+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 14:43:08 on 09-Oct-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 03src0046 in P-1 CELL 0.71073 8.8185 9.1331 19.1308 84.397 79.078 77.729 ZERR 2.00 0.0002 0.0002 0.0004 0.001 0.001 0.001 LATT 1 SFAC C H BR N O UNIT 58 106 2 4 2 V = 1475.68 F(000) = 568.0 Mu = 1.41 mm-1 Cell Wt = 1051.29 Rho = 1.183 MERG 2 OMIT -3.00 55.00 OMIT 4 4 3 DFIX 0.84 H10 O1 H20 O1 DANG 1.37 H10 H20 FMAP 2 PLAN 10 SIZE 0.04 0.16 0.44 ACTA BOND $H WGHT 0.03170 2.47200 L.S. 15 TEMP -153.00 FVAR 0.74982 C1 1 0.921008 0.008323 0.751090 11.00000 0.03794 0.03084 = 0.01848 0.00243 -0.00433 -0.00442 AFIX 137 H1A 2 0.851941 -0.060267 0.746891 11.00000 -1.50000 H1B 2 0.904465 0.035086 0.800726 11.00000 -1.50000 H1C 2 1.031164 -0.040907 0.736388 11.00000 -1.50000 AFIX 0 C2 1 0.882858 0.149851 0.703319 11.00000 0.02805 0.02275 = 0.02109 -0.00221 -0.00442 -0.00389 AFIX 23 H2A 2 0.771737 0.199419 0.718726 11.00000 -1.20000 H2B 2 0.950285 0.220156 0.709184 11.00000 -1.20000 AFIX 0 C3 1 0.907789 0.118244 0.624961 11.00000 0.02326 0.01792 = 0.01789 -0.00076 -0.00399 -0.00337 AFIX 23 H3A 2 0.840334 0.047768 0.619352 11.00000 -1.20000 H3B 2 1.018833 0.068100 0.609862 11.00000 -1.20000 AFIX 0 C4 1 0.870811 0.258072 0.575800 11.00000 0.02284 0.01741 = 0.01957 -0.00137 -0.00497 -0.00388 AFIX 23 H4A 2 0.938016 0.328818 0.581360 11.00000 -1.20000 H4B 2 0.759598 0.308069 0.590587 11.00000 -1.20000 AFIX 0 C5 1 0.897139 0.224300 0.497223 11.00000 0.02694 0.01664 = 0.02003 -0.00052 -0.00490 -0.00477 AFIX 23 H5A 2 1.007967 0.172909 0.482729 11.00000 -1.20000 H5B 2 0.828917 0.154495 0.491675 11.00000 -1.20000 AFIX 0 C6 1 0.862532 0.363867 0.447295 11.00000 0.02480 0.01755 = 0.02014 -0.00046 -0.00609 -0.00376 AFIX 23 H6A 2 0.751490 0.415058 0.461385 11.00000 -1.20000 H6B 2 0.930430 0.434023 0.452781 11.00000 -1.20000 AFIX 0 C7 1 0.890451 0.327543 0.369046 11.00000 0.02854 0.01714 = 0.01972 0.00074 -0.00646 -0.00458 AFIX 23 H7A 2 1.000656 0.273609 0.355538 11.00000 -1.20000 H7B 2 0.820524 0.259339 0.363538 11.00000 -1.20000 AFIX 0 C8 1 0.860842 0.465539 0.318121 11.00000 0.02575 0.01688 = 0.01991 0.00025 -0.00731 -0.00508 AFIX 23 H8A 2 0.932937 0.532526 0.322408 11.00000 -1.20000 H8B 2 0.751500 0.521101 0.332201 11.00000 -1.20000 AFIX 0 C9 1 0.885235 0.426095 0.240206 11.00000 0.02687 0.01579 = 0.02100 0.00095 -0.00824 -0.00383 AFIX 23 H9A 2 0.991900 0.363975 0.227303 11.00000 -1.20000 H9B 2 0.807792 0.365189 0.235346 11.00000 -1.20000 AFIX 0 C10 1 0.867454 0.564031 0.188101 11.00000 0.02058 0.01531 = 0.01956 0.00120 -0.00749 -0.00622 AFIX 23 H10A 2 0.947181 0.623198 0.191899 11.00000 -1.20000 H10B 2 0.762065 0.627793 0.201999 11.00000 -1.20000 AFIX 0 C11 1 0.886572 0.525302 0.110457 11.00000 0.01412 0.01700 = 0.02044 0.00103 -0.00468 -0.00557 AFIX 23 H11A 2 0.889744 0.617654 0.078939 11.00000 -1.20000 H11B 2 0.987740 0.454237 0.097502 11.00000 -1.20000 AFIX 0 C12 1 0.762214 0.312237 0.092863 11.00000 0.01501 0.01286 = 0.01694 0.00018 -0.00346 -0.00020 AFIX 43 H12 2 0.854224 0.235852 0.092226 11.00000 -1.20000 AFIX 0 C13 1 0.602479 0.534652 0.098146 11.00000 0.01408 0.01329 = 0.01231 -0.00093 -0.00189 -0.00239 C14 1 0.534343 0.687159 0.101399 11.00000 0.01878 0.01191 = 0.02073 -0.00215 -0.00276 -0.00331 AFIX 43 H14 2 0.593582 0.760230 0.105936 11.00000 -1.20000 AFIX 0 C15 1 0.375924 0.725419 0.097634 11.00000 0.02061 0.01203 = 0.02248 -0.00229 -0.00320 -0.00080 AFIX 