++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XL - CRYSTAL STRUCTURE REFINEMENT - SHELXTL Version 2008/4 + + Copyright(c) 2008 Bruker Analytical X-ray Solutions All Rights Reserved + + UDEL6 started at 16:22:37 on 04-Feb-2011 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL UDel6 in P2(1)/c CELL 1.54178 19.6526 12.4231 9.5355 90.000 94.330 90.000 ZERR 8.00 0.0023 0.0015 0.0011 0.000 0.003 0.000 LATT 1 SYMM -x, y+1/2, -z+1/2 SFAC C H N O F Cl UNIT 80 48 8 8 48 8 V = 2321.41 F(000) = 1216.0 Mu = 3.66 mm-1 Cell Wt = 2444.86 Rho = 1.749 L.S. 12 BOND $H FMAP 2 PLAN 20 SIZE 0.076 0.356 0.794 TEMP -173 EXYZ C7 C7' EADP C7 C7' EXYZ C8 C8' EADP C8 C8' EXYZ C17A C17B C17C C17D EADP C17A C17B C17C C17D EXYZ C18 C18' EADP C18 C18' SUMP 1.0000 0.005 1 4 1 5 1 6 1 7 SADI C7 F1 C7 F2 C7 F3 C7' F1' C7' F2' C7' F3' = C8 F4 C8 F5 C8 F6 C8' F4' C8' F5' C8' F5' = C17A F7A C17A F8A C17A F9A C17B F7B C17B F8B C17B F9B = C17C F7C C17C F8C C17C F9C C17D F7D C17D F8D C17D F9D = C18 F10 C18 F11 C18 F12 C18' F10' C18' F11' C18' F12' SADI F1 F2 F2 F3 F3 F1 F1' F2' F2' F3' F3' F1' = F4 F5 F5 F6 F6 F4 F4' F5' F5' F6' F6' F4' = F7A F8A F8A F9A F9A F7A F7B F8B F8B F9B F9B F7B = F7C F8C F8C F9C F9C F7C F7D F8D F8D F9D F9D F7D = F10 F11 F11 F12 F12 F10 F10' F11' F11' F12' F12' F11' ACTA BOND $H CONF WGHT 0.0686 1.7879 FVAR 0.08928 0.40440 0.49765 0.32274 0.21653 0.21263 0.25234 FVAR 0.55607 C1 1 0.486863 0.118922 0.775017 11.00000 0.02987 0.02890 = 0.02329 0.00003 0.00781 0.00000 AFIX 43 H1A 2 0.515446 0.126150 0.699550 11.00000 -1.20000 AFIX 0 C2 1 0.421641 0.078774 0.749928 11.00000 0.03191 0.02744 = 0.02599 -0.00170 0.00342 -0.00009 C3 1 0.378800 0.067161 0.858416 11.00000 0.02657 0.02780 = 0.03399 -0.00025 0.00497 -0.00077 AFIX 43 H3A 2 0.333840 0.039719 0.840928 11.00000 -1.20000 AFIX 0 C4 1 0.403518 0.096730 0.992709 11.00000 0.02797 0.02619 = 0.03046 0.00158 0.00864 0.00275 C5 1 0.469021 0.136843 1.021230 11.00000 0.02886 0.02756 = 0.02383 -0.00059 0.00698 0.00075 AFIX 43 H5A 2 0.485000 0.155751 1.114494 11.00000 -1.20000 AFIX 0 C6 1 0.511030 0.148939 0.910593 11.00000 0.02674 0.02416 = 0.02595 0.00043 0.00598 0.00063 PART 1 C7 1 0.397991 0.045820 0.603167 21.00000 0.03821 0.04181 = 0.03209 -0.00569 0.00157 -0.00652 F1 5 0.432541 -0.041530 0.563818 21.00000 0.05233 0.05982 = 0.04963 -0.03091 0.01233 0.00200 F2 5 0.406914 0.119650 0.505688 21.00000 0.09359 0.04235 = 0.03395 -0.00299 -0.02320 -0.00644 F3 5 0.332660 0.017047 0.588683 21.00000 0.03970 0.12232 = 0.05908 -0.05639 0.01633 -0.03491 PART 2 SAME C7 > F3 C7' 1 0.397991 0.045820 0.603167 -21.00000 0.03821 0.04181 = 0.03209 -0.00569 0.00157 -0.00652 F1' 5 0.423471 -0.048066 0.566568 -21.00000 0.09058 0.03467 = 0.04077 -0.01051 -0.00409 -0.00147 F2' 5 0.417551 0.117770 0.511458 -21.00000 0.08423 0.06595 = 0.02253 0.00733 -0.00361 -0.02644 F3' 5 0.330671 0.037493 0.586674 -21.00000 0.04163 0.11688 = 0.04564 -0.01251 -0.01388 -0.00662 PART 1 SAME C7 > F3 C8 1 0.358761 0.087534 1.113829 31.00000 0.02924 0.03726 = 0.03492 0.00296 0.01156 0.00089 F4 5 0.298541 0.043905 1.075105 31.00000 0.02469 0.08174 = 0.05893 0.01476 0.01425 -0.01494 F5 5 0.346309 0.184757 1.166912 31.00000 0.06357 0.03941 = 0.07748 -0.01009 0.04921 0.00002 F6 5 0.387089 0.029617 1.218444 31.00000 0.03771 0.05069 = 0.04843 0.00608 0.01667 0.00761 PART 2 SAME C7 > F3 C8' 1 0.358761 0.087534 1.113829 -31.00000 0.02924 0.03726 = 0.03492 0.00296 0.01156 0.00089 F4' 5 0.303815 0.025066 1.083281 -31.00000 0.04549 0.07387 = 0.03695 0.00196 0.01099 -0.02092 F5' 5 0.335648 0.181761 1.154321 -31.00000 0.05049 0.05703 = 0.05015 0.00215 0.02840 0.01978 F6' 5 0.391872 0.042921 1.227243 -31.00000 0.04682 0.07047 = 0.01460 0.01100 0.00927 -0.00003 PART 0 N1 3 0.577863 0.191493 0.927140 11.00000 0.02793 0.03528 = 0.01751 -0.00017 0.00790 -0.00425 AFIX 43 H1B 2 0.597578 0.204456 0.849028 11.00000 -1.20000 AFIX 0 C9 1 0.615097 0.214648 1.047896 11.00000 0.02823 0.02518 = 0.02022 -0.00185 0.00604 0.00096 O1 4 0.595837 0.202073 1.165084 11.00000 0.03385 0.04523 = 0.02132 -0.00415 0.00766 -0.00797 C10 1 0.686667 0.254910 1.023897 11.00000 0.02874 0.04228 = 0.02564 -0.00388 0.00801 -0.00387 AFIX 23 H10A 2 0.685450 0.296039 0.934816 11.00000 -1.20000 H10B 2 0.717635 0.192734 1.015792 11.00000 -1.20000 AFIX 0 CL1 6 0.717814 0.337794 1.164318 11.00000 0.04171 0.05390 = 0.03074 -0.00558 0.00350 -0.01857 C11 1 0.960881 0.368602 0.921262 11.00000 0.03097 0.03314 = 0.02612 -0.00029 0.00816 -0.00198 AFIX 43 H11A 2 0.976963 0.350947 0.832636 11.00000 -1.20000 AFIX 0 C12 1 0.897468 0.417192 0.929148 11.00000 0.02784 0.03574 = 0.03482 0.00217 0.00683 -0.00318 C13 1 0.872468 0.444921 1.056392 11.00000 0.02949 0.03086 = 0.04131 0.00263 0.01200 0.00001 AFIX 43 H13A 2 0.829093 0.478146 1.059928 11.00000 -1.20000 AFIX 0 C14 1 0.912725 0.422615 1.177613 11.00000 0.03663 0.02937 = 0.03301 -0.00087 0.01531 -0.00210 C15 1 0.975804 0.373694 1.173390 11.00000 0.03494 0.03016 = 0.02682 0.00030 0.00914 0.00038 AFIX 43 H15A 2 1.002468 0.358755 1.258434 11.00000 -1.20000 AFIX 0 C16 1 1.000291 0.346316 1.044914 11.00000 0.02962 0.02678 = 0.02617 0.00010 0.00928 -0.00214 PART 1 SAME C7 > F3 C17A 1 0.855088 0.439526 0.794631 41.00000 0.03360 0.06099 = 0.04147 0.00582 0.00174 0.00276 F7A 5 0.788432 0.441332 0.804107 41.00000 0.02599 0.13808 = 0.03743 -0.00499 0.00469 0.01509 F8A 5 0.864510 0.359630 0.698612 41.00000 0.02430 0.07755 = 0.02895 -0.01817 -0.00819 0.01031 F9A 5 0.871551 0.528463 0.728249 41.00000 0.10860 0.06855 = 0.05980 0.04282 -0.01850 -0.00730 PART 2 SAME C7 > F3 C17B 1 0.855088 0.439526 0.794631 51.00000 0.03360 0.06099 = 0.04147 0.00582 0.00174 0.00276 F7B 5 0.892062 0.472892 0.690547 51.00000 0.03867 0.09523 = 0.01165 -0.01847 -0.01086 -0.00782 F8B 5 0.815727 0.528818 0.817437 51.00000 0.04856 0.05830 = 0.04822 0.02009 0.01445 0.03074 F9B 5 0.813247 0.366306 0.743721 51.00000 0.13639 0.12306 = 0.11888 0.05641 -0.08394 -0.07412 PART 3 SAME C7 > F3 C17C 1 0.855088 0.439526 0.794631 61.00000 0.03360 0.06099 = 0.04147 0.00582 0.00174 0.00276 F7C 5 0.882122 0.411798 0.678038 61.00000 0.04003 0.37456 = 0.03317 -0.04607 0.00297 -0.01063 F8C 5 0.838282 0.543517 0.783067 61.00000 0.13656 0.05531 = 0.04583 0.03488 -0.04346 -0.04467 F9C 5 0.797488 0.386109 0.799552 61.00000 0.06986 0.09719 = 0.08940 0.01744 -0.04071 -0.04812 PART 4 SAME C7 > F3 