+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s93 started at 22:45:51 on 20-Feb-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s93 in P2(1)/c CELL 0.71073 20.5017 11.5753 15.4309 90.000 107.669 90.000 ZERR 4.00 0.0043 0.0020 0.0030 0.000 0.021 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O CL ZN UNIT 96 112 48 64 12 8 V = 3489.21 F(000) = 1980.0 Mu = 1.70 mm-1 Cell Wt = 3910.70 Rho = 1.861 MERG 2 OMIT -3.00 55.00 OMIT 0 0 4 SHEL 7 0.77 DFIX 0.84 O1 H1A O1 H1B O11 H11A O11 H11B O12 H12A O12 H12B O61 H61A O61 H61B DANG 1.35 H1A H1B H11A H11B H12A H12B H61A H61B DANG -2.65 0.04 ZN1 H1A ZN1 H1B ZN2 H11A ZN2 H11B ZN2 H12A ZN2 H12B FMAP 2 PLAN 5 SIZE 0.03 0.14 0.16 ACTA BOND $H WGHT 0.05400 36.00610 L.S. 10 TEMP -153.00 FVAR 0.22906 MOLE 1 C1 1 0.090771 0.383728 0.133661 11.00000 0.02860 0.02525 = 0.02910 0.00479 0.00660 0.00577 AFIX 43 H1 2 0.119057 0.449311 0.154432 11.00000 -1.20000 AFIX 0 C2 1 0.020999 0.399859 0.093430 11.00000 0.03387 0.02766 = 0.02794 -0.00113 0.00816 0.00369 AFIX 43 H2 2 0.001595 0.474920 0.089661 11.00000 -1.20000 AFIX 0 C3 1 -0.019635 0.306043 0.059150 11.00000 0.02640 0.03827 = 0.02556 0.00533 0.00885 0.00539 AFIX 43 H3 2 -0.067212 0.315339 0.029289 11.00000 -1.20000 AFIX 0 C4 1 0.010422 0.196928 0.069109 11.00000 0.02350 0.03139 = 0.02897 0.00017 0.00553 -0.00238 AFIX 43 H4 2 -0.016639 0.130362 0.047090 11.00000 -1.20000 AFIX 0 C5 1 0.079497 0.186594 0.111038 11.00000 0.02729 0.02675 = 0.01853 -0.00036 0.01200 -0.00120 C6 1 0.115810 0.073594 0.123120 11.00000 0.02391 0.02711 = 0.01469 -0.00371 0.00565 0.00024 C7 1 0.209796 -0.095521 0.085945 11.00000 0.02045 0.02775 = 0.02121 -0.00522 0.00702 -0.00267 C8 1 0.249845 -0.206159 0.109419 11.00000 0.01960 0.02643 = 0.02484 -0.00096 0.00750 0.00188 C9 1 0.241503 -0.298278 0.049843 11.00000 0.02782 0.03150 = 0.02535 -0.00317 0.00709 -0.00152 AFIX 43 H9 2 0.210044 -0.294434 -0.009703 11.00000 -1.20000 AFIX 0 C10 1 0.280568 -0.396206 0.079990 11.00000 0.03105 0.02663 = 0.02462 -0.00422 0.00926 0.00079 AFIX 43 H10 2 0.275766 -0.461274 0.041028 11.00000 -1.20000 AFIX 0 C11 1 0.326137 -0.399609 0.165832 11.00000 0.02695 0.02588 = 0.02246 -0.00062 0.00625 0.00298 AFIX 43 H11 2 0.352811 -0.466692 0.187439 11.00000 -1.20000 AFIX 0 C12 1 0.332201 -0.303199 0.219879 11.00000 0.02379 0.03177 = 0.02179 -0.00039 0.00821 -0.00312 C13 1 0.381979 -0.293146 0.314571 11.00000 0.02510 0.02876 = 0.01611 0.00203 0.00548 -0.00276 C14 1 0.429852 -0.376023 0.355874 11.00000 0.02348 0.02624 = 0.03121 -0.00079 0.00843 0.00003 AFIX 43 H14 2 0.431661 -0.447796 0.326834 11.00000 -1.20000 AFIX 0 C15 1 0.474157 -0.352146 0.438935 11.00000 0.02809 0.02841 = 0.02868 0.00874 0.00772 0.00338 AFIX 43 H15 2 0.507999 -0.407166 0.468437 11.00000 -1.20000 AFIX 0 C16 1 0.470172 -0.246719 0.481308 11.00000 0.02945 0.02905 = 0.02270 0.00116 0.00608 -0.00222 AFIX 43 H16 2 0.500900 -0.229073 0.539545 11.00000 -1.20000 AFIX 0 C17 1 0.420666 -0.169489 0.436456 11.00000 0.01995 0.03088 = 0.01881 -0.00117 0.00645 -0.00208 C18 1 0.411358 -0.052907 0.469647 11.00000 0.02115 0.02663 = 0.02026 -0.00261 0.00666 -0.00206 C19 1 0.320227 0.180572 0.367936 11.00000 0.02558 0.03123 = 0.02031 -0.00710 0.00812 -0.00643 C20 1 0.305426 0.301755 0.380667 11.00000 0.01967 0.02522 = 0.02909 0.00579 0.00901 -0.00115 C21 1 0.337121 0.361466 0.461568 11.00000 0.02625 0.03468 = 0.01996 0.00078 0.00831 -0.00226 AFIX 43 H21 2 0.368154 0.322288 0.511273 11.00000 -1.20000 AFIX 0 C22 1 0.323432 0.475936 0.469010 11.00000 0.03121 0.03318 = 0.02113 -0.00542 0.01095 -0.00436 AFIX 43 H22 2 0.343254 0.516983 0.524040 11.00000 -1.20000 AFIX 0 C23 1 0.279858 0.529847 0.393909 11.00000 0.03354 0.02607 = 0.03172 -0.00137 0.01361 -0.00040 AFIX 43 H23 2 0.271593 0.610430 0.395749 11.00000 -1.20000 AFIX 0 C24 1 0.248083 0.467764 0.315963 11.00000 0.02665 0.03003 = 0.02642 -0.00175 0.01000 0.00114 AFIX 43 H24 2 0.216749 0.505651 0.265789 11.00000 -1.20000 AFIX 0 N1 3 0.119393 0.278990 0.144094 11.00000 0.02387 0.02995 = 0.02597 -0.00405 0.00967 -0.00241 N2 3 0.080264 -0.021223 0.120207 11.00000 0.02727 0.02898 = 0.02625 0.00179 0.01293 0.00367 AFIX 93 H2A 2 0.100808 -0.088854 0.127079 11.00000 -1.20000 H2B 2 0.035852 -0.017254 0.111380 11.00000 -1.20000 AFIX 0 N3 3 0.181984 0.081419 0.135691 11.00000 0.02169 0.02301 = 0.02278 -0.00081 0.00643 -0.00210 N4 3 0.220193 -0.022390 0.153800 11.00000 0.02107 0.02189 = 0.02140 -0.00512 0.00595 0.00083 N5 3 0.166551 -0.082684 0.003274 11.00000 0.02887 0.02890 = 0.01576 -0.00326 0.00376 0.00523 AFIX 93 H5A 2 0.141182 -0.020042 -0.010529 11.00000 -1.20000 H5B 2 0.163144 -0.136784 -0.037933 11.00000 -1.20000 AFIX 0 N6 3 0.295031 -0.208623 0.193499 11.00000 0.02132 0.02168 = 0.01984 0.00048 0.00595 0.00138 N7 3 0.376357 -0.193840 0.353919 11.00000 0.02428 0.02769 = 0.02041 0.00395 0.00723 -0.00034 N8 3 0.442509 -0.021174 0.554341 11.00000 0.02868 0.02834 = 0.02060 0.00295 0.00466 0.00113 AFIX 93 H8A 2 0.436934 0.049269 0.572345 11.00000 -1.20000 H8B 2 0.468841 -0.070472 0.592771 11.00000 -1.20000 AFIX 0 N9 3 0.371188 0.013203 0.407058 11.00000 0.02485 0.02762 = 0.01933 -0.00009 0.00448 -0.00019 N10 3 0.361926 0.124861 0.435003 11.00000 0.02649 0.02576 = 0.01751 -0.00181 0.00212 -0.00177 N11 3 0.291932 0.137287 0.286651 11.00000 0.01674 0.01570 = 0.00591 0.00046 -0.00149 0.00108 N12 3 0.260983 0.353542 0.310064 11.00000 0.02415 0.02855 = 0.02366 -0.00159 0.00907 -0.00091 O1 4 0.269775 0.312232 0.117058 11.00000 0.02893 0.02916 = 0.02515 -0.00064 0.00942 -0.00034 O11 4 0.380276 -0.005999 0.205211 