43 H15 2 0.324557 0.827841 0.099916 11.00000 -1.20000 AFIX 0 C16 1 0.287804 0.617216 0.090503 11.00000 0.01436 0.01672 = 0.02128 -0.00242 -0.00298 0.00014 AFIX 43 H16 2 0.178914 0.648867 0.088283 11.00000 -1.20000 AFIX 0 C17 1 0.355698 0.466018 0.086645 11.00000 0.01593 0.01339 = 0.02002 -0.00148 -0.00300 -0.00252 AFIX 43 H17 2 0.296879 0.393048 0.081448 11.00000 -1.20000 AFIX 0 C18 1 0.515414 0.427622 0.090856 11.00000 0.01589 0.01162 = 0.01376 -0.00121 -0.00331 -0.00155 C19 1 0.579154 0.142854 0.082238 11.00000 0.02124 0.00803 = 0.02329 -0.00514 -0.00590 -0.00125 AFIX 23 H19A 2 0.675595 0.069725 0.064273 11.00000 -1.20000 H19B 2 0.506267 0.154066 0.047694 11.00000 -1.20000 AFIX 0 C20 1 0.501570 0.083706 0.154217 11.00000 0.01890 0.01060 = 0.02428 -0.00191 -0.00533 -0.00456 AFIX 23 H20A 2 0.460874 -0.005795 0.147134 11.00000 -1.20000 H20B 2 0.410292 0.161185 0.173411 11.00000 -1.20000 AFIX 0 C21 1 0.610309 0.041376 0.209293 11.00000 0.02031 0.01840 = 0.02282 0.00148 -0.00643 -0.00563 AFIX 23 H21A 2 0.639770 0.133144 0.221631 11.00000 -1.20000 H21B 2 0.708034 -0.026614 0.188259 11.00000 -1.20000 AFIX 0 C22 1 0.533567 -0.035627 0.277046 11.00000 0.02217 0.01926 = 0.02260 0.00186 -0.00533 -0.00544 AFIX 23 H22A 2 0.506771 -0.128483 0.264427 11.00000 -1.20000 H22B 2 0.433841 0.031378 0.296696 11.00000 -1.20000 AFIX 0 C23 1 0.635539 -0.076126 0.334877 11.00000 0.02180 0.02071 = 0.02430 0.00179 -0.00463 -0.00464 AFIX 23 H23A 2 0.734942 -0.144199 0.315745 11.00000 -1.20000 H23B 2 0.662752 0.016313 0.347748 11.00000 -1.20000 AFIX 0 C24 1 0.554183 -0.151739 0.401600 11.00000 0.02126 0.02239 = 0.02360 0.00434 -0.00506 -0.00367 AFIX 23 H24A 2 0.528629 -0.244788 0.388505 11.00000 -1.20000 H24B 2 0.453561 -0.084274 0.419739 11.00000 -1.20000 AFIX 0 C25 1 0.651139 -0.191457 0.461474 11.00000 0.02121 0.02215 = 0.02398 0.00221 -0.00484 -0.00343 AFIX 23 H25A 2 0.751071 -0.260505 0.443913 11.00000 -1.20000 H25B 2 0.677759 -0.098897 0.474543 11.00000 -1.20000 AFIX 0 C26 1 0.564885 -0.265076 0.527703 11.00000 0.02273 0.02083 = 0.02434 0.00153 -0.00258 -0.00192 AFIX 23 H26A 2 0.537638 -0.357032 0.514291 11.00000 -1.20000 H26B 2 0.465086 -0.195649 0.545068 11.00000 -1.20000 AFIX 0 C27 1 0.659042 -0.306761 0.588379 11.00000 0.02420 0.01867 = 0.02254 0.00102 -0.00325 -0.00027 AFIX 23 H27A 2 0.758909 -0.376268 0.571188 11.00000 -1.20000 H27B 2 0.685977 -0.214923 0.602096 11.00000 -1.20000 AFIX 0 C28 1 0.570741 -0.380580 0.654053 11.00000 0.02784 0.02611 = 0.02489 0.00248 0.00055 0.00067 AFIX 23 H28A 2 0.471402 -0.310658 0.671549 11.00000 -1.20000 H28B 2 0.542843 -0.471854 0.640239 11.00000 -1.20000 AFIX 0 C29 1 0.665551 -0.423624 0.714374 11.00000 0.04640 0.02951 = 0.02059 0.00127 -0.00438 0.00276 AFIX 137 H29A 2 0.763640 -0.493731 0.697634 11.00000 -1.50000 H29B 2 0.603670 -0.471527 0.754700 11.00000 -1.50000 H29C 2 0.690310 -0.333292 0.729578 11.00000 -1.50000 AFIX 0 BR1 3 0.171163 0.157550 0.046918 11.00000 0.02041 0.01850 = 0.03859 -0.00650 -0.00409 -0.00449 N1 4 0.756503 0.457783 0.099087 11.00000 0.01443 0.01350 = 0.01666 0.00001 -0.00434 -0.00267 N2 4 0.620773 0.289373 0.087680 11.00000 0.01603 0.00905 = 0.01725 -0.00243 -0.00372 -0.00094 O1 5 0.036207 0.113259 -0.093876 11.00000 0.04163 0.03823 = 0.04284 0.00002 -0.01134 -0.00890 H20 2 -0.047022 0.021698 -0.090237 11.00000 -1.500 H10 2 0.060863 0.118525 -0.052302 11.00000 -1.500 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 Covalent