C17D 1 0.855088 0.439526 0.794631 71.00000 0.03360 0.06099 = 0.04147 0.00582 0.00174 0.00276 F7D 5 0.889868 0.507202 0.718290 71.00000 0.07714 0.04471 = 0.02257 -0.00232 -0.01486 -0.01978 F8D 5 0.797748 0.488629 0.819337 71.00000 0.03949 0.33341 = 0.09989 0.02760 -0.00109 0.06717 F9D 5 0.841017 0.355382 0.714818 71.00000 0.04426 0.06564 = 0.11465 0.01380 -0.05444 -0.03363 PART 1 SAME C7 > F3 C18 1 0.888827 0.448711 1.320012 81.00000 0.04489 0.04088 = 0.03721 -0.00327 0.01794 0.00493 F10 5 0.830334 0.498181 1.318036 81.00000 0.04130 0.09431 = 0.08102 -0.03915 0.02809 -0.00275 F11 5 0.886741 0.363362 1.404089 81.00000 0.20510 0.04766 = 0.06531 0.01809 0.08803 0.03799 F12 5 0.934765 0.514903 1.389018 81.00000 0.04965 0.06977 = 0.02762 -0.00955 0.00888 0.00918 PART 2 SAME C7 > F3 C18' 1 0.888827 0.448711 1.320012 -81.00000 0.04489 0.04088 = 0.03721 -0.00327 0.01794 0.00493 F10' 5 0.831722 0.508034 1.308825 -81.00000 0.04106 0.03960 = 0.03295 -0.00637 0.01344 0.01601 F11' 5 0.871099 0.358133 1.382354 -81.00000 0.07047 0.06051 = 0.03300 0.00849 0.02922 0.00381 F12' 5 0.933053 0.498506 1.407233 -81.00000 0.04253 0.14287 = 0.03367 -0.02580 0.00724 -0.00972 PART 0 N2 3 1.065378 0.297129 1.050009 11.00000 0.03129 0.03597 = 0.01925 0.00200 0.00648 0.00508 AFIX 43 H2A 2 1.082792 0.277707 1.133933 11.00000 -1.20000 AFIX 0 C19 1 1.103896 0.276402 0.942537 11.00000 0.03069 0.02770 = 0.02022 -0.00189 0.00681 -0.00197 O2 4 1.086668 0.296340 0.819666 11.00000 0.03344 0.04896 = 0.01991 -0.00171 0.00633 0.00502 C20 1 1.171629 0.223045 0.988138 11.00000 0.03421 0.04949 = 0.02490 0.00567 0.01048 0.00862 AFIX 23 H20A 2 1.166311 0.143840 0.983934 11.00000 -1.20000 H20B 2 1.185548 0.243190 1.086595 11.00000 -1.20000 AFIX 0 CL2 6 1.235094 0.262994 0.878685 11.00000 0.03094 0.09364 = 0.05802 0.03309 0.01473 0.00708 HKLF 4 1 1 0 0 0 1 0 0 0 1 Covalent radii and connectivity table for UDel6 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 CL 0.990 C1 - C2 C6 C2 - C1 C3 C7'_b C7_a C3 - C4 C2 C4 - C3 C5 C8'_b C8_a C5 - C4 C6 C6 - C1 C5 N1 C7_a - F2_a F3_a F1_a C2 F1_a - C7_a F2_a - C7_a F3_a - C7_a C7'_b - F3'_b F1'_b F2'_b C2 F1'_b - C7'_b F2'_b - C7'_b F3'_b - C7'_b C8_a - F6_a F4_a F5_a C4 F4_a - C8_a F5_a - C8_a F6_a - C8_a C8'_b - F5'_b F6'_b F4'_b C4 F4'_b - C8'_b F5'_b - C8'_b F6'_b - C8'_b N1 - C9 C6 C9 - O1 N1 C10 O1 - C9 C10 - C9 Cl1 Cl1 - C10 C11 - C16 C12 C12 - C13 C11 C17D_d C17A_a C17B_b C17C_c C13 - C14 C12 C14 - C13 C15 C18'_b C18_a C15 - C14 C16 C16 - C11 C15 N2 C17A_a - F7A_a F9A_a F8A_a C12 F7A_a - C17A_a F8A_a - C17A_a F9A_a - C17A_a C17B_b - F9B_b F7B_b F8B_b C12 F7B_b - C17B_b F8B_b - C17B_b F9B_b - C17B_b C17C_c - F7C_c F9C_c F8C_c C12 F7C_c - C17C_c F8C_c - C17C_c F9C_c - C17C_c C17D_d - F9D_d F8D_d F7D_d C12 F7D_d - C17D_d F8D_d - C17D_d F9D_d - C17D_d C18_a - F10_a F11_a F12_a C14 F10_a - C18_a F11_a - C18_a F12_a - C18_a C18'_b - F12'_b F11'_b F10'_b C14 F10'_b - C18'_b F11'_b - C18'_b F12'_b - C18'_b N2 - C19 C16 C19 - O2 N2 C20 O2 - C19 C20 - C19 Cl2 Cl2 - C20 h k l Fo^2 Sigma Why rejected 0 3 0 0.04 0.01 observed but should be systematically absent -7 0 3 0.04 0.01 observed but should be systematically absent -13 0 5 0.12 0.03 observed but should be systematically absent -13 0 1 0.06 0.01 observed but should be systematically absent 18876 Reflections read, of which 626 rejected -24 =< h =< 23, -14 =< k =< 15, -11 =< l =< 11, Max. 2-theta = 142.57 4 Systematic absence violations 0 Inconsistent equivalents 4389 Unique reflections, of which 0 suppressed R(int) = 0.0542 R(sigma) = 0.0521 Friedel opposites merged Maximum memory for data reduction = 4079 / 43824 Default effective X-H distances for T = -173.0 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 = 5407 / 680655 wR2 = 0.1312 before cycle 1 for 4389 data and 512 / 512 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.0832 0.0200 SAME/SADI C17B_b F8B_b C17B_b F9B_b etc. 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. 976. 0. 0. 0. 0. 0. 0. 1. rms sigma 0.000 0.000 0.000 0.024 0.000 0.000 0.000 0.000 0.000 0.000 0.005 rms deviation 0.000 0.000 0.000 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.004 GooF = S = 1.045; Restrained GooF = 1.023 for 977 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0686 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08907 0.00021 -0.966 OSF 2 0.40832 0.08853 0.044 FVAR 2 3 0.49756 0.09405 -0.001 FVAR 3 4 0.32283 0.02192 0.004 FVAR 4 5 0.21364 0.02079 -0.139 FVAR 5 6 0.20191 0.02171 -0.494 FVAR 6 7 0.26967 0.02817 0.615 FVAR 7 8 0.55454 0.04139 -0.037 FVAR 8 Mean shift/esd = 0.136 Maximum = 1.019 for U13 F9C_c Max. shift = 0.023 A for F9B_b Max. dU =-0.016 for F9C_c Least-squares cycle 2 Maximum vector length = 511 Memory required = 5407 / 680655 wR2 = 0.1302 before cycle 2 for 4389 data and 512 / 512 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.0815 0.0200 SAME/SADI C17B_b F8B_b C17B_b F9B_b etc. 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. 976. 0. 0. 0. 0. 0. 0. 1. rms sigma 0.000 0.000 0.000 0.024 0.000 0.000 0.000 0.000 0.000 0.000 0.005 rms deviation 0.000 0.000 0.000 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.008 GooF = S = 1.037; Restrained GooF = 1.012 for 977 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0686 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08901 0.00021 -0.288 OSF 2 0.41216 0.08663 0.044 FVAR 2 3 0.49424 0.09295 -0.036 FVAR 3 4 0.31726 0.02216 -0.251 FVAR 4 5 0.20389 0.02158 -0.452 FVAR 5 6 0.21126 0.02256 0.415 FVAR 6 7 0.27360 0.02849 0.138 FVAR 7 8 0.55466 0.04176 0.003 FVAR 8 Mean shift/esd = 0.074 Maximum = -0.793 for y F7A_a Max. shift = 0.021 A for F7C_c Max. dU = 0.012 for F7C_c Least-squares cycle 3 Maximum vector length = 511 Memory required = 5407 / 680655 wR2 = 0.1301 before cycle 3 for 4389 data and 512 / 512 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 0.0800 0.0200 SAME/SADI C17B_b F8B_b C17B_b F9B_b etc. 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. 976. 0. 0. 0. 0. 0. 0. 