11.00000 0.02639 0.03062 = 0.02650 -0.00092 0.01120 -0.00271 O12 4 0.233242 -0.082541 0.346286 11.00000 0.02805 0.03509 = 0.02286 0.00188 0.01133 0.00326 ZN1 6 0.221830 0.237833 0.200373 11.00000 0.02142 0.02480 = 0.01949 0.00030 0.00392 0.00069 ZN2 6 0.307152 -0.050985 0.278555 11.00000 0.02192 0.02571 = 0.01688 -0.00021 0.00427 -0.00025 H1A 2 0.258176 0.370628 0.083485 11.00000 0.38667 H1B 2 0.308380 0.291740 0.112975 11.00000 0.09152 H11A 2 0.389835 0.065469 0.208224 11.00000 0.01222 H11B 2 0.418940 -0.037874 0.226675 11.00000 0.04963 H12A 2 0.206770 -0.028367 0.350690 11.00000 0.05777 H12B 2 0.209021 -0.142801 0.336484 11.00000 0.08921 MOLE 2 O31 4 0.158697 0.715998 0.332515 11.00000 0.04325 0.03415 = 0.03593 0.01103 -0.00042 -0.00802 O32 4 0.071864 0.592261 0.251777 11.00000 0.05435 0.02933 = 0.04502 0.00124 0.00920 -0.01019 O33 4 0.125238 0.715210 0.173368 11.00000 0.06336 0.07709 = 0.04052 -0.00332 0.03132 -0.01514 O34 4 0.053393 0.791578 0.248246 11.00000 0.05194 0.03847 = 0.04953 0.00388 0.01184 0.01265 CL31 5 0.101006 0.703912 0.249938 11.00000 0.03234 0.02927 = 0.02225 0.00178 0.00636 -0.00264 MOLE 3 O41 4 0.146008 0.041782 0.465770 11.00000 0.04334 0.03992 = 0.03279 0.00438 0.00989 0.00400 O42 4 0.185478 0.230268 0.449769 11.00000 0.03807 0.06109 = 0.03376 0.00595 0.00654 -0.01026 O43 4 0.069911 0.187578 0.393408 11.00000 0.02768 0.04268 = 0.05995 -0.00485 0.01258 0.00489 O44 4 0.145254 0.110908 0.321785 11.00000 0.08647 0.06449 = 0.02311 0.00436 0.01999 0.03586 CL41 5 0.136178 0.141817 0.407773 11.00000 0.02705 0.04275 = 0.02208 -0.00215 0.00635 0.00554 MOLE 4 O51 4 0.502911 0.198610 0.297449 11.00000 0.05883 0.04827 = 0.01984 0.00886 0.01416 0.02044 O52 4 0.494542 0.370857 0.215401 11.00000 0.04036 0.04255 = 0.04573 0.00345 0.01753 -0.01497 O53 4 0.406190 0.236237 0.173997 11.00000 0.02966 0.05231 = 0.03350 -0.01009 0.00261 -0.00396 O54 4 0.426031 0.342789 0.310539 11.00000 0.04077 0.03825 = 0.03553 -0.00545 0.02062 0.00516 CL51 5 0.457911 0.287982 0.251000 11.00000 0.02367 0.02696 = 0.02159 0.00272 0.00636 0.00060 MOLE 5 O61 4 0.061590 0.436194 0.389483 11.00000 0.03259 0.03619 = 0.02967 -0.00204 0.01066 -0.00415 H61A 2 0.053465 0.365148 0.382524 11.00000 0.11845 H61B 2 0.068655 0.461102 0.341870 11.00000 0.01823 HKLF 4 Covalent radii and connectivity table for s93 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 CL 0.990 ZN 1.330 C1 - N1 C2 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 C5 - N1 C4 C6 C6 - N2 N3 C5 C7 - N4 N5 C8 C8 - N6 C9 C7 C9 - C8 C10 C10 - C11 C9 C11 - C10 C12 C12 - N6 C11 C13 C13 - N7 C14 C12 C14 - C15 C13 C15 - C14 C16 C16 - C17 C15 C17 - N7 C16 C18 C18 - N9 N8 C17 C19 - N10 N11 C20 C20 - N12 C21 C19 C21 - C22 C20 C22 - C21 C23 C23 - C22 C24 C24 - N12 C23 N1 - C1 C5 Zn1 N2 - C6 N3 - C6 N4 Zn1 N4 - C7 N3 Zn2 N5 - C7 N6 - C12 C8 Zn2 N7 - C13 C17 Zn2 N8 - C18 N9 - C18 N10 Zn2 N10 - C19 N9 N11 - C19 Zn1 Zn2 N12 - C20 C24 Zn1 O1 - Zn1 O11 - Zn2 O12 - Zn2 Zn1 - N11 O1 N1 N3 N12 Zn2 - O12 N9 O11 N11 N4 N6 N7 O31 - Cl31 O32 - Cl31 O33 - Cl31 O34 - Cl31 Cl31 - O34 O33 O32 O31 O41 - Cl41 O42 - Cl41 O43 - Cl41 O44 - Cl41 Cl41 - O43 O41 O44 O42 O51 - Cl51 O52 - Cl51 O53 - Cl51 O54 - Cl51 Cl51 - O51 O52 O54 O53 O61 - no bonds found h k l Fo^2 Sigma Why rejected 0 0 7 46.26 10.69 observed but should be systematically absent 0 0 7 28.13 6.05 observed but should be systematically absent 0 11 0 20.99 4.74 observed but should be systematically absent -2 0 11 24.47 6.01 observed but should be systematically absent -2 0 9 23.37 5.80 observed but should be systematically absent -3 0 9 39.30 8.04 observed but should be systematically absent -3 0 7 35.25 8.12 observed but should be systematically absent -3 0 7 45.61 10.67 observed but should be systematically absent -3 0 7 47.25 8.77 observed but should be systematically absent -3 0 7 50.13 10.75 observed but should be systematically absent -3 0 7 40.83 9.61 observed but should be systematically absent -4 0 9 83.74 15.42 observed but should be systematically absent -4 0 9 87.77 16.59 observed but should be systematically absent -4 0 7 92.55 14.08 observed but should be systematically absent -4 0 7 69.66 15.34 observed but should be systematically absent -4 0 7 62.80 14.39 observed but should be systematically absent -4 0 7 81.61 15.40 observed but should be systematically absent -4 0 7 76.30 13.98 observed but should be systematically absent -4 0 5 62.22 15.50 observed but should be systematically absent -7 0 7 18.96 4.54 observed but should be systematically absent -7 0 7 36.86 8.31 observed but should be systematically absent -9 0 9 110.72 25.20 observed but should be systematically absent 38787 Reflections read, of which 1468 rejected -26 =< h =< 26, -14 =< k =< 15, -19 =< l =< 19, Max. 2-theta = 54.96 22 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -6 1 2 226.78 9.64 7 66.27 5 1 2 162.62 7.75 9 41.21 5 8 3 28.04 1.75 11 9.68 7 0 4 92.64 9.57 3 69.36 1 5 4 4.82 0.72 9 4.98 4 2 5 62.66 3.34 6 17.11 -3 5 5 53.12 2.14 11 11.07 -1 3 6 134.80 5.18 11 46.72 -7 1 7 186.60 5.37 14 33.85 -4 0 8 349.54 19.79 7 102.55 -5 1 8 49.78 3.50 13 19.18 11 Inconsistent equivalents 7835 Unique reflections, of which 0 suppressed R(int) = 0.1064 R(sigma) = 0.0836 Friedel opposites merged Maximum memory for data reduction = 4236 / 78715 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 = 5631 / 733474 wR2 = 0.2127 before cycle 1 for 7835 data and 546 / 546 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 8. 10. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.005 0.016 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.148; Restrained GooF = 1.146 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0540 * P )^2 + 36.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22906 0.00057 0.001 OSF Mean shift/esd = 0.001 Maximum = -0.012 for U13 Zn2 Max. shift = 0.001 A for H1A Max. dU = 0.000 for H1A Least-squares cycle 2 Maximum vector length = 511 Memory required = 5631 / 733474 wR2 = 0.2127 before cycle 2 for 7835 data and 546 / 546 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 8. 10. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.005 0.016 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.148; Restrained GooF = 1.146 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0540 * P )^2 + 36.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22906 0.00057 0.002 OSF Mean shift/esd = 0.000 Maximum = -0.005 for U13 Zn2 Max. shift = 0.001 A for H1A Max. dU = 0.000 for H1A Least-squares cycle 3 Maximum vector length = 511 Memory required = 5631 / 733474 wR2 = 0.2127 before cycle 3 for 7835 data and 546 / 546 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 8. 10. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.005 0.016 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.148; Restrained GooF = 1.146 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0540 * P )^2 + 36.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22906 0.00057 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for x H1A Max. shift = 0.000 A for H1A Max. dU = 0.000 for H1A Least-squares cycle 4 Maximum vector length = 511 Memory required = 5631 / 733474 wR2 = 0.2127 before cycle 4 for 7835 data and 546 / 546 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 8. 10. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.005 0.016 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.148; Restrained GooF = 1.146 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0540 * P )^2 + 36.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22906 0.00057 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for x H1A Max. shift = 0.000 A for H1A Max. dU = 0.000 for H1A Least-squares cycle 5 Maximum vector length = 511 Memory required = 5631 / 733474 wR2 = 0.2127 before cycle 5 for 7835 data and 546 / 546 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 8. 10. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.005 0.016 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.148; Restrained GooF = 1.146 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0540 * P )^2 + 36.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22906 0.00057 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for x H1A Max. shift = 0.000 A for H1A Max. dU = 0.000 for H1A Least-squares cycle 6 Maximum vector length = 511 Memory required = 5631 / 733474 wR2 = 0.2127 before cycle 6 for 7835 data and 546 / 546 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 8. 10. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.005 0.016 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.148; Restrained GooF = 1.146 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0540 * P )^2 + 36.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22906 0.00057 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x H1A Max. shift = 0.000 A for H1A Max. dU = 0.000 for H1A Least-squares cycle 7 Maximum vector length = 511 Memory required = 5631 / 733474 wR2 = 0.2127 before cycle 7 for 7835 data and 546 / 546 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 8. 10. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.005 0.016 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.148; Restrained GooF = 1.146 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0540 * P )^2 + 36.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22906 0.00057 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x H1A Max. shift = 0.000 A for H1A Max. dU = 0.000 for H1A Least-squares cycle 8 Maximum vector length = 511 Memory required = 5631 / 733474 wR2 = 0.2127 before cycle 8 for 7835 data and 546 / 546 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 8. 10. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.005 0.016 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.148; Restrained GooF = 1.146 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0540 * P )^2 + 36.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22906 0.00057 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x H61A Max. shift = 0.000 A for H1A Max. dU = 0.000 for H1A Least-squares cycle 9 Maximum vector length = 511 Memory required = 5631 / 733474 wR2 = 0.2127 before cycle 9 for 7835 data and 546 / 546 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 8. 10. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.005 0.016 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.148; Restrained GooF = 1.146 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0540 * P )^2 + 36.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22906 0.00057 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x H1A Max. shift = 0.000 A for H1A Max. dU = 0.000 for H1A Least-squares cycle 10 Maximum vector length = 511 Memory required = 5631 / 733474 wR2 = 0.2127 before cycle 10 for 7835 data and 546 / 546 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 8. 10. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.005 0.016 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.148; Restrained GooF = 1.146 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0540 * P )^2 + 36.