radii and connectivity table for 03src0046 in P-1 C 0.770 H 0.320 BR 1.140 N 0.700 O 0.660 C1 - C2 C2 - C3 C1 C3 - C2 C4 C4 - C3 C5 C5 - C4 C6 C6 - C7 C5 C7 - C8 C6 C8 - C7 C9 C9 - C10 C8 C10 - C9 C11 C11 - N1 C10 C12 - N2 N1 C13 - N1 C18 C14 C14 - C15 C13 C15 - C14 C16 C16 - C17 C15 C17 - C16 C18 C18 - C17 C13 N2 C19 - N2 C20 C20 - C19 C21 C21 - C22 C20 C22 - C21 C23 C23 - C24 C22 C24 - C23 C25 C25 - C26 C24 C26 - C25 C27 C27 - C26 C28 C28 - C29 C27 C29 - C28 Br1 - no bonds found N1 - C12 C13 C11 N2 - C12 C18 C19 O1 - no bonds found 20109 Reflections read, of which 5 rejected -11 =< h =< 11, -11 =< k =< 11, -24 =< l =< 24, Max. 2-theta = 54.98 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 8 2 7 208.96 6.93 2 34.69 -3 -5 11 106.35 7.70 2 39.31 7 4 18 8.86 1.56 3 13.12 3 Inconsistent equivalents 6555 Unique reflections, of which 0 suppressed R(int) = 0.0701 R(sigma) = 0.0545 Friedel opposites merged Maximum memory for data reduction = 3975 / 65496 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 = 4992 / 384332 wR2 = 0.1136 before cycle 1 for 6555 data and 306 / 306 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 1.2137 0.8400 0.3737 0.0200 DFIX H20 O1 1.7200 1.3700 0.3500 0.0400 DANG H10 H20 Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.265 0.350 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.080 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0317 * P )^2 + 2.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.74971 0.00112 -0.103 OSF 301 -0.02983 0.00413 4.164 x H20 302 0.03924 0.00371 4.723 y H20 Mean shift/su = 0.069 Maximum = 4.723 for y H20 Max. shift = 0.245 A for H20 Max. dU = 0.000 for O1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4992 / 384332 wR2 = 0.1136 before cycle 2 for 6555 data and 306 / 306 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.9726 0.8400 0.1326 0.0200 DFIX H20 O1 1.4988 1.3700 0.1288 0.0400 DANG H10 H20 Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.097 0.129 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.051 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0317 * P )^2 + 2.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.74957 0.00109 -0.123 OSF Mean shift/su = 0.037 Maximum = 2.209 for y H20 Max. shift = 0.102 A for H20 Max. dU = 0.000 for O1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4992 / 384332 wR2 = 0.1137 before cycle 3 for 6555 data and 306 / 306 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.043 0.044 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.048; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0317 * P )^2 + 2.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.74956 0.00108 -0.007 OSF Mean shift/su = 0.011 Maximum = 0.579 for z H20 Max. shift = 0.025 A for H20 Max. dU = 0.000 for O1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4992 / 384332 wR2 = 0.1138 before cycle 4 for 6555 data and 306 / 306 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.041 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.048; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0317 * P )^2 + 2.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.74956 0.00108 0.000 OSF Mean shift/su = 0.003 Maximum = -0.166 for x H20 Max. shift = 0.007 A for H20 Max. dU = 0.000 for O1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 4992 / 384332 wR2 = 0.1138 before cycle 5 for 6555 data and 306 / 306 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.043 0.036 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.048; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0317 * P )^2 + 2.