1. rms sigma 0.000 0.000 0.000 0.024 0.000 0.000 0.000 0.000 0.000 0.000 0.005 rms deviation 0.000 0.000 0.000 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.006 GooF = S = 1.037; Restrained GooF = 1.014 for 977 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0686 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08901 0.00021 -0.005 OSF 2 0.41485 0.08673 0.031 FVAR 2 3 0.48980 0.09346 -0.048 FVAR 3 4 0.31566 0.02171 -0.074 FVAR 4 5 0.20621 0.02150 0.108 FVAR 5 6 0.20807 0.02244 -0.143 FVAR 6 7 0.28002 0.02820 0.228 FVAR 7 8 0.55548 0.04215 0.019 FVAR 8 Mean shift/esd = 0.048 Maximum = 0.654 for U33 F9B_b Max. shift = 0.019 A for F9C_c Max. dU =-0.003 for F8C_c Least-squares cycle 4 Maximum vector length = 511 Memory required = 5407 / 680655 wR2 = 0.1300 before cycle 4 for 4389 data and 512 / 512 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.0792 0.0200 SAME/SADI C17B_b F8B_b C17B_b F9B_b etc. 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. 976. 0. 0. 0. 0. 0. 0. 1. rms sigma 0.000 0.000 0.000 0.024 0.000 0.000 0.000 0.000 0.000 0.000 0.005 rms deviation 0.000 0.000 0.000 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.010 GooF = S = 1.036; Restrained GooF = 1.012 for 977 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0686 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08901 0.00021 -0.017 OSF 2 0.41584 0.08676 0.011 FVAR 2 3 0.48687 0.09295 -0.032 FVAR 3 4 0.31120 0.02174 -0.205 FVAR 4 5 0.20703 0.02163 0.038 FVAR 5 6 0.20578 0.02241 -0.102 FVAR 6 7 0.28733 0.02824 0.259 FVAR 7 8 0.55600 0.04217 0.012 FVAR 8 Mean shift/esd = 0.052 Maximum = 0.626 for x F9D_d Max. shift = 0.019 A for F9C_c Max. dU = 0.006 for F7C_c Least-squares cycle 5 Maximum vector length = 511 Memory required = 5407 / 680655 wR2 = 0.1300 before cycle 5 for 4389 data and 512 / 512 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 0.0769 0.0200 SAME/SADI C17B_b F8B_b C17B_b F9B_b etc. 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. 976. 0. 0. 0. 0. 0. 0. 1. rms sigma 0.000 0.000 0.000 0.024 0.000 0.000 0.000 0.000 0.000 0.000 0.005 rms deviation 0.000 0.000 0.000 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.011 GooF = S = 1.036; Restrained GooF = 1.010 for 977 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0686 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08901 0.00021 -0.002 OSF 2 0.41599 0.08661 0.002 FVAR 2 3 0.48532 0.09247 -0.017 FVAR 3 4 0.30600 0.02164 -0.240 FVAR 4 5 0.20670 0.02127 -0.015 FVAR 5 6 0.20400 0.02208 -0.081 FVAR 6 7 0.29437 0.02787 0.253 FVAR 7 8 0.55650 0.04215 0.012 FVAR 8 Mean shift/esd = 0.038 Maximum = 0.471 for U33 F9B_b Max. shift = 0.013 A for F9C_c Max. dU = 0.004 for F9B_b Least-squares cycle 6 Maximum vector length = 511 Memory required = 5407 / 680655 wR2 = 0.1300 before cycle 6 for 4389 data and 512 / 512 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint 0.0744 0.0200 SAME/SADI C17B_b F8B_b C17B_b F9B_b etc. Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 976. 0. 0. 0. 0. 0. 0. 1. rms sigma 0.000 0.000 0.000 0.024 0.000 0.000 0.000 0.000 0.000 0.000 0.005 rms deviation 0.000 0.000 0.000 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.011 GooF = S = 1.036; Restrained GooF = 1.008 for 977 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0686 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08901 0.00021 0.010 OSF 2 0.41659 0.08642 0.007 FVAR 2 3 0.48426 0.09221 -0.011 FVAR 3 4 0.30321 0.02149 -0.130 FVAR 4 5 0.20578 0.02101 -0.044 FVAR 5 6 0.20332 0.02155 -0.032 FVAR 6 7 0.29847 0.02768 0.148 FVAR 7 8 0.55664 0.04209 0.003 FVAR 8 Mean shift/esd = 0.028 Maximum = 0.295 for U23 F8D_d Max. shift = 0.008 A for F8D_d Max. dU = 0.003 for F7C_c Least-squares cycle 7 Maximum vector length = 511 Memory required = 5407 / 680655 wR2 = 0.1300 before cycle 7 for 4389 data and 512 / 512 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint 0.0733 0.0200 SAME/SADI C17B_b F8B_b C17B_b F9B_b etc. Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 976. 0. 0. 0. 0. 0. 0. 1. rms sigma 0.000 0.000 0.000 0.024 0.000 0.000 0.000 0.000 0.000 0.000 0.005 rms deviation 0.000 0.000 0.000 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.011 GooF = S = 1.036; Restrained GooF = 1.007 for 977 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0686 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08901 0.00021 0.005 OSF 2 0.41700 0.08633 0.005 FVAR 2 3 0.48368 0.09201 -0.006 FVAR 3 4 0.30058 0.02151 -0.122 FVAR 4 5 0.20586 0.02083 0.004 FVAR 5 6 0.20207 0.02137 -0.058 FVAR 6 7 0.30230 0.02767 0.138 FVAR 7 8 0.55675 0.04208 0.003 FVAR 8 Mean shift/esd = 0.020 Maximum = 0.271 for z F7A_a Max. shift = 0.008 A for F8D_d Max. dU = 0.002 for F9B_b Least-squares cycle 8 Maximum vector length = 511 Memory required = 5407 / 680655 wR2 = 0.1300 before cycle 8 for 4389 data and 512 / 512 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint 0.0727 0.0200 SAME/SADI C17B_b F8B_b C17B_b F9B_b etc. Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 976. 0. 0. 0. 0. 0. 0. 1. rms sigma 0.000 0.000 0.000 0.024 0.000 0.000 0.000 0.000 0.000 0.000 0.005 rms deviation 0.000 0.000 0.000 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.011 GooF = S = 1.036; Restrained GooF = 1.006 for 977 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0686 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08901 0.00021 0.000 OSF 2 0.41731 0.08621 0.004 FVAR 2 3 0.48345 0.09200 -0.002 FVAR 3 4 0.29945 0.02149 -0.052 FVAR 4 5 0.20618 0.02077 0.015 FVAR 5 6 0.20157 0.02121 -0.024 FVAR 6 7 0.30339 0.02763 0.040 FVAR 7 8 0.55662 0.04204 -0.003 FVAR 8 Mean shift/esd = 0.016 Maximum = -0.209 for z F8B_b Max. shift = 0.006 A for F8D_d Max. dU = 0.002 for F7C_c Least-squares cycle 9 Maximum vector length = 511 Memory required = 5407 / 680655 wR2 = 0.1300 before cycle 9 for 4389 data and 512 / 512 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint 0.0725 0.0200 SAME/SADI C17B_b F8B_b C17B_b F9B_b etc. Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 976. 0. 0. 0. 0. 0. 0. 1. rms sigma 0.000 0.000 0.000 0.024 0.000 0.000 0.000 0.000 0.000 0.000 0.005 rms deviation 0.000 0.000 0.000 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.011 GooF = S = 1.036; Restrained GooF = 1.006 for 977 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0686 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08901 0.00021 0.003 OSF 2 0.41743 0.08621 0.001 FVAR 2 3 0.48330 0.09201 -0.002 FVAR 3 4 0.29828 0.02151 -0.055 FVAR 4 5 0.20667 0.02063 0.024 FVAR 5 6 0.20033 0.02114 -0.059 FVAR 6 7 0.30532 0.02758 0.070 FVAR 7 8 0.55654 0.04204 -0.002 FVAR 8 Mean shift/esd = 0.011 Maximum = 0.157 for z F7A_a Max. shift = 0.005 A for F8D_d Max. dU =-0.001 for F8C_c Least-squares cycle 10 Maximum vector length = 511 Memory required = 5407 / 680655 wR2 = 0.1300 before cycle 10 for 4389 data and 512 / 512 parameters Disagreeable restraints before cycle 10 Observed Target Error Sigma Restraint 0.0725 0.0200 SAME/SADI C17B_b F8B_b C17B_b F9B_b etc. Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 976. 0. 0. 0. 0. 0. 0. 1. rms sigma 0.000 0.000 0.000 0.024 0.000 0.000 0.000 0.000 0.000 0.000 0.005 rms deviation 0.000 0.000 0.000 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.011 GooF = S = 1.036; Restrained GooF = 1.006 for 977 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0686 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08901 0.00021 -0.001 OSF 2 0.41755 0.08618 0.001 FVAR 2 3 0.48329 0.09198 0.000 FVAR 3 4 0.29781 0.02149 -0.022 FVAR 4 5 0.20722 0.02063 0.026 FVAR 5 6 0.19978 0.02107 -0.026 FVAR 6 7 0.30580 0.02757 0.018 FVAR 7 8 0.55643 0.04202 -0.003 FVAR 8 Mean shift/esd = 0.009 Maximum = -0.112 for x F7D_d Max. shift = 0.004 A for F8D_d Max. dU = 0.001 for F7C_c Least-squares cycle 11 Maximum vector length = 511 Memory required = 5407 / 680655 wR2 = 0.1300 before cycle 11 for 4389 data and 512 / 512 parameters Disagreeable restraints before cycle 11 Observed Target Error Sigma Restraint 0.0725 0.0200 SAME/SADI C17B_b F8B_b C17B_b F9B_b etc. Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 976. 0. 0. 0. 0. 0. 0. 1. rms sigma 0.000 0.000 0.000 0.024 0.000 0.000 0.000 0.000 0.000 0.000 0.005 rms deviation 0.000 0.000 0.000 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.011 GooF = S = 1.036; Restrained GooF = 1.006 for 977 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0686 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08901 0.00021 0.003 OSF 2 0.41758 0.08622 0.000 FVAR 2 3 0.48338 0.09193 0.001 FVAR 3 4 0.29729 0.02150 -0.024 FVAR 4 5 0.20756 0.02057 0.016 FVAR 5 6 0.19901 0.02102 -0.037 FVAR 6 7 0.30673 0.02756 0.034 FVAR 7 8 0.55640 0.04202 -0.001 FVAR 8 Mean shift/esd = 0.006 Maximum = -0.078 for x F8D_d Max. shift = 0.003 A for F8D_d Max. dU = 0.000 for F8C_c Least-squares cycle 12 Maximum vector length = 511 Memory required = 5407 / 680655 wR2 = 0.1300 before cycle 12 for 4389 data and 512 / 512 parameters Disagreeable restraints before cycle 12 Observed Target Error Sigma Restraint 0.0725 0.0200 SAME/SADI C17B_b F8B_b C17B_b F9B_b etc. Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 976. 0. 0. 0. 0. 0. 0. 1. rms sigma 0.000 0.000 0.000 0.024 0.000 0.000 0.000 0.000 0.000 0.000 0.005 rms deviation 0.000 0.000 0.000 0.018 0.000 0.000 0.000 0.000 0.000 0.000 0.011 GooF = S = 1.036; Restrained GooF = 1.006 for 977 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0686 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08901 0.00021 0.001 OSF 2 0.41763 0.08623 0.001 FVAR 2 3 0.48347 0.09196 0.001 FVAR 3 4 0.29712 0.02150 -0.008 FVAR 4 5 0.20794 0.02057 0.019 FVAR 5 6 0.19863 0.02099 -0.018 FVAR 6 7 0.30691 0.02755 0.006 FVAR 7 8 0.55636 0.04200 -0.001 FVAR 8 Mean shift/esd = 0.005 Maximum = -0.065 for x F7D_d Max. shift = 0.002 A for F8D_d Max. dU = 0.001 for F7C_c Largest correlation matrix elements -0.938 U11 F10'_b / U11 F10_a 0.862 z F5'_b / U33 F5_a -0.811 U33 F3'_b / U33 F3_a -0.922 z F3'_b / z F3_a -0.862 U11 F3'_b / U11 F3_a 0.811 U11 F1_a / FVAR 2 -0.905 z F1'_b / z F1_a -0.853 U22 F12'_b / y F12_a -0.810 x F1'_b / FVAR 2 -0.904 x F12'_b / x F12_a -0.850 U11 F12'_b / U11 F12_a -0.806 U33 F1'_b / U33 F1_a -0.900 x F10'_b / x F10_a 0.843 y F3'_b / FVAR 2 -0.803 y F5'_b / y F5_a -0.894 U11 F11'_b / FVAR 8 0.822 U11 F5'_b / x F5'_b 0.800 x F5_a / y F4_a -0.887 x F11_a / FVAR 8 -0.819 U11 F1'_b / x F1_a 0.798 x F11'_b / U11 F11_a -0.869 y F2'_b / y F2_a -0.817 y F3'_b / x F1'_b -0.798 y F4'_b / x F4'_b Idealized hydrogen atom generation before cycle 13 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.5154 0.1262 0.6995 43 0.950 0.000 C1 C2 C6 H3A 0.3338 0.0398 0.8409 43 0.950 0.000 C3 C4 C2 H5A 0.4850 0.1557 1.1145 43 0.950 0.000 C5 C4 C6 H1B 0.5975 0.2045 0.8490 43 0.880 0.000 N1 C9 C6 H10A 0.6855 0.2961 0.9348 23 0.990 0.000 C10 C9 Cl1 H10B 0.7176 0.1928 1.0158 23 0.990 0.000 C10 C9 Cl1 H11A 0.9770 0.3509 0.8326 43 0.950 0.000 C11 C16 C12 H13A 0.8291 0.4782 1.0599 43 0.950 0.000 C13 C14 C12 H15A 1.0025 0.3588 1.2585 43 0.950 0.000 C15 C14 C16 H2A 1.0828 0.2776 1.1340 43 0.880 0.000 N2 C19 C16 H20A 1.1663 0.1438 0.9839 23 0.990 0.000 C20 C19 Cl2 H20B 1.1856 0.2431 1.0866 23 0.990 0.000 C20 C19 Cl2 UDel6 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.48685 0.11894 0.77499 1.00000 0.02983 0.02890 0.02312 -0.00007 0.00775 -0.00017 0.02699 0.00350 0.00010 0.00016 0.00020 0.00000 0.00094 0.00093 0.00090 0.00073 0.00071 0.00074 0.00039 H1A 0.51543 0.12620 0.69953 1.00000 0.03239 0.00000 0.00000 C2 0.42166 0.07881 0.74988 1.00000 0.03180 0.02746 0.02596 -0.00165 0.00345 -0.00013 0.02834 0.00351 0.00010 0.00016 0.00021 0.00000 0.00098 0.00092 0.00095 0.00076 0.00074 0.00075 0.00040 C3 0.37874 0.06717 0.85839 1.00000 0.02644 0.02782 0.03382 -0.00031 0.00504 -0.00068 0.02922 0.00362 0.00010 0.00016 0.00022 0.00000 0.00092 0.00093 0.00102 0.00079 0.00076 0.00073 0.00041 H3A 0.33377 0.03977 0.84088 1.00000 0.03507 0.00000 0.00000 C4 0.40352 0.09671 0.99271 1.00000 0.02781 0.02614 0.03026 0.00154 0.00856 0.00277 0.02775 0.00362 0.00010 0.00015 0.00021 0.00000 0.00091 0.00090 0.00100 0.00076 0.00076 0.00072 0.00040 C5 0.46903 0.13682 1.02127 1.00000 0.02868 0.02755 0.02348 -0.00056 0.00697 0.00071 0.02632 0.00350 0.00010 0.00015 0.00020 0.00000 0.00092 0.00088 0.00090 0.00073 0.00072 0.00073 0.00038 H5A 0.48501 0.15571 1.11454 1.00000 0.03158 0.00000 0.00000 C6 0.51103 0.14893 0.91061 1.00000 0.02684 0.02405 0.02562 0.00038 0.00578 0.00064 0.02531 0.00340 0.00010 0.00015 0.00020 0.00000 0.00090 0.00088 0.00092 0.00072 0.00072 0.00069 0.00039 C7_a 0.39795 0.04579 0.60318 0.41763 0.03781 0.04192 0.03194 -0.00577 0.00161 -0.00662 0.03727 0.00382 0.00011 0.00019 0.00023 0.08623 0.00115 0.00121 0.00109 0.00093 0.00088 0.00091 0.00049 F1_a 0.43241 -0.04171 0.56360 0.41763 0.05235 0.05871 0.04871 -0.03025 0.01216 0.00212 0.05283 0.03911 0.00109 0.00120 0.00194 0.08623 0.00562 0.00719 0.00520 0.00485 0.00344 0.00327 0.00325 F2_a 