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22906 0.00057 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x H61A Max. shift = 0.000 A for H1A Max. dU = 0.000 for H1A Largest correlation matrix elements 0.995 z H1A / y H1A 0.794 z H12B / x H12B 0.578 z H11B / y H11B 0.957 z H1A / x H1A 0.768 y H11B / x H11B 0.551 z H61A / x H61A 0.957 y H1A / x H1A 0.736 z H1B / y H1B 0.542 z H11B / x H11B 0.936 z H1B / x H1B 0.721 z H61B / x H61B 0.537 y H12B / x H12A -0.893 y H12B / x H12B -0.671 z H12B / y H12B -0.531 x H12B / y H12A 0.831 z H12A / x H12A 0.635 y H12A / x H12A 0.525 U13 O33 / U11 O33 -0.829 y H61A / x H61A 0.627 y H12B / y H12A -0.525 y H11B / x H11A 0.829 y H1B / x H1B 0.624 z H11A / x H11A 0.517 U13 O33 / U33 O33 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.1191 0.4493 0.1544 43 0.950 0.000 C1 N1 C2 H2 0.0016 0.4749 0.0897 43 0.950 0.000 C2 C3 C1 H3 -0.0672 0.3153 0.0293 43 0.950 0.000 C3 C2 C4 H4 -0.0166 0.1304 0.0471 43 0.950 0.000 C4 C5 C3 H9 0.2100 -0.2944 -0.0097 43 0.950 0.000 C9 C8 C10 H10 0.2758 -0.4613 0.0410 43 0.950 0.000 C10 C11 C9 H11 0.3528 -0.4667 0.1874 43 0.950 0.000 C11 C10 C12 H14 0.4317 -0.4478 0.3268 43 0.950 0.000 C14 C15 C13 H15 0.5080 -0.4072 0.4684 43 0.950 0.000 C15 C14 C16 H16 0.5009 -0.2291 0.5395 43 0.950 0.000 C16 C17 C15 H21 0.3682 0.3223 0.5113 43 0.950 0.000 C21 C22 C20 H22 0.3433 0.5170 0.5240 43 0.950 0.000 C22 C21 C23 H23 0.2716 0.6104 0.3957 43 0.950 0.000 C23 C22 C24 H24 0.2167 0.5056 0.2658 43 0.950 0.000 C24 N12 C23 H2A 0.1008 -0.0889 0.1271 93 0.880 0.000 N2 C6 N3 H2B 0.0359 -0.0173 0.1114 93 0.880 0.000 N2 C6 N3 H5A 0.1412 -0.0200 -0.0105 93 0.880 0.000 N5 C7 N4 H5B 0.1631 -0.1368 -0.0379 93 0.880 0.000 N5 C7 N4 H8A 0.4369 0.0493 0.5723 93 0.880 0.000 N8 C18 N9 H8B 0.4688 -0.0705 0.5928 93 0.880 0.000 N8 C18 N9 s93 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.09077 0.38373 0.13366 1.00000 0.02860 0.02525 0.02910 0.00479 0.00660 0.00577 0.02813 0.01576 0.00039 0.00067 0.00053 0.00000 0.00378 0.00374 0.00412 0.00317 0.00310 0.00308 0.00162 H1 0.11906 0.44931 0.15443 1.00000 0.03375 0.00000 0.00000 C2 0.02100 0.39986 0.09343 1.00000 0.03387 0.02766 0.02794 -0.00114 0.00816 0.00370 0.03009 0.01540 0.00040 0.00069 0.00053 0.00000 0.00409 0.00395 0.00414 0.00323 0.00323 0.00323 0.00168 H2 0.00160 0.47492 0.08966 1.00000 0.03611 0.00000 0.00000 C3 -0.01964 0.30604 0.05915 1.00000 0.02640 0.03827 0.02556 0.00532 0.00884 0.00539 0.02986 0.01608 0.00040 0.00071 0.00053 0.00000 0.00373 0.00438 0.00400 0.00340 0.00307 0.00329 0.00168 H3 -0.06721 0.31534 0.02929 1.00000 0.03584 0.00000 0.00000 C4 0.01042 0.19693 0.06911 1.00000 0.02350 0.03138 0.02898 0.00018 0.00553 -0.00238 0.02850 0.01512 0.00038 0.00070 0.00053 0.00000 0.00355 0.00402 0.00412 0.00328 0.00303 0.00307 0.00163 H4 -0.01664 0.13036 0.04709 1.00000 0.03419 0.00000 0.00000 C5 0.07950 0.18659 0.11104 1.00000 0.02729 0.02675 0.01853 -0.00036 0.01200 -0.00120 0.02306 0.01424 0.00037 0.00064 0.00048 0.00000 0.00357 0.00369 0.00354 0.00287 0.00284 0.00292 0.00147 C6 0.11581 0.07359 0.12312 1.00000 0.02391 0.02711 0.01469 -0.00371 0.00565 0.00024 0.02195 0.01342 0.00035 0.00063 0.00046 0.00000 0.00338 0.00369 0.00334 0.00277 0.00265 0.00284 0.00144 C7 0.20980 -0.09552 0.08595 1.00000 0.02046 0.02775 0.02121 -0.00522 0.00702 -0.00267 0.02298 0.01359 0.00035 0.00063 0.00049 0.00000 0.00326 0.00373 0.00360 0.00297 0.00269 0.00283 0.00146 C8 0.24985 -0.20616 0.10942 1.00000 0.01960 0.02643 0.02484 -0.00096 0.00750 0.00188 0.02346 0.01414 0.00035 0.00064 0.00050 0.00000 0.00327 0.00368 0.00373 0.00298 0.00277 0.00277 0.00148 C9 0.24150 -0.29828 0.04984 1.00000 0.02782 0.03150 0.02536 -0.00317 0.00709 -0.00152 0.02845 0.01501 0.00039 0.00068 0.00054 0.00000 0.00376 0.00403 0.00397 0.00321 0.00305 0.00314 0.00163 H9 0.21004 -0.29443 -0.00970 1.00000 0.03414 0.00000 0.00000 C10 0.28057 -0.39621 0.07999 1.00000 0.03105 0.02663 0.02461 -0.00422 0.00926 0.00079 0.02725 0.01499 0.00039 0.00066 0.00052 0.00000 0.00386 0.00382 0.00389 0.00311 0.00308 0.00310 0.00159 H10 0.27577 -0.46127 0.04103 1.00000 0.03270 0.00000 0.00000 C11 0.32614 -0.39961 0.16583 1.00000 0.02695 0.02588 0.02246 -0.00062 0.00625 0.00298 0.02537 0.01436 0.00037 0.00065 0.00050 0.00000 0.00364 0.00374 0.00373 0.00299 0.00288 0.00295 0.00153 H11 0.35281 -0.46669 0.18744 1.00000 0.03045 0.00000 0.00000 C12 0.33220 -0.30320 0.21988 1.00000 0.02379 0.03177 0.02180 -0.00039 0.00821 -0.00312 0.02550 0.01445 0.00037 0.00067 0.00050 0.00000 0.00350 0.00395 0.00373 0.00308 0.00287 0.00301 0.00154 C13 0.38198 -0.29315 0.31457 1.00000 0.02511 0.02877 0.01611 0.00203 0.00548 -0.00276 0.02350 0.01390 0.00036 0.00065 0.00047 0.00000 0.00349 0.00380 0.00344 0.00289 0.00273 0.00291 0.00149 C14 0.42985 -0.37602 0.35587 1.00000 0.02348 0.02624 0.03121 -0.00079 0.00843 0.00003 0.02695 0.01485 0.00037 0.00066 0.00053 0.00000 0.00349 0.00374 0.00417 0.00319 0.00301 0.00296 0.00158 H14 0.43166 -0.44780 0.32684 1.00000 0.03233 0.00000 0.00000 C15 0.47416 -0.35215 0.43894 1.00000 0.02809 0.02841 0.02868 0.00874 0.00773 0.00339 0.02859 0.01553 0.00039 0.00067 0.00053 0.00000 0.00377 0.00394 0.00410 0.00320 0.00311 0.00308 0.00164 H15 0.50800 -0.40717 0.46844 1.00000 0.03431 0.00000 0.00000 C16 0.47017 -0.24672 0.48131 1.00000 0.02945 0.02905 0.02270 0.00117 0.00608 -0.00222 0.02748 0.01503 0.00038 0.00066 0.00053 0.00000 0.00377 0.00395 0.00382 0.00306 0.00297 0.00311 0.00160 H16 0.50090 -0.22907 0.53955 1.00000 0.03297 0.00000 0.00000 C17 0.42067 -0.16949 0.43646 