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.74957 0.00108 0.001 OSF Mean shift/su = 0.001 Maximum = 0.028 for x H10 Max. shift = 0.001 A for H10 Max. dU = 0.000 for O1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 4992 / 384332 wR2 = 0.1137 before cycle 6 for 6555 data and 306 / 306 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.043 0.036 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.048; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0317 * P )^2 + 2.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.74956 0.00108 -0.001 OSF Mean shift/su = 0.000 Maximum = 0.013 for x H10 Max. shift = 0.001 A for H10 Max. dU = 0.000 for C15 Least-squares cycle 7 Maximum vector length = 511 Memory required = 4992 / 384332 wR2 = 0.1137 before cycle 7 for 6555 data and 306 / 306 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.043 0.036 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.048; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0317 * P )^2 + 2.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.74956 0.00108 0.000 OSF Mean shift/su = 0.000 Maximum = 0.005 for x H10 Max. shift = 0.000 A for H10 Max. dU = 0.000 for C7 Least-squares cycle 8 Maximum vector length = 511 Memory required = 4992 / 384332 wR2 = 0.1137 before cycle 8 for 6555 data and 306 / 306 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.043 0.036 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.048; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0317 * P )^2 + 2.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.74956 0.00108 0.000 OSF Mean shift/su = 0.000 Maximum = 0.002 for x H10 Max. shift = 0.000 A for H10 Max. dU = 0.000 for O1 Least-squares cycle 9 Maximum vector length = 511 Memory required = 4992 / 384332 wR2 = 0.1137 before cycle 9 for 6555 data and 306 / 306 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.043 0.036 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.048; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0317 * P )^2 + 2.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.74956 0.00108 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for x H10 Max. shift = 0.000 A for H10 Max. dU = 0.000 for C1 Least-squares cycle 10 Maximum vector length = 511 Memory required = 4992 / 384332 wR2 = 0.1137 before cycle 10 for 6555 data and 306 / 306 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.043 0.036 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.048; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0317 * P )^2 + 2.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.74956 0.00108 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x H10 Max. shift = 0.000 A for H10 Max. dU = 0.000 for O1 Least-squares cycle 11 Maximum vector length = 511 Memory required = 4992 / 384332 wR2 = 0.1137 before cycle 11 for 6555 data and 306 / 306 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.043 0.036 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.048; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0317 * P )^2 + 2.