0.40687 0.11961 0.50552 0.41763 0.09203 0.04296 0.03461 -0.00292 -0.02317 -0.00744 0.05795 0.04362 0.00155 0.00091 0.00173 0.08623 0.00749 0.00512 0.00484 0.00334 0.00446 0.00418 0.00350 F3_a 0.33260 0.01703 0.58866 0.41763 0.03951 0.11963 0.05899 -0.05428 0.01550 -0.03264 0.07212 0.02867 0.00052 0.00245 0.00178 0.08623 0.00454 0.00798 0.00713 0.00739 0.00521 0.00501 0.00411 C7'_b 0.39795 0.04579 0.60318 0.58237 0.03781 0.04192 0.03194 -0.00577 0.00161 -0.00662 0.03727 0.00382 0.00011 0.00019 0.00023 0.08623 0.00115 0.00121 0.00109 0.00093 0.00088 0.00091 0.00049 F1'_b 0.42330 -0.04812 0.56676 0.58237 0.09128 0.03463 0.04036 -0.00995 -0.00421 -0.00168 0.05589 0.03228 0.00107 0.00084 0.00130 0.08623 0.00641 0.00339 0.00349 0.00259 0.00355 0.00286 0.00240 F2'_b 0.41780 0.11784 0.51170 0.58237 0.08318 0.06593 0.02159 0.00734 -0.00386 -0.02625 0.05730 0.03106 0.00113 0.00081 0.00122 0.08623 0.00474 0.00475 0.00295 0.00240 0.00314 0.00316 0.00252 F3'_b 0.33063 0.03800 0.58659 0.58237 0.04150 0.11541 0.04490 -0.01222 -0.01405 -0.00715 0.06815 0.02780 0.00035 0.00206 0.00114 0.08623 0.00327 0.00622 0.00400 0.00445 0.00314 0.00320 0.00286 C8_a 0.35873 0.08751 1.11378 0.48347 0.02915 0.03715 0.03467 0.00308 0.01168 0.00094 0.03318 0.00389 0.00010 0.00017 0.00022 0.09196 0.00100 0.00110 0.00108 0.00089 0.00084 0.00083 0.00045 F4_a 0.29839 0.04430 1.07495 0.48347 0.02396 0.08007 0.05795 0.01477 0.01406 -0.01431 0.05344 0.02077 0.00073 0.00244 0.00181 0.09196 0.00340 0.00666 0.00509 0.00367 0.00233 0.00313 0.00310 F5_a 0.34641 0.18478 1.16732 0.48347 0.06336 0.03888 0.07708 -0.00953 0.04887 0.00027 0.05757 0.04698 0.00155 0.00088 0.00272 0.09196 0.00734 0.00438 0.00869 0.00424 0.00545 0.00345 0.00366 F6_a 0.38691 0.02932 1.21833 0.48347 0.03673 0.05026 0.04779 0.00601 0.01654 0.00706 0.04425 0.04750 0.00086 0.00187 0.00157 0.09196 0.00363 0.00413 0.00618 0.00282 0.00286 0.00294 0.00260 C8'_b 0.35873 0.08751 1.11378 0.51653 0.02915 0.03715 0.03467 0.00308 0.01168 0.00094 0.03318 0.00389 0.00010 0.00017 0.00022 0.09196 0.00100 0.00110 0.00108 0.00089 0.00084 0.00083 0.00045 F4'_b 0.30388 0.02506 1.08323 0.51653 0.04534 0.07330 0.03745 0.00255 0.01102 -0.02026 0.05163 0.01493 0.00087 0.00216 0.00165 0.09196 0.00467 0.00562 0.00367 0.00337 0.00242 0.00353 0.00283 F5'_b 0.33585 0.18187 1.15419 0.51653 0.05073 0.05697 0.05008 0.00153 0.02878 0.01918 0.05133 0.04263 0.00135 0.00099 0.00223 0.09196 0.00486 0.00527 0.00416 0.00341 0.00361 0.00400 0.00297 F6'_b 0.39196 0.04284 1.22711 0.51653 0.04638 0.06931 0.01573 0.01106 0.00944 -0.00003 0.04345 0.04118 0.00078 0.00173 0.00119 0.09196 0.00374 0.00587 0.00380 0.00257 0.00206 0.00312 0.00253 N1 0.57785 0.19153 0.92714 1.00000 0.02786 0.03527 0.01730 -0.00012 0.00789 -0.00418 0.02650 0.00287 0.00008 0.00014 0.00016 0.00000 0.00079 0.00085 0.00074 0.00063 0.00059 0.00065 0.00035 H1B 0.59754 0.20454 0.84901 1.00000 0.03180 0.00000 0.00000 C9 0.61510 0.21467 1.04784 1.00000 0.02814 0.02515 0.01997 -0.00189 0.00607 0.00102 0.02421 0.00334 0.00010 0.00015 0.00019 0.00000 0.00091 0.00087 0.00088 0.00069 0.00069 0.00069 0.00038 O1 0.59585 0.20203 1.16512 1.00000 0.03368 0.04524 0.02113 -0.00412 0.00759 -0.00792 0.03307 0.00250 0.00007 0.00013 0.00014 0.00000 0.00073 0.00083 0.00069 0.00059 0.00054 0.00062 0.00033 C10 0.68666 0.25493 1.02391 1.00000 0.02873 0.04208 0.02540 -0.00391 0.00789 -0.00388 0.03178 0.00366 0.00010 0.00018 0.00021 0.00000 0.00097 0.00112 0.00098 0.00083 0.00075 0.00082 0.00044 H10A 0.68546 0.29606 0.93483 1.00000 0.03813 0.00000 0.00000 H10B 0.71763 0.19275 1.01582 1.00000 0.03813 0.00000 0.00000 Cl1 0.71781 0.33781 1.16434 1.00000 0.04152 0.05376 0.03061 -0.00558 0.00353 -0.01856 0.04192 0.00089 0.00003 0.00005 0.00005 0.00000 0.00030 0.00035 0.00028 0.00022 0.00021 0.00023 0.00018 C11 0.96090 0.36857 0.92126 1.00000 0.03108 0.03298 0.02603 -0.00030 0.00822 -0.00202 0.02972 0.00365 0.00010 0.00017 0.00021 0.00000 0.00098 0.00099 0.00094 0.00079 0.00076 0.00079 0.00041 H11A 0.97697 0.35087 0.83264 1.00000 0.03567 0.00000 0.00000 C12 0.89746 0.41722 0.92918 1.00000 0.02772 0.03563 0.03442 0.00212 0.00662 -0.00324 0.03237 0.00380 0.00010 0.00017 0.00023 0.00000 0.00096 0.00105 0.00109 0.00086 0.00080 0.00080 0.00044 C13 0.87245 0.44498 1.05634 1.00000 0.02934 0.03086 0.04110 0.00265 0.01202 0.00009 0.03329 0.00397 0.00011 0.00017 0.00024 0.00000 0.00098 0.00101 0.00116 0.00085 0.00084 0.00078 0.00045 H13A 0.82909 0.47824 1.05987 1.00000 0.03995 0.00000 0.00000 C14 0.91273 0.42263 1.17759 1.00000 0.03659 0.02939 0.03262 -0.00070 0.01533 -0.00206 0.03222 0.00388 0.00011 0.00017 0.00022 0.00000 0.00107 0.00098 0.00106 0.00082 0.00084 0.00081 0.00044 C15 0.97582 0.37370 1.17341 1.00000 0.03479 0.02998 0.02655 0.00004 0.00923 0.00036 0.03009 0.00372 0.00011 0.00016 0.00021 0.00000 0.00101 0.00098 0.00096 0.00077 0.00078 0.00079 0.00042 H15A 1.00248 0.35876 1.25846 1.00000 0.03611 0.00000 0.00000 C16 1.00030 0.34632 1.04493 1.00000 0.02962 0.02661 0.02625 0.00018 0.00927 -0.00222 0.02713 0.00352 0.00010 0.00015 0.00021 0.00000 0.00095 0.00092 0.00093 0.00073 0.00075 0.00072 0.00040 C17A_a 0.85503 0.43944 0.79466 0.29712 0.03412 0.06120 0.04165 0.00616 0.00139 0.00277 0.04573 0.00460 0.00012 0.00022 0.00026 0.02150 0.00120 0.00166 0.00133 0.00117 0.00098 0.00111 0.00061 F7A_a 0.78848 0.43494 0.80786 0.29712 0.02415 0.11156 0.04380 -0.01990 -0.00041 0.00704 0.05999 0.02584 0.00051 0.00188 0.00173 0.02150 0.00441 0.01538 0.00586 0.01039 0.00341 0.00682 0.00622 F8A_a 0.86609 0.36131 0.69826 0.29712 0.03210 0.08585 0.02567 -0.02150 -0.00434 0.01806 0.04820 0.02404 0.00077 0.00115 0.00134 0.02150 0.00761 0.00888 0.00422 0.00362 0.00420 0.00560 0.00420 F9A_a 0.86849 0.53042 0.73181 0.29712 0.11584 0.07683 0.06626 0.05591 -0.02849 -0.01981 0.08810 0.03169 0.00120 0.00116 0.00225 0.02150 0.01927 0.01032 0.01394 0.01062 0.01085 0.01146 0.00950 C17B_b 0.85503 0.43944 0.79466 0.20794 0.03412 0.06120 0.04165 0.00616 0.00139 0.00277 0.04573 0.00460 0.00012 0.00022 0.00026 0.02057 0.00120 0.00166 0.00133 0.00117 0.00098 0.00111 0.00061 F7B_b 0.89281 0.47135 0.69194 0.20794 0.03697 0.10342 0.00791 -0.01842 -0.00948 0.00051 0.05000 0.04106 0.00072 0.00215 0.00159 0.02057 0.00662 0.01674 0.00593 0.00783 0.00412 0.00920 0.00618 F8B_b 0.81519 0.52810 0.81465 0.20794 0.04371 0.06168 0.04347 