1.00000 0.01995 0.03088 0.01882 -0.00117 0.00646 -0.00209 0.02309 0.01371 0.00035 0.00065 0.00048 0.00000 0.00327 0.00382 0.00352 0.00293 0.00269 0.00286 0.00147 C18 0.41136 -0.05291 0.46965 1.00000 0.02116 0.02663 0.02026 -0.00261 0.00666 -0.00206 0.02260 0.01357 0.00035 0.00063 0.00048 0.00000 0.00327 0.00363 0.00357 0.00290 0.00268 0.00284 0.00145 C19 0.32023 0.18057 0.36794 1.00000 0.02557 0.03123 0.02031 -0.00710 0.00811 -0.00643 0.02545 0.01386 0.00037 0.00067 0.00050 0.00000 0.00355 0.00394 0.00365 0.00305 0.00288 0.00303 0.00155 C20 0.30543 0.30176 0.38067 1.00000 0.01968 0.02522 0.02909 0.00579 0.00902 -0.00115 0.02430 0.01456 0.00035 0.00064 0.00052 0.00000 0.00331 0.00365 0.00399 0.00304 0.00289 0.00278 0.00152 C21 0.33712 0.36147 0.46157 1.00000 0.02625 0.03468 0.01996 0.00078 0.00831 -0.00225 0.02667 0.01459 0.00038 0.00069 0.00050 0.00000 0.00359 0.00417 0.00370 0.00311 0.00288 0.00312 0.00158 H21 0.36815 0.32229 0.51127 1.00000 0.03201 0.00000 0.00000 C22 0.32343 0.47594 0.46901 1.00000 0.03121 0.03318 0.02113 -0.00542 0.01095 -0.00436 0.02784 0.01501 0.00039 0.00068 0.00052 0.00000 0.00392 0.00416 0.00377 0.00310 0.00305 0.00317 0.00163 H22 0.34325 0.51698 0.52404 1.00000 0.03341 0.00000 0.00000 C23 0.27986 0.52985 0.39391 1.00000 0.03354 0.02607 0.03172 -0.00137 0.01361 -0.00040 0.02962 0.01574 0.00040 0.00068 0.00055 0.00000 0.00407 0.00386 0.00432 0.00323 0.00333 0.00316 0.00168 H23 0.27159 0.61043 0.39575 1.00000 0.03554 0.00000 0.00000 C24 0.24808 0.46776 0.31596 1.00000 0.02666 0.03003 0.02642 -0.00175 0.01000 0.00114 0.02727 0.01496 0.00038 0.00066 0.00053 0.00000 0.00368 0.00399 0.00403 0.00319 0.00304 0.00306 0.00160 H24 0.21675 0.50565 0.26579 1.00000 0.03272 0.00000 0.00000 N1 0.11939 0.27899 0.14409 1.00000 0.02386 0.02995 0.02598 -0.00405 0.00966 -0.00241 0.02613 0.01209 0.00031 0.00055 0.00043 0.00000 0.00300 0.00333 0.00337 0.00268 0.00251 0.00256 0.00134 N2 0.08026 -0.02122 0.12021 1.00000 0.02727 0.02898 0.02625 0.00179 0.01293 0.00367 0.02643 0.01269 0.00032 0.00055 0.00043 0.00000 0.00316 0.00334 0.00335 0.00264 0.00260 0.00260 0.00135 H2A 0.10081 -0.08885 0.12708 1.00000 0.03171 0.00000 0.00000 H2B 0.03585 -0.01725 0.11138 1.00000 0.03171 0.00000 0.00000 N3 0.18198 0.08142 0.13569 1.00000 0.02169 0.02301 0.02278 -0.00081 0.00643 -0.00210 0.02256 0.01144 0.00030 0.00051 0.00041 0.00000 0.00284 0.00299 0.00310 0.00246 0.00236 0.00236 0.00124 N4 0.22019 -0.02239 0.15380 1.00000 0.02107 0.02189 0.02141 -0.00512 0.00595 0.00083 0.02156 0.01123 0.00029 0.00050 0.00041 0.00000 0.00280 0.00299 0.00312 0.00240 0.00232 0.00231 0.00124 N5 0.16655 -0.08268 0.00327 1.00000 0.02887 0.02890 0.01576 -0.00326 0.00376 0.00523 0.02518 0.01193 0.00031 0.00056 0.00040 0.00000 0.00315 0.00325 0.00295 0.00250 0.00239 0.00257 0.00132 H5A 0.14118 -0.02004 -0.01053 1.00000 0.03022 0.00000 0.00000 H5B 0.16314 -0.13678 -0.03793 1.00000 0.03022 0.00000 0.00000 N6 0.29503 -0.20862 0.19350 1.00000 0.02133 0.02168 0.01984 0.00048 0.00596 0.00138 0.02101 0.01138 0.00029 0.00051 0.00040 0.00000 0.00280 0.00295 0.00300 0.00237 0.00230 0.00231 0.00121 N7 0.37636 -0.19384 0.35392 1.00000 0.02428 0.02769 0.02042 0.00394 0.00724 -0.00034 0.02403 0.01201 0.00030 0.00054 0.00041 0.00000 0.00298 0.00321 0.00311 0.00256 0.00241 0.00252 0.00129 N8 0.44251 -0.02117 0.55434 1.00000 0.02868 0.02834 0.02060 0.00295 0.00466 0.00113 0.02650 0.01211 0.00032 0.00056 0.00042 0.00000 0.00321 0.00329 0.00320 0.00255 0.00251 0.00260 0.00135 H8A 0.43693 0.04927 0.57234 1.00000 0.03180 0.00000 0.00000 H8B 0.46884 -0.07047 0.59277 1.00000 0.03180 0.00000 0.00000 N9 0.37119 0.01320 0.40706 1.00000 0.02485 0.02762 0.01933 -0.00008 0.00448 -0.00019 0.02443 0.01181 0.00031 0.00054 0.00041 0.00000 0.00303 0.00321 0.00310 0.00252 0.00239 0.00252 0.00130 N10 0.36193 0.12486 0.43500 1.00000 0.02649 0.02576 0.01751 -0.00181 0.00212 -0.00177 0.02427 0.01142 0.00031 0.00053 0.00040 0.00000 0.00306 0.00314 0.00302 0.00244 0.00237 0.00251 0.00129 N11 0.29193 0.13729 0.28665 1.00000 0.01675 0.01570 0.00591 0.00046 -0.00149 0.00108 0.01388 0.00977 0.00026 0.00045 0.00034 0.00000 0.00251 0.00257 0.00239 0.00201 0.00190 0.00204 0.00105 N12 0.26098 0.35354 0.31006 1.00000 0.02415 0.02855 0.02366 -0.00159 0.00907 -0.00091 0.02505 0.01205 0.00031 0.00054 0.00042 0.00000 0.00300 0.00331 0.00323 0.00260 0.00247 0.00252 0.00131 O1 0.26977 0.31223 0.11706 1.00000 0.02893 0.02916 0.02515 -0.00064 0.00941 -0.00034 0.02748 0.01066 0.00028 0.00048 0.00037 0.00000 0.00282 0.00279 0.00279 0.00225 0.00223 0.00226 0.00113 O11 0.38028 -0.00600 0.20521 1.00000 0.02640 0.03062 0.02651 -0.00092 0.01119 -0.00271 0.02714 0.01032 0.00027 0.00048 0.00036 0.00000 0.00273 0.00296 0.00286 0.00236 0.00222 0.00233 0.00114 O12 0.23324 -0.08254 0.34629 1.00000 0.02805 0.03508 0.02286 0.00188 0.01133 0.00326 0.02786 0.01101 0.00027 0.00051 0.00036 0.00000 0.00268 0.00305 0.00276 0.00237 0.00218 0.00250 0.00115 Zn1 0.22183 0.23783 0.20037 1.00000 0.02142 0.02480 0.01950 0.00030 0.00392 0.00069 0.02241 0.00161 0.00004 0.00007 0.00006 0.00000 0.00040 0.00043 0.00043 0.00033 0.00031 0.00033 0.00021 Zn2 0.30715 -0.05099 0.27855 1.00000 0.02192 0.02571 0.01689 -0.00021 0.00426 -0.00025 0.02187 0.00157 0.00004 0.00007 0.00005 0.00000 0.00040 0.00044 0.00042 0.00033 0.00031 0.00033 0.00021 H1A 0.25809 0.37046 0.08331 1.00000 0.38758 0.75698 0.01034 0.02045 0.02043 0.00000 0.22586 H1B 0.30838 0.29176 0.11298 1.00000 0.09162 0.26962 0.00345 0.00864 0.00753 0.00000 0.04759 H11A 0.38983 0.06547 0.20822 1.00000 0.01226 