491 0.1176 -0.2968 1.00000 0.05 0.41 1.28 O5 1.51 PD2 1.78 N4 1.83 H23B Q8 1 -0.3774 0.2184 -0.0880 1.00000 0.05 0.41 1.36 H16B 1.78 H26 1.91 H27 1.93 H17A Q9 1 0.1276 0.3032 0.1610 1.00000 0.05 0.40 0.89 C15 1.44 PD1 1.64 C14 1.86 H14 Q10 1 -0.4475 0.4163 -0.5645 1.00000 0.05 0.39 1.16 H27 1.88 F5 1.94 F4 1.96 C27 Shortest distances between peaks (including symmetry equivalents) 5 9 2.07 8 10 2.73 1 8 2.83 3 6 2.89 Time profile in seconds ----------------------- 0.11: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.22: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.05: Structure factors and derivatives 5.00: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 1.09: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.22: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.11: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 15:56:59 Total elapsed time: 7.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++