0.03062 0.02916 0.03030 0.04831 0.04409 0.00109 0.00138 0.00201 0.02057 0.01030 0.01278 0.00690 0.00632 0.00607 0.00885 0.00650 F9B_b 0.81348 0.36498 0.74457 0.20794 0.06454 0.10736 0.18991 0.04471 -0.09219 -0.03218 0.12575 0.02897 0.00139 0.00151 0.00351 0.02057 0.01914 0.01723 0.03293 0.01774 0.02203 0.01473 0.01606 C17C_c 0.85503 0.43944 0.79466 0.19863 0.03412 0.06120 0.04165 0.00616 0.00139 0.00277 0.04573 0.00460 0.00012 0.00022 0.00026 0.02099 0.00120 0.00166 0.00133 0.00117 0.00098 0.00111 0.00061 F7C_c 0.88202 0.41829 0.67461 0.19863 0.04316 0.44717 0.03033 -0.06058 -0.00457 -0.00798 0.17393 0.05444 0.00118 0.00318 0.00196 0.02099 0.01019 0.06888 0.00912 0.02398 0.00759 0.02641 0.02380 F8C_c 0.83564 0.54385 0.78608 0.19863 0.12450 0.05653 0.02960 0.03287 -0.02253 -0.04815 0.07164 0.02530 0.00128 0.00083 0.00199 0.02099 0.02238 0.00830 0.01114 0.00848 0.01236 0.01367 0.01015 F9C_c 0.79658 0.38538 0.79093 0.19863 0.07154 0.04983 0.07866 0.00063 -0.02402 -0.03108 0.06818 0.03328 0.00102 0.00166 0.00290 0.02099 0.01792 0.01159 0.01513 0.00979 0.01273 0.01019 0.00883 C17D_d 0.85503 0.43944 0.79466 0.30691 0.03412 0.06120 0.04165 0.00616 0.00139 0.00277 0.04573 0.00460 0.00012 0.00022 0.00026 0.02755 0.00120 0.00166 0.00133 0.00117 0.00098 0.00111 0.00061 F7D_d 0.88752 0.50959 0.71877 0.30691 0.07933 0.05438 0.02654 0.00314 -0.01363 -0.02118 0.05431 0.03027 0.00114 0.00155 0.00201 0.02755 0.00972 0.00854 0.00696 0.00563 0.00584 0.00706 0.00526 F8D_d 0.79561 0.48234 0.81845 0.30691 0.04279 0.32013 0.09144 0.09097 0.02351 0.07076 0.15052 0.06377 0.00103 0.00297 0.00305 0.02755 0.01189 0.04227 0.01539 0.01906 0.00845 0.01766 0.01539 F9D_d 0.84420 0.35380 0.71500 0.30691 0.05509 0.06333 0.10872 0.01053 -0.06721 -0.02616 0.07943 0.02100 0.00119 0.00095 0.00210 0.02755 0.01604 0.00667 0.01287 0.00697 0.01064 0.00811 0.00815 C18_a 0.88883 0.44873 1.31998 0.55636 0.04472 0.04072 0.03693 -0.00324 0.01811 0.00506 0.04003 0.00440 0.00012 0.00018 0.00024 0.04200 0.00128 0.00120 0.00117 0.00096 0.00098 0.00098 0.00052 F10_a 0.83029 0.49829 1.31808 0.55636 0.04154 0.09244 0.07797 -0.03743 0.02864 -0.00274 0.06943 0.02247 0.00045 0.00110 0.00153 0.04200 0.00446 0.00650 0.00637 0.00430 0.00372 0.00346 0.00334 F11_a 0.88660 0.36327 1.40391 0.55636 0.20053 0.04718 0.06402 0.01777 0.08661 0.03736 0.10003 0.04209 0.00117 0.00065 0.00176 0.04200 0.00995 0.00315 0.00516 0.00281 0.00594 0.00416 0.00372 F12_a 0.93483 0.51487 1.38915 0.55636 0.04944 0.07023 0.02782 -0.00932 0.00912 0.00936 0.04885 0.01305 0.00050 0.00095 0.00147 0.04200 0.00330 0.00366 0.00289 0.00226 0.00201 0.00213 0.00202 C18'_b 0.88883 0.44873 1.31998 0.44364 0.04472 0.04072 0.03693 -0.00324 0.01811 0.00506 0.04003 0.00440 0.00012 0.00018 0.00024 0.04200 0.00128 0.00120 0.00117 0.00096 0.00098 0.00098 0.00052 F10'_b 0.83175 0.50813 1.30840 0.44364 0.04079 0.04013 0.03423 -0.00647 0.01271 0.01610 0.03788 0.02253 0.00050 0.00085 0.00126 0.04200 0.00489 0.00370 0.00382 0.00279 0.00301 0.00283 0.00253 F11'_b 0.87098 0.35813 1.38218 0.44364 0.07049 0.06101 0.03366 0.00867 0.02862 0.00391 0.05380 0.02163 0.00056 0.00075 0.00133 0.04200 0.00584 0.00409 0.00317 0.00228 0.00314 0.00266 0.00257 F12'_b 0.93297 0.49871 1.40699 0.44364 0.04218 0.14166 0.03399 -0.02579 0.00795 -0.00998 0.07236 0.01638 0.00067 0.00132 0.00198 0.04200 0.00394 0.01141 0.00473 0.00580 0.00271 0.00484 0.00452 N2 1.06538 0.29710 1.05005 1.00000 0.03092 0.03591 0.01934 0.00180 0.00652 0.00498 0.02849 0.00309 0.00008 0.00014 0.00017 0.00000 0.00083 0.00088 0.00076 0.00065 0.00061 0.00069 0.00036 H2A 1.08278 0.27763 1.13397 1.00000 0.03418 0.00000 0.00000 C19 1.10391 0.27641 0.94253 1.00000 0.03074 0.02762 0.01961 -0.00178 0.00672 -0.00190 0.02575 0.00337 0.00010 0.00015 0.00020 0.00000 0.00093 0.00092 0.00091 0.00071 0.00070 0.00073 0.00039 O2 1.08667 0.29637 0.81969 1.00000 0.03319 0.04887 0.01995 -0.00180 0.00632 0.00492 0.03378 0.00269 0.00007 0.00013 0.00014 0.00000 0.00073 0.00088 0.00069 0.00060 0.00054 0.00063 0.00034 C20 1.17163 0.22301 0.98813 1.00000 0.03386 0.04919 0.02499 0.00560 0.01038 0.00864 0.03560 0.00432 0.00011 0.00020 0.00022 0.00000 0.00105 0.00126 0.00099 0.00089 0.00080 0.00090 0.00048 H20A 1.16630 0.14381 0.98388 1.00000 0.04272 0.00000 0.00000 H20B 1.18555 0.24313 1.08659 1.00000 0.04272 0.00000 0.00000 Cl2 1.23510 0.26300 0.87866 1.00000 0.03074 0.09335 0.05778 0.03294 0.01471 0.00702 0.06005 0.00149 0.00003 0.00007 0.00007 0.00000 0.00030 0.00054 0.00041 0.00036 0.00026 0.00029 0.00023 Final Structure Factor Calculation for UDel6 in P2(1)/c Total number of l.s. parameters = 512 Maximum vector length = 511 Memory required = 4895 / 25039 wR2 = 0.1300 before cycle 13 for 4389 data and 0 / 512 parameters Disagreeable restraints before cycle 13 Observed Target Error Sigma Restraint 0.0725 0.0200 SAME/SADI C17B_b F8B_b C17B_b F9B_b etc. Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 976. 0. 0. 0. 0. 0. 0. 1. rms sigma 0.000 0.000 0.000 0.024 0.000 0.000 0.000 0.000 0.000 0.000 0.005 rms deviation 0.000 0.000 0.000 0.018 0.000 0.000 0.000 0.000 0.000 0.000 0.011 GooF = S = 1.036; Restrained GooF = 1.006 for 977 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0686 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0479 for 4139 Fo > 4sig(Fo) and 0.0495 for all 4389 data wR2 = 0.1300, GooF = S = 1.036, Restrained GooF = 1.006 for all data Occupancy sum of asymmetric unit = 38.04 for non-hydrogen and 12.00 for hydrogen atoms Principal mean square atomic displacements U 0.0327 0.0289 0.0193 C1 0.0320 0.0283 0.0247 C2 0.0346 0.0279 0.0252 C3 0.0359 0.0257 0.0217 C4 0.0314 0.0276 0.0199 C5 0.0299 0.0240 0.0221 C6 0.0477 0.0362 0.0280 C7_a 0.0845 0.0538 0.0202 F1_a 0.1062 0.0439 0.0238 F2_a 0.1591 0.0337 0.0236 F3_a 0.0477 0.0362 0.0280 C7'_b 0.0937 0.0473 0.0267 F1'_b 0.1045 0.0470 0.0204 F2'_b 0.1176 0.0617 0.0251 F3'_b 0.0425 0.0356 0.0214 C8_a 0.0890 0.0570 0.0143 F4_a 0.1119 0.0407 0.0201 F5_a 0.0621 0.0442 0.0264 F6_a 0.0425 0.0356 0.0214 C8'_b 0.0839 0.0442 0.0268 F4'_b 0.0825 0.0529 0.0186 F5'_b 0.0715 0.0473 0.0115 F6'_b 0.0374 0.0283 0.0138 N1 0.0297 0.0257 0.0172 C9 0.0503 0.0304 0.0186 O1 0.0445 0.0304 0.0205 C10 0.0675 0.0315 0.0268 Cl1 0.0358 0.0319 0.0214 C11 0.0372 0.0359 0.0239 C12 0.0460 0.0307 0.0232 C13 0.0468 0.0293 0.0206 C14 0.0382 0.0300 0.0221 C15 