0.10600 0.00275 0.00199 0.00426 0.00000 0.01816 H11B 0.41894 -0.03787 0.22668 1.00000 0.04968 0.14608 0.00171 0.00530 0.00467 0.00000 0.03063 H12A 0.20677 -0.02837 0.35070 1.00000 0.05780 0.18768 0.00350 0.00370 0.00649 0.00000 0.03391 H12B 0.20902 -0.14280 0.33648 1.00000 0.08908 0.14036 0.00406 0.00458 0.00690 0.00000 0.04776 O31 0.15870 0.71600 0.33251 1.00000 0.04325 0.03415 0.03592 0.01103 -0.00042 -0.00802 0.04055 0.01160 0.00031 0.00052 0.00041 0.00000 0.00339 0.00318 0.00340 0.00264 0.00267 0.00265 0.00148 O32 0.07186 0.59226 0.25178 1.00000 0.05435 0.02933 0.04501 0.00124 0.00920 -0.01018 0.04421 0.01206 0.00034 0.00051 0.00044 0.00000 0.00390 0.00311 0.00381 0.00276 0.00304 0.00280 0.00154 O33 0.12524 0.71521 0.17337 1.00000 0.06335 0.07708 0.04052 -0.00332 0.03131 -0.01513 0.05685 0.01467 0.00038 0.00070 0.00048 0.00000 0.00457 0.00515 0.00398 0.00359 0.00353 0.00391 0.00193 O34 0.05339 0.79158 0.24825 1.00000 0.05193 0.03848 0.04953 0.00388 0.01184 0.01265 0.04744 0.01362 0.00035 0.00056 0.00047 0.00000 0.00390 0.00350 0.00406 0.00300 0.00318 0.00301 0.00162 Cl31 0.10101 0.70391 0.24994 1.00000 0.03234 0.02927 0.02225 0.00178 0.00636 -0.00264 0.02838 0.00358 0.00010 0.00016 0.00012 0.00000 0.00092 0.00093 0.00090 0.00072 0.00071 0.00074 0.00040 O41 0.14601 0.04178 0.46577 1.00000 0.04334 0.03992 0.03280 0.00438 0.00989 0.00400 0.03906 0.01207 0.00031 0.00052 0.00041 0.00000 0.00341 0.00336 0.00329 0.00267 0.00265 0.00271 0.00140 O42 0.18548 0.23027 0.44977 1.00000 0.03807 0.06109 0.03377 0.00595 0.00654 -0.01026 0.04528 0.01238 0.00032 0.00061 0.00043 0.00000 0.00332 0.00426 0.00342 0.00303 0.00266 0.00305 0.00158 O43 0.06991 0.18758 0.39341 1.00000 0.02768 0.04268 0.05995 -0.00485 0.01259 0.00489 0.04360 0.01243 0.00029 0.00055 0.00047 0.00000 0.00296 0.00352 0.00428 0.00313 0.00285 0.00262 0.00154 O44 0.14526 0.11091 0.32179 1.00000 0.08648 0.06449 0.02311 0.00436 0.01999 0.03587 0.05728 0.01564 0.00041 0.00065 0.00042 0.00000 0.00536 0.00465 0.00330 0.00307 0.00335 0.00407 0.00204 Cl41 0.13618 0.14182 0.40777 1.00000 0.02705 0.04275 0.02208 -0.00215 0.00635 0.00554 0.03087 0.00374 0.00009 0.00018 0.00012 0.00000 0.00087 0.00110 0.00091 0.00079 0.00069 0.00078 0.00042 O51 0.50291 0.19861 0.29745 1.00000 0.05882 0.04827 0.01984 0.00886 0.01416 0.02043 0.04181 0.01322 0.00034 0.00056 0.00038 0.00000 0.00395 0.00367 0.00287 0.00262 0.00269 0.00310 0.00152 O52 0.49454 0.37086 0.21540 1.00000 0.04036 0.04256 0.04573 0.00346 0.01753 -0.01496 0.04189 0.01198 0.00031 0.00054 0.00043 0.00000 0.00333 0.00348 0.00374 0.00292 0.00287 0.00280 0.00148 O53 0.40619 0.23624 0.17400 1.00000 0.02966 0.05230 0.03350 -0.01009 0.00261 -0.00396 0.04004 0.01106 0.00029 0.00056 0.00041 0.00000 0.00291 0.00381 0.00330 0.00281 0.00244 0.00269 0.00144 O54 0.42603 0.34279 0.31054 1.00000 0.04077 0.03825 0.03553 -0.00545 0.02062 0.00516 0.03617 0.01178 0.00030 0.00050 0.00040 0.00000 0.00323 0.00322 0.00329 0.00262 0.00266 0.00263 0.00134 Cl51 0.45791 0.28798 0.25100 1.00000 0.02367 0.02697 0.02159 0.00272 0.00636 0.00060 0.02419 0.00340 0.00009 0.00015 0.00012 0.00000 0.00080 0.00087 0.00086 0.00068 0.00065 0.00066 0.00037 O61 0.06159 0.43620 0.38948 1.00000 0.03259 0.03618 0.02968 -0.00204 0.01067 -0.00415 0.03255 0.01131 0.00029 0.00053 0.00039 0.00000 0.00296 0.00334 0.00320 0.00257 0.00242 0.00256 0.00125 H61A 0.05350 0.36514 0.38254 1.00000 0.11815 0.22279 0.00827 0.00328 0.00739 0.00000 0.06124 H61B 0.06866 0.46110 0.34187 1.00000 0.01822 0.14565 0.00391 0.00591 0.00315 0.00000 0.02010 Final Structure Factor Calculation for s93 in P2(1)/c Total number of l.s. parameters = 546 Maximum vector length = 511 Memory required = 5085 / 25039 wR2 = 0.2127 before cycle 11 for 7835 data and 0 / 546 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 8. 10. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.005 0.016 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.148; Restrained GooF = 1.146 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0540 * P )^2 + 36.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0821 for 5761 Fo > 4sig(Fo) and 0.1130 for all 7835 data wR2 = 0.2127, GooF = S = 1.148, Restrained GooF = 1.146 for all data Occupancy sum of asymmetric unit = 57.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.0330 0.0319 0.0196 C1 0.0367 0.0282 0.0254 C2 0.0413 0.0247 0.0236 C3 0.0329 0.0300 0.0226 C4 0.0290 0.0262 0.0140 C5 0.0284 0.0240 0.0134 C6 0.0308 0.0198 0.0183 C7 0.0274 0.0245 0.0184 C8 0.0329 0.0286 0.0239 C9 0.0315 0.0298 0.0205 C10 0.0304 0.0234 0.0223 C11 0.0328 0.0233 0.0204 C12 0.0312 0.0237 0.0156 C13 0.0315 0.0261 0.0232 C14 0.0373 0.0289 0.0196 C15 0.0329 0.0271 0.0225 C16 0.0313 0.0196 0.0183 C17 0.0279 0.0206 0.0193 C18 0.0368 0.0228 0.0168 C19 0.0334 0.0226 0.0168 C20 0.0354 0.0258 0.0189 C21 0.0377 0.0279 0.0179 C22 0.0357 0.0277 0.0255 C23 0.0309 0.0280 0.0229 C24 0.0329 0.0239 0.0216 N1 0.0333 0.0264 0.0196 N2 0.0245 0.0230 0.0201 N3 0.0276 0.0209 0.0162 N4 0.0369 0.0237 0.0150 N5 0.0229 0.0205 0.0196 N6 0.0296 0.0243 0.0182 N7 0.0309 0.0293 0.0194 N8 0.0276 0.0266 0.0190 N9 0.0305 0.0261 0.0162 N10 0.0210 0.0156 0.0051 N11 0.0292 0.0247 0.0212 N12 0.0295 0.0287 0.0242 O1 0.0323 0.0275 0.0216 O11 0.0366 0.0275 0.0194 O12 0.0250 0.0238 0.0185 Zn1 0.0257 0.0231 0.0167 Zn2 0.0659 0.0318 0.0239 O31 0.0633 0.0437 0.0256 O32 0.0874 0.0581 0.0251 O33 0.0609 0.0507 0.0307 O34 0.0355 0.0278 0.0218 Cl31 0.0461 0.0405 0.0306 O41 0.0686 0.0352 0.0321 O42 0.0628 0.0428 0.0251 O43 0.1139 0.0381 0.0198 O44 0.0454 0.0254 0.0218 Cl41 0.0747 0.0338 0.0170 O51 0.0570 0.0468 0.0219 O52 0.0569 0.0396 0.0236 O53 0.0457 0.0424 0.0203 O54 0.0281 0.0240 0.0204 Cl51 0.0390 0.0299 0.0287 O61 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.023 0.035 0.046 0.060 0.076 0.096 0.125 0.178 1.000 Number in group 793. 