0.0351 0.0267 0.0196 C16 0.0631 0.0407 0.0334 C17A_a 0.1179 0.0385 0.0236 F7A_a 0.0992 0.0266 0.0188 F8A_a 0.1652 0.0845 0.0146 F9A_a 0.0631 0.0407 0.0334 C17B_b 0.1071 0.0410 0.0020 F7B_b 0.1063 0.0230 0.0156 F8B_b 0.2744 0.0887 0.0142 F9B_b may be split into 0.8094 0.3706 0.7636 and 0.8176 0.3594 0.7256 0.0631 0.0407 0.0334 C17C_c 0.4558 0.0464 0.0196 F7C_c may be split into 0.8816 0.4438 0.6699 and 0.8825 0.3928 0.6793 0.1653 0.0428 0.0068 F8C_c 0.1157 0.0654 0.0235 F9C_c 0.0631 0.0407 0.0334 C17D_d 0.0971 0.0437 0.0222 F7D_d 0.3653 0.0605 0.0258 F8D_d may be split into 0.7991 0.5029 0.8273 and 0.7922 0.4618 0.8096 0.1717 0.0618 0.0047 F9D_d 0.0556 0.0423 0.0222 C18_a 0.1258 0.0596 0.0229 F10_a 0.2380 0.0387 0.0234 F11_a may be split into 0.8972 0.3670 1.4125 and 0.8760 0.3596 1.3953 0.0750 0.0489 0.0226 F12_a 0.0556 0.0423 0.0222 C18'_b 0.0567 0.0414 0.0156 F10'_b 0.0834 0.0596 0.0184 F11'_b 0.1483 0.0415 0.0272 F12'_b 0.0396 0.0286 0.0173 N2 0.0332 0.0267 0.0173 C19 0.0503 0.0331 0.0179 O2 0.0551 0.0323 0.0195 C20 0.1140 0.0413 0.0248 Cl2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.012 0.019 0.026 0.034 0.043 0.055 0.074 0.108 1.000 Number in group 486. 401. 454. 455. 443. 394. 463. 422. 439. 432. GooF 0.992 0.971 1.130 1.005 1.001 1.031 0.983 1.019 1.069 1.144 K 1.580 1.084 1.049 1.022 1.011 1.005 1.011 1.006 1.003 1.021 Resolution(A) 0.81 0.85 0.88 0.92 0.97 1.03 1.11 1.22 1.40 1.75 inf Number in group 451. 445. 420. 453. 428. 436. 442. 436. 439. 439. GooF 1.001 0.958 0.920 0.991 0.901 0.813 0.895 0.893 1.223 1.550 K 1.014 1.027 1.024 1.027 0.997 0.997 0.988 0.991 0.996 1.035 R1 0.080 0.071 0.060 0.057 0.046 0.038 0.038 0.041 0.046 0.051 Recommended weighting scheme: WGHT 0.0733 1.6868 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) -6 0 10 112.81 35.33 6.06 0.017 0.93 0 0 8 1028.62 1898.53 6.00 0.127 1.19 6 2 1 27.99 0.83 5.34 0.003 2.72 -3 0 4 1459.98 889.92 5.09 0.087 2.29 -4 1 2 110.77 44.19 4.91 0.019 3.41 -1 3 2 46.07 109.50 4.57 0.031 3.11 0 2 3 632.50 408.77 4.41 0.059 2.82 -1 4 3 63.17 22.76 4.40 0.014 2.22 -1 2 3 895.73 590.07 4.29 0.071 2.82 -5 7 1 3376.15 5266.61 4.18 0.212 1.60 1 1 4 341.69 200.11 4.14 0.041 2.30 -7 2 5 189.61 318.62 4.14 0.052 1.58 -3 3 11 51.56 13.32 4.09 0.011 0.85 -1 2 5 73.22 138.18 3.90 0.034 1.82 7 3 0 335.27 550.66 3.84 0.069 2.32 4 3 0 3426.35 2448.39 3.76 0.145 3.16 2 3 3 2183.92 1435.47 3.75 0.111 2.40 0 8 0 81.13 37.28 3.74 0.018 1.55 -6 4 3 265.93 405.14 3.68 0.059 1.88 -5 1 4 163.78 98.26 3.67 0.029 2.07 -4 0 2 722.29 495.91 3.58 0.065 3.55 -5 6 1 849.40 1266.48 3.51 0.104 1.81 -6 3 9 98.86 167.20 3.47 0.038 1.00 -2 2 10 52.48 22.93 3.47 0.014 0.94 1 1 2 112.75 62.24 3.40 0.023 4.27 1 2 11 43.17 17.18 3.38 0.012 0.85 4 2 4 1055.41 1435.09 3.36 0.111 1.97 -9 2 10 20.45 3.27 3.36 0.005 0.89 7 2 6 555.29 769.88 3.34 0.081 1.31 2 1 2 1244.26 1725.30 3.34 0.121 3.94 10 1 0 434.23 311.12 3.33 0.052 1.94 -7 1 11 186.05 118.62 3.32 0.032 0.84 10 1 2 56.76 27.84 3.29 0.015 1.75 4 6 8 10.24 0.08 3.25 0.001 1.00 -13 0 10 142.62 78.31 3.23 0.026 0.83 2 6 1 484.75 344.79 3.21 0.054 1.98 4 4 1 2895.29 2212.39 3.20 0.137 2.50 -3 8 2 773.67 1086.73 3.17 0.096 1.45 3 7 1 6569.75 4855.07 3.15 0.204 1.68 -8 2 4 10.18 31.25 3.15 0.016 1.71 10 3 10 20.19 49.79 3.15 0.021 0.81 4 6 0 1367.01 1022.04 3.15 0.093 1.91 5 1 4 684.97 506.57 3.13 0.066 1.94 -6 2 11 84.47 41.22 3.11 0.019 0.84 -6 7 8 186.80 125.07 3.09 0.033 0.96 7 0 6 480.21 653.34 3.08 0.075 1.34 4 5 2 68.15 118.88 3.07 0.032 1.98 2 0 0 1907.05 1250.77 3.04 0.103 9.80 -2 0 4 982.04 702.37 3.03 0.077 2.35 5 2 9 236.92 336.33 3.02 0.054 0.99 Bond lengths and angles C1 - Distance Angles C2 1.3788 (0.0028) C6 1.3944 (0.0028) 120.32 (0.17) H1A 0.9500 119.84 119.84 C1 - C2 C6 C2 - Distance Angles C1 1.3788 (0.0028) C3 1.3909 (0.0028) 121.07 (0.18) C7_a 1.4980 (0.0029) 118.73 (0.18) 120.19 (0.19) C2 - C1 C3 C3 - Distance Angles C4 1.3850 (0.0030) C2 1.3909 (0.0028) 118.02 (0.18) H3A 0.9500 120.99 120.99 C3 - C4 C2 C4 - Distance Angles C3 1.3850 (0.0029) C5 1.3883 (0.0028) 122.18 (0.18) C8_a 1.5080 (0.0026) 120.21 (0.18) 117.60 (0.18) C4 - C3 C5 C5 - Distance Angles C4 1.3883 (0.0028) C6 1.3960 (0.0026) 118.88 (0.18) H5A 0.9500 120.56 120.56 C5 - C4 C6 C6 - Distance Angles C1 1.3944 (0.0028) C5 1.3960 (0.0026) 119.52 (0.18) N1 1.4135 (0.0025) 116.88 (0.16) 123.60 (0.17) C6 - C1 C5 C7_a - Distance Angles F2_a 1.3280 (0.0096) F3_a 1.3303 (0.0093) 106.86 (0.89) F1_a 1.3495 (0.0090) 105.35 (0.78) 104.80 (0.89) C2 1.4980 (0.0029) 114.68 (0.94) 113.61 (0.70) 110.76 (0.86) C7_a - F2_a F3_a F1_a F1_a - Distance Angles C7_a 1.3495 (0.0090) F1_a - F2_a - Distance Angles C7_a 1.3280 (0.0095) F2_a - F3_a - Distance Angles C7_a 1.3303 (0.0093) F3_a - C8_a - Distance Angles F6_a 1.3190 (0.0085) F4_a 1.3285 (0.0085) 107.71 (0.83) F5_a 1.3409 (0.0094) 106.48 (0.83) 106.70 (0.83) C4 1.5080 (0.0026) 112.59 (0.59) 112.18 (0.72) 110.84 (1.10) C8_a - F6_a F4_a F5_a F4_a - Distance Angles C8_a 1.3285 (0.0084) F4_a - F5_a - Distance Angles C8_a 1.3409 (0.0094) F5_a - F6_a - Distance Angles C8_a 1.3190 (0.0085) F6_a - N1 - Distance Angles C9 1.3476 (0.0025) C6 1.4135 (0.0025) 127.97 (0.16) H1B 0.8800 116.01 116.01 N1 - C9 C6 C9 - Distance Angles O1 1.2175 (0.0024) N1 1.3476 (0.0025) 124.79 (0.18) C10 1.5259 (0.0027) 122.24 (0.17) 112.93 (0.16) C9 - O1 N1 O1 - Distance Angles C9 1.2175 (0.0024) O1 - C10 - Distance Angles C9 1.5259 (0.0027) Cl1 1.7618 (0.0021) 110.44 (0.13) H10A 0.9900 109.56 109.56 H10B 0.9900 109.56 109.56 108.11 C10 - C9 Cl1 H10A Cl1 - Distance Angles C10 1.7618 (0.0021) Cl1 - C11 - Distance Angles C16 1.3888 (0.0030) C12 1.3927 (0.0029) 118.97 (0.18) H11A 0.9500 120.51 120.51 C11 - C16 C12 C12 - Distance Angles C13 1.3859 (0.0030) C11 1.3927 (0.0029) 122.24 (0.20) C17A_a 1.5018 (0.0032) 119.40 (0.20) 118.36 (0.19) C12 - C13 C11 C13 - Distance Angles C14 1.3792 (0.0032) C12 1.3859 (0.0030) 117.67 (0.19) H13A 0.9500 121.16 121.16 C13 - C14 C12 C14 - Distance Angles C13 1.3792 (0.0032) C15 1.3842 (0.0030) 121.52 (0.19) C18_a 1.5052 (0.0029) 120.96 (0.19) 117.51 (0.20) C14 - C13 C15 C15 - Distance Angles C14 1.3842 (0.0030) C16 1.3918 (0.0027) 120.18 (0.20) H15A 0.9500 119.91 119.91 C15 - C14 C16 C16 - Distance Angles C11 1.3888 (0.0029) C15 1.3918 (0.0027) 119.41 (0.19) N2 1.4151 (0.0026) 124.05 (0.17) 116.54 (0.18) C16 - C11 C15 C17A_a - Distance Angles F7A_a 1.3245 (0.0096) F9A_a 1.3156 (0.0100) 108.27 (0.92) F8A_a 1.3654 (0.0077) 104.04 (0.75) 104.85 (0.88) C12 1.5018 (0.0032) 113.55 (0.85) 115.42 (0.85) 109.76 (0.68) C17A_a - F7A_a F9A_a F8A_a F7A_a - Distance Angles C17A_a 1.3245 (0.0096) F7A_a - F8A_a - Distance Angles C17A_a 1.3654 (0.0077) F8A_a - F9A_a - Distance Angles C17A_a 1.3156 (0.0100) F9A_a - C18_a - Distance Angles F10_a 1.3037 (0.0082) F11_a 1.3323 (0.0076) 108.41 (0.66) F12_a 1.3556 (0.0080) 106.02 (0.64) 103.99 (0.84) C14 1.5052 (0.0029) 115.11 (0.66) 113.38 (0.52) 109.11 (0.65) C18_a - F10_a F11_a F12_a F10_a - Distance Angles C18_a 1.3037 (0.0082) F10_a - F11_a - Distance Angles C18_a 1.3323 (0.0076) F11_a - F12_a - Distance Angles C18_a 1.3556 (0.0079) F12_a - N2 - Distance Angles C19 1.3446 (0.0025) C16 1.4151 (0.0026) 128.01 (0.17) H2A 0.8800 116.00 116.00 N2 - C19 C16 C19 - Distance Angles O2 1.2200 (0.0025) N2 1.3446 (0.0025) 124.18 (0.19) C20 1.5209 (0.0029) 122.46 (0.17) 113.35 (0.17) C19 - O2 N2 O2 - Distance Angles C19 1.2200 (0.0025) O2 - C20 - Distance Angles C19 1.5209 (0.0029) Cl2 1.7574 (0.0021) 110.60 (0.15) H20A 0.9900 109.53 109.53 H20B 0.9900 109.53 109.53 108.09 C20 - C19 Cl2 H20A Cl2 - Distance Angles C20 1.7574 (0.0021) Cl2 - Selected torsion angles -0.09 ( 0.30) C6 - C1 - C2 - C3 -179.01 ( 0.19) C6 - C1 - C2 - C7_a -0.25 ( 0.30) C1 - C2 - C3 - C4 178.65 ( 0.19) C7_a - C2 - C3 - C4 -0.09 ( 0.30) C2 - C3 - C4 - C5 178.97 ( 0.18) C2 - C3 - C4 - C8_a 0.76 ( 0.29) C3 - C4 - C5 - C6 -178.32 ( 0.17) C8_a - C4 - C5 - C6 0.76 ( 0.29) C2 - C1 - C6 - C5 -178.66 ( 0.17) C2 - C1 - C6 - N1 -1.08 ( 0.28) C4 - C5 - C6 - C1 178.30 ( 0.18) C4 - C5 - C6 - N1 -51.26 ( 1.33) C1 - C2 - C7_a - F2_a 129.82 ( 1.32) C3 - C2 - C7_a - F2_a -174.56 ( 1.49) C1 - C2 - C7_a - F3_a 6.51 ( 1.50) C3 - C2 - C7_a - F3_a 67.80 ( 1.08) C1 - C2 - C7_a - F1_a -111.13 ( 1.08) C3 - C2 - C7_a - F1_a 125.09 ( 1.35) C3 - C4 - C8_a - F6_a -55.81 ( 1.36) C5 - C4 - C8_a - F6_a 3.40 ( 1.56) C3 - C4 - C8_a - F4_a -177.50 ( 1.55) C5 - C4 - C8_a - F4_a -115.76 ( 1.43) C3 - C4 - C8_a - F5_a 63.34 ( 1.44) C5 - C4 - C8_a - F5_a -171.87 ( 0.19) C1 - C6 - N1 - C9 8.74 ( 0.31) C5 - C6 - N1 - C9 -0.20 ( 0.33) C6 - N1 - C9 - O1 177.37 ( 0.18) C6 - N1 - C9 - C10 -28.77 ( 0.25) O1 - C9 - C10 - Cl1 153.59 ( 0.15) N1 - C9 - C10 - Cl1 0.49 ( 0.31) C16 - C11 - C12 - C13 -179.20 ( 0.20) C16 - C11 - C12 - C17A_a -0.11 ( 0.32) C11 - C12 - C13 - C14 179.58 ( 0.20) C17A_a - C12 - C13 - C14 -0.33 ( 0.31) C12 - C13 - C14 - C15 -179.07 ( 0.20) C12 - C13 - C14 - C18_a 0.38 ( 0.31) C13 - C14 - C15 - C16 179.16 ( 0.19) C18_a - C14 - C15 - C16 -0.43 ( 0.30) C12 - C11 - C16 - C15 179.92 ( 0.18) C12 - C11 - C16 - N2 0.01 ( 0.30) C14 - C15 - C16 - C11 179.68 ( 0.18) C14 - C15 - C16 - N2 -30.70 ( 1.04) C13 - C12 - C17A_a - F7A_a 149.00 ( 1.02) C11 - C12 - C17A_a - F7A_a 95.16 ( 1.38) C13 - C12 - C17A_a - F9A_a -85.14 ( 1.38) C11 - C12 - C17A_a - F9A_a -146.65 ( 0.78) C13 - C12 - C17A_a - F8A_a 33.04 ( 0.81) C11 - C12 - C17A_a - F8A_a -3.63 ( 0.77) C13 - C14 - C18_a - F10_a 177.58 ( 0.73) C15 - C14 - C18_a - F10_a 122.00 ( 1.21) C13 - C14 - C18_a - F11_a -56.79 ( 1.22) C15 - C14 - C18_a - F11_a -122.63 ( 0.61) C13 - C14 - C18_a - F12_a 58.58 ( 0.63) C15 - C14 - C18_a - F12_a 9.35 ( 0.32) C11 - C16 - N2 - C19 -170.31 ( 0.19) C15 - C16 - N2 - C19 -1.48 ( 0.33) C16 - N2 - C19 - O2 179.59 ( 0.19) C16 - N2 - C19 - C20 33.51 ( 0.27) O2 - C19 - C20 - Cl2 -147.54 ( 0.16) N2 - C19 - C20 - Cl2 FMAP and GRID set by program FMAP 2 3 22 GRID -2.632 -1 -2 2.632 1 2 R1 = 0.0488 for 4389 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.74 at 0.2377 0.1997 0.4678 [ 0.97 A from CL2 ] Deepest hole -0.67 at 0.2341 0.2574 0.3170 [ 0.64 A from CL2 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 4873 / 34081 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.2377 0.3003 0.9678 1.00000 0.05 0.74 0.97 CL2 1.64 C20 1.74 H20B 2.41 H20A Q2 1 1.2166 0.1853 0.8536 1.00000 0.05 0.47 1.05 CL2 1.68 C20 1.72 H20A 2.39 F8C Q3 1 0.4067 0.0587 0.8041 1.00000 0.05 0.41 0.66 C2 0.79 C3 1.52 H3A 1.78 C1 Q4 1 0.9043 0.4269 1.2407 1.00000 0.05 0.34 0.64 C14 0.88 C18 0.88 C18' 1.72 C15 Q5 1 0.7168 0.3447 1.0566 1.00000 0.05 0.33 1.03 CL1 1.29 C10 1.41 H10A 1.93 H10B Q6 1 0.3801 0.0993 1.0485 1.00000 0.05 0.30 0.73 C4 0.79 C8 0.79 C8' 1.72 F5' Q7 1 0.4570 0.0779 0.7625 1.00000 0.05 0.30 0.70 C2 0.78 C1 1.46 H1A 1.85 C3 Q8 1 0.4124 0.0711 0.6800 1.00000 0.05 0.29 0.68 C2 0.83 C7 0.83 C7' 1.72 F2' Q9 1 0.8910 0.4319 0.9938 1.00000 0.05 0.29 0.66 C12 0.74 C13 1.53 H13A 1.77 C11 Q10 1 1.0866 0.2547 0.8634 1.00000 0.05 0.28 0.66 O2 0.85 C19 1.93 N2 2.02 C20 Q11 1 0.7701 0.3410 1.1527 1.00000 0.05 0.27 1.04 CL1 2.24 C10 2.28 H13A 2.44 H10B Q12 1 0.9480 0.4047 1.4607 1.00000 0.05 0.26 1.30 F12' 1.38 F11 1.54 F12 1.74 F11' Q13 1 0.7279 0.2786 1.2396 1.00000 0.05 0.25 1.04 CL1 2.17 C10 2.29 H10A 2.38 H10B Q14 1 1.1255 0.2848 0.7616 1.00000 0.05 0.25 0.99 O2 1.62 H2A 1.81 C19 2.14 H20B Q15 1 0.9912 0.3760 1.1136 1.00000 0.05 0.25 0.67 C15 0.78 C16 1.40 H15A 1.80 C14 Q16 1 0.6646 0.3432 1.1512 1.00000 0.05 0.25 1.05 CL1 1.72 C10 2.08 C9 2.21 H10A Q17 1 1.1855 0.2616 0.9015 1.00000 0.05 0.24 1.01 C20 1.02 CL2 1.69 C19 1.72 H20A Q18 1 0.7358 0.2823 1.1267 1.00000 0.05 0.24 0.86 CL1 1.37 C10 1.56 H10B 2.02 H10A Q19 1 0.3902 0.0705 0.8980 1.00000 0.05 0.23 0.43 C3 0.98 C4 1.26 H3A 1.59 C2 Q20 1 0.5978 0.2403 1.1209 1.00000 0.05 0.23 0.64 O1 0.86 C9 1.96 N1 2.04 C10 Shortest distances between peaks (including symmetry equivalents) 3 19 0.99 11 18 1.01 5 18 1.07 13 18 1.10 3 7 1.12 7 8 1.14 3 8 1.21 2 17 1.23 1 17 1.26 10 14 1.33 5 11 1.34 5 16 1.42 11 13 1.44 6 19 1.51 16 18 1.62 13 16 1.66 14 17 1.73 1 2 1.82 16 20 1.84 7 19 1.91 5 13 1.93 10 17 1.95 11 16 2.07 8 19 2.15 4 12 2.22 4 15 2.26 2 14 2.29 9 15 2.31 4 9 2.35 3 6 2.48 2 10 2.71 13 20 2.76 18 20 2.76 5 20 2.78 1 14 2.85 4 11 2.91 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 0.06: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.06: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.72: Structure factors and derivatives 5.89: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 1.58: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + udel6 finished at 16:22:46 Total CPU time: 8.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++