830. 783. 737. 799. 791. 747. 784. 781. 790. GooF 1.395 1.357 1.195 1.149 1.180 1.023 0.944 0.928 1.014 1.165 K 9.998 2.560 1.493 1.269 1.136 1.085 1.024 1.018 1.025 1.001 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.16 1.32 1.66 inf Number in group 783. 808. 764. 791. 772. 792. 784. 774. 778. 789. GooF 0.954 0.885 0.878 0.926 0.856 0.912 0.958 1.175 1.363 2.030 K 0.937 1.054 1.051 1.027 1.037 1.024 1.015 1.031 1.017 1.033 R1 0.255 0.191 0.173 0.137 0.102 0.092 0.082 0.079 0.078 0.088 Recommended weighting scheme: WGHT 0.0540 35.9803 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) 5 3 2 2370.65 2.73 10.14 0.004 2.41 1 1 5 4666.25 1242.54 7.56 0.088 2.71 -3 3 5 3113.99 454.67 7.36 0.053 2.39 7 0 0 3148.91 11.36 7.15 0.008 2.79 -6 2 1 1042.46 14.39 6.96 0.010 2.93 -7 0 2 6341.56 698.91 6.73 0.066 2.92 0 1 16 -61.56 1630.21 6.66 0.101 0.92 7 4 3 3298.20 279.72 6.66 0.042 1.73 4 0 2 4189.12 876.22 6.60 0.074 3.60 -2 0 4 2292.48 96.84 6.55 0.025 3.85 5 6 4 8080.06 2756.69 6.34 0.132 1.49 -6 3 7 4897.18 227.85 6.33 0.038 1.83 1 3 2 13366.91 4134.15 6.33 0.161 3.29 -4 2 6 3380.21 477.43 6.27 0.055 2.31 8 3 4 2158.76 440.95 6.24 0.053 1.63 8 5 1 1290.52 40.38 6.21 0.016 1.63 1 0 6 1461.05 24.17 6.21 0.012 2.35 8 1 4 8742.08 2000.76 6.15 0.112 1.78 10 2 10 3258.07 482.84 6.15 0.055 1.02 -1 3 7 1403.32 13.94 6.12 0.009 1.88 1 1 3 882.99 61.81 5.88 0.020 4.15 6 1 6 5905.85 568.78 5.84 0.060 1.70 -7 7 4 8924.94 2717.35 5.73 0.131 1.40 -5 3 5 4090.00 27.26 5.68 0.013 2.26 7 4 5 1749.65 364.34 5.60 0.048 1.51 8 1 9 2192.91 54.46 5.58 0.019 1.19 -12 4 7 2687.95 828.75 5.50 0.072 1.35 -9 3 5 1505.62 10.83 5.42 0.008 1.83 2 0 10 22370.79 39872.53 5.40 0.501 1.39 -8 4 7 1008.38 68.94 5.38 0.021 1.59 -5 4 2 797.67 2.32 5.37 0.004 2.34 -5 3 9 3004.66 47.55 5.32 0.017 1.56 -12 5 6 1319.78 140.17 5.27 0.030 1.31 4 0 4 1904.86 270.53 5.23 0.041 2.58 -5 1 6 1021.80 74.43 5.23 0.022 2.38 -10 7 2 2332.68 564.23 5.23 0.060 1.29 -5 3 7 7361.73 3205.90 5.21 0.142 1.87 -8 3 5 1406.41 115.25 5.18 0.027 1.94 -4 3 7 689.54 0.94 5.16 0.002 1.90 4 4 0 6080.54 2128.65 5.07 0.116 2.49 3 1 5 1356.80 296.37 5.06 0.043 2.37 3 3 2 6127.54 3270.40 5.03 0.143 2.86 9 5 3 2522.99 62.96 4.99 0.020 1.42 -3 2 12 2445.43 17.28 4.97 0.010 1.25 -2 2 3 1234.78 134.63 4.96 0.029 3.80 7 1 5 3673.81 701.20 4.93 0.066 1.75 -1 1 18 20.17 925.12 4.85 0.076 0.82 -12 6 8 4524.71 1955.03 4.83 0.111 1.16 0 2 16 3273.74 8046.90 4.82 0.225 0.91 -6 3 5 693.86 42.16 4.75 0.016 2.16 Bond lengths and angles C1 - Distance Angles N1 1.3352 (0.0097) C2 1.3883 (0.0106) 122.11 (0.74) H1 0.9500 118.95 118.95 C1 - N1 C2 C2 - Distance Angles C3 1.3732 (0.0114) C1 1.3883 (0.0106) 119.22 (0.74) H2 0.9500 120.39 120.39 C2 - C3 C1 C3 - Distance Angles C2 1.3732 (0.0114) C4 1.3933 (0.0112) 118.56 (0.71) H3 0.9500 120.72 120.72 C3 - C2 C4 C4 - Distance Angles C5 1.3720 (0.0102) C3 1.3933 (0.0112) 119.32 (0.73) H4 0.9500 120.34 120.34 C4 - C5 C3 C5 - Distance Angles N1 1.3490 (0.0095) C4 1.3720 (0.0102) 121.99 (0.70) C6 1.4885 (0.0101) 115.25 (0.62) 122.76 (0.67) C5 - N1 C4 C6 - Distance Angles N2 1.3107 (0.0095) N3 1.3140 (0.0089) 126.96 (0.68) C5 1.4885 (0.0101) 118.67 (0.62) 114.37 (0.63) C6 - N2 N3 C7 - Distance Angles N4 1.3126 (0.0091) N5 1.3225 (0.0091) 126.59 (0.69) C8 1.5050 (0.0101) 114.34 (0.63) 119.00 (0.63) C7 - N4 N5 C8 - Distance Angles N6 1.3464 (0.0090) C9 1.3842 (0.0106) 122.27 (0.67) C7 1.5050 (0.0101) 114.55 (0.62) 123.18 (0.66) C8 - N6 C9 C9 - Distance Angles C8 1.3842 (0.0106) C10 1.3844 (0.0108) 117.73 (0.71) H9 0.9500 121.13 121.13 C9 - C8 C10 C10 - Distance Angles C11 1.3704 (0.0103) C9 1.3844 (0.0108) 120.23 (0.71) H10 0.9500 119.88 119.88 C10 - C11 C9 C11 - Distance Angles C10 1.3704 (0.0103) C12 1.3760 (0.0106) 118.18 (0.70) H11 0.9500 120.91 120.91 C11 - C10 C12 C12 - Distance Angles N6 1.3254 (0.0096) C11 1.3760 (0.0106) 123.09 (0.68) C13 1.5116 (0.0098) 112.95 (0.65) 123.96 (0.69) C12 - N6 C11 C13 - Distance Angles N7 1.3213 (0.0098) C14 1.3821 (0.0103) 122.73 (0.67) C12 1.5116 (0.0098) 112.56 (0.63) 124.68 (0.69) C13 - N7 C14 C14 - Distance Angles C15 1.3555 (0.0108) C13 1.3821 (0.0103) 118.22 (0.72) H14 0.9500 120.89 120.89 C14 - C15 C13 C15 - Distance Angles C14 1.3555 (0.0108) C16 1.3985 (0.0111) 120.17 (0.71) H15 0.9500 119.92 119.92 C15 - C14 C16 C16 - Distance Angles C17 1.3718 (0.0104) C15 1.3985 (0.0111) 118.17 (0.70) H16 0.9500 120.92 120.92 C16 - C17 C15 C17 - Distance Angles N7 1.3507 (0.0090) C16 1.3718 (0.0104) 121.51 (0.69) C18 1.4762 (0.0103) 113.40 (0.62) 125.06 (0.66) C17 - N7 C16 C18 - Distance Angles N9 1.3091 (0.0094) N8 1.3206 (0.0094) 125.06 (0.69) C17 1.4762 (0.0103) 113.39 (0.63) 121.53 (0.66) C18 - N9 N8 C19 - Distance Angles N10 1.2964 (0.0096) N11 1.3112 (0.0087) 124.52 (0.70) C20 1.4610 (0.0107) 118.93 (0.65) 116.48 (0.67) C19 - N10 N11 C20 - Distance Angles N12 1.3319 (0.0094) C21 1.4021 (0.0106) 121.57 (0.69) C19 1.4610 (0.0107) 116.14 (0.68) 122.27 (0.67) C20 - N12 C21 C21 - Distance Angles C22 1.3665 (0.0111) C20 1.4021 (0.0106) 120.09 (0.71) H21 0.9500 119.96 119.96 C21 - C22 C20 C22 - Distance Angles C21 1.3665 (0.0111) C23 1.3791 (0.0112) 117.73 (0.72) H22 0.9500 121.13 121.13 C22 - C21 C23 C23 - Distance Angles C22 1.3791 (0.0112) C24 1.3827 (0.0111) 120.65 (0.73) H23 0.9500 119.68 119.68 C23 - C22 C24 C24 - Distance Angles N12 1.3568 (0.0098) C23 1.3827 (0.0111) 120.99 (0.72) H24 0.9500 119.51 119.51 C24 - N12 C23 N1 - Distance Angles C1 1.3352 (0.0097) C5 1.3490 (0.0094) 118.72 (0.64) Zn1 2.0699 (0.0062) 127.76 (0.52) 113.43 (0.49) N1 - C1 C5 N2 - Distance Angles C6 1.3107 (0.0095) H2A 0.8800 120.00 H2B 0.8800 120.00 120.00 N2 - C6 H2A N3 - Distance Angles C6 1.3140 (0.0089) N4 1.4152 (0.0082) 117.09 (0.58) Zn1 2.1087 (0.0059) 111.31 (0.47) 121.59 (0.41) N3 - C6 N4 N4 - Distance Angles C7 1.3126 (0.0091) N3 1.4152 (0.0082) 116.36 (0.59) Zn2 2.2160 (0.0059) 119.32 (0.47) 123.34 (0.41) N4 - C7 N3 N5 - Distance Angles C7 1.3225 (0.0091) H5A 0.8800 120.00 H5B 0.8800 120.00 120.00 N5 - C7 H5A N6 - Distance Angles C12 1.3254 (0.0095) C8 1.3464 (0.0090) 118.48 (0.62) Zn2 2.2172 (0.0059) 123.18 (0.48) 118.28 (0.47) N6 - C12 C8 N7 - Distance Angles C13 1.3213 (0.0098) C17 1.3507 (0.0090) 119.17 (0.63) Zn2 2.2579 (0.0061) 121.96 (0.48) 118.06 (0.49) N7 - C13 C17 N8 - Distance Angles C18 1.3206 (0.0094) H8A 0.8800 120.00 H8B 0.8800 120.00 120.00 N8 - C18 H8A N9 - Distance Angles C18 1.3091 (0.0094) N10 1.3936 (0.0087) 115.35 (0.59) Zn2 2.1511 (0.0061) 123.33 (0.50) 120.21 (0.43) N9 - C18 N10 N10 - Distance Angles C19 1.2964 (0.0096) N9 1.3936 (0.0087) 109.46 (0.58) N10 - C19 N11 - Distance Angles C19 1.3112 (0.0087) Zn1 2.0078 (0.0050) 115.64 (0.48) Zn2 2.2104 (0.0053) 113.69 (0.46) 128.24 (0.24) N11 - C19 Zn1 N12 - Distance Angles C20 1.3319 (0.0094) C24 1.3568 (0.0098) 118.85 (0.66) Zn1 2.1162 (0.0062) 111.63 (0.50) 129.50 (0.52) N12 - C20 C24 O1 - Distance Angles Zn1 2.0317 (0.0055) H1A 0.8409 (0.0190) 129.05 (4.02) H1B 0.8467 (0.0191) 124.83 (3.67) 105.99 (3.90) O1 - Zn1 H1A O11 - Distance Angles Zn2 2.1976 (0.0052) H11A 0.8482 (0.0192) 112.66 (3.01) H11B 0.8455 (0.0197) 113.57 (3.37) 103.33 (4.21) O11 - Zn2 H11A O12 - Distance Angles Zn2 2.1173 (0.0053) H12A 0.8454 (0.0195) 119.00 (3.57) H12B 0.8429 (0.0196) 121.67 (3.83) 105.70 (4.38) O12 - Zn2 H12A Zn1 - Distance Angles N11 2.0078 (0.0050) O1 2.0317 (0.0055) 106.19 (0.22) N1 2.0699 (0.0062) 147.41 (0.24) 105.13 (0.24) N3 2.1087 (0.0059) 84.99 (0.22) 104.88 (0.23) 78.53 (0.24) N12 2.1162 (0.0063) 79.34 (0.23) 95.68 (0.23) 106.27 (0.24) 156.98 (0.24) Zn1 - N11 O1 N1 N3 Zn2 - Distance Angles O12 2.1173 (0.0053) N9 2.1511 (0.0061) 86.13 (0.23) O11 2.1976 (0.0052) 175.83 (0.22) 94.13 (0.22) N11 2.2104 (0.0053) 90.44 (0.21) 70.40 (0.21) 85.73 (0.21) N4 2.2160 (0.0059) 86.96 (0.21) 148.67 (0.23) 90.68 (0.21) 79.15 (0.20) N6 2.2172 (0.0060) 100.48 (0.22) 139.23 (0.23) 82.04 (0.21) 148.48 (0.20) 72.10 (0.21) N7 2.2579 (0.0061) 92.95 (0.21) 70.48 (0.23) 91.06 (0.21) 140.38 (0.21) 140.44 (0.22) 69.03 (0.22) Zn2 - O12 N9 O11 N11 N4 N6 O31 - Distance Angles Cl31 1.4585 (0.0060) O31 - O32 - Distance Angles Cl31 1.4277 (0.0061) O32 - O33 - Distance Angles Cl31 1.4199 (0.0067) O33 - O34 - Distance Angles Cl31 1.4028 (0.0065) O34 - Cl31 - Distance Angles O34 1.4028 (0.0065) O33 1.4199 (0.0067) 109.58 (0.46) O32 1.4277 (0.0061) 111.23 (0.42) 110.74 (0.44) O31 1.4585 (0.0060) 108.79 (0.41) 108.81 (0.42) 107.62 (0.36) Cl31 - O34 O33 O32 O41 - Distance Angles Cl41 1.4397 (0.0062) O41 - O42 - Distance Angles Cl41 1.4464 (0.0067) O42 - O43 - Distance Angles Cl41 1.4116 (0.0059) O43 - O44 - Distance Angles Cl41 1.4398 (0.0063) O44 - Cl41 - Distance Angles O43 1.4116 (0.0059) O41 1.4397 (0.0062) 110.23 (0.39) O44 1.4398 (0.0063) 109.63 (0.42) 109.88 (0.40) O42 1.4464 (0.0067) 108.25 (0.40) 110.11 (0.37) 108.70 (0.45) Cl41 - O43 O41 O44 O51 - Distance Angles Cl51 1.4261 (0.0060) O51 - O52 - Distance Angles Cl51 1.4270 (0.0058) O52 - O53 - Distance Angles Cl51 1.4595 (0.0058) O53 - O54 - Distance Angles Cl51 1.4277 (0.0056) O54 - Cl51 - Distance Angles O51 1.4261 (0.0060) O52 1.4270 (0.0058) 110.20 (0.40) O54 1.4277 (0.0056) 110.58 (0.36) 110.26 (0.38) O53 1.4595 (0.0058) 108.11 (0.39) 107.44 (0.38) 110.17 (0.36) Cl51 - O51 O52 O54 O61 - Distance Angles H61A 0.8395 (0.0204) H61B 0.8417 (0.0201) 107.69 (5.04) O61 - H61A FMAP and GRID set by program FMAP 2 3 38 GRID -1.429 -1 -2 1.429 1 2 R1 = 0.1087 for 7835 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.08 at 0.2534 0.9471 0.2440 [ 1.07 A from ZN2 ] Deepest hole -0.77 at 0.2329 0.2479 0.1432 [ 0.98 A from ZN1 ] Mean = 0.00, Rms deviation from mean = 0.16 e/A^3, Highest memory used = 5089 / 56562 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2534 -0.0529 0.2440 1.00000 0.05 1.08 1.07 ZN2 1.40 N4 1.78 O12 2.16 H12A Q2 1 0.2244 -0.0364 0.2565 1.00000 0.05 1.07 1.44 O12 1.57 N4 1.60 H12A 1.64 ZN2 Q3 1 0.2980 0.0224 0.2726 1.00000 0.05 0.99 0.87 ZN2 1.36 N11 2.10 N4 2.16 N9 Q4 1 0.3029 0.2456 0.3489 1.00000 0.05 0.91 0.81 C20 0.85 C19 1.53 N12 1.55 N11 Q5 1 0.1682 0.2418 0.1664 1.00000 0.05 0.86 1.05 N1 1.07 ZN1 1.87 C5 1.96 N3 Shortest distances between peaks (including symmetry equivalents) 1 2 0.70 1 3 1.24 2 3 1.61 3 4 2.83 Time profile in seconds ----------------------- 0.05: Read and process instructions 0.00: Fit rigid groups 0.01: 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. 1.40: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 8.02: Structure factors and derivatives 33.53: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 2.80: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.19: Analysis of variance 0.07: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s93 finished at 22:46:38 Total CPU time: 47.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++