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.74956 0.00108 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z C4 Max. shift = 0.000 A for H10 Max. dU = 0.000 for C6 Least-squares cycle 12 Maximum vector length = 511 Memory required = 4992 / 384332 wR2 = 0.1137 before cycle 12 for 6555 data and 306 / 306 parameters Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.043 0.036 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.048; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0317 * P )^2 + 2.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.74957 0.00108 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H10 Max. dU = 0.000 for C13 Least-squares cycle 13 Maximum vector length = 511 Memory required = 4992 / 384332 wR2 = 0.1137 before cycle 13 for 6555 data and 306 / 306 parameters Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.043 0.036 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.048; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0317 * P )^2 + 2.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.74957 0.00108 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z C4 Max. shift = 0.000 A for H10 Max. dU = 0.000 for C8 Least-squares cycle 14 Maximum vector length = 511 Memory required = 4992 / 384332 wR2 = 0.1137 before cycle 14 for 6555 data and 306 / 306 parameters Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.043 0.036 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.048; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0317 * P )^2 + 2.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.74957 0.00108 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H20 Max. dU = 0.000 for O1 Least-squares cycle 15 Maximum vector length = 511 Memory required = 4992 / 384332 wR2 = 0.1137 before cycle 15 for 6555 data and 306 / 306 parameters Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.043 0.036 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.048; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0317 * P )^2 + 2.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.74957 0.00108 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H10 Max. dU = 0.000 for C19 Largest correlation matrix elements -0.770 y H20 / x H20 0.548 U22 Br1 / OSF -0.588 z H10 / x H10 0.533 U11 Br1 / OSF Idealized hydrogen atom generation before cycle 16 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.8519 -0.0602 0.7469 137 0.980 0.000 C1 C2 H1A H1B 0.9045 0.0351 0.8007 137 0.980 0.000 C1 C2 H1A H1C 1.0311 -0.0409 0.7364 137 0.980 0.000 C1 C2 H1A H2A 0.7717 0.1994 0.7187 23 0.990 0.000 C2 C3 C1 H2B 0.9503 0.2202 0.7092 23 0.990 0.000 C2 C3 C1 H3A 0.8403 0.0478 0.6193 23 0.990 0.000 C3 C2 C4 H3B 1.0188 0.0681 0.6099 23 0.990 0.000 C3 C2 C4 H4A 0.9380 0.3288 0.5814 23 0.990 0.000 C4 C3 C5 H4B 0.7596 0.3081 0.5906 23 0.990 0.000 C4 C3 C5 H5A 0.8289 0.1545 0.4917 23 0.990 0.000 C5 C4 C6 H5B 1.0080 0.1729 0.4827 23 0.990 0.000 C5 C4 C6 H6A 0.7515 0.4151 0.4614 23 0.990 0.000 C6 C7 C5 H6B 0.9304 0.4340 0.4528 23 0.990 0.000 C6 C7 C5 H7A 1.0006 0.2736 0.3555 23 0.990 0.000 C7 C8 C6 H7B 0.8205 0.2593 0.3636 23 0.990 0.000 C7 C8 C6 H8A 0.9329 0.5325 0.3224 23 0.990 0.000 C8 C7 C9 H8B 0.7515 0.5211 0.3322 23 0.990 0.000 C8 C7 C9 H9A 0.9919 0.3640 0.2273 23 0.990 0.000 C9 C10 C8 H9B 0.8078 0.3652 0.2353 23 0.990 0.000 C9 C10 C8 H10A 0.9471 0.6232 0.1919 23 0.990 0.000 C10 C9 C11 H10B 0.7620 0.6278 0.2020 23 0.990 0.000 C10 C9 C11 H11A 0.8898 0.6177 0.0789 23 0.990 0.000 C11 N1 C10 H11B 0.9877 0.4542 0.0975 23 0.990 0.000 C11 N1 C10 H12 0.8542 0.2358 0.0922 43 0.950 0.000 C12 N2 N1 H14 0.5936 0.7602 0.1059 43 0.950 0.000 C14 C15 C13 H15 0.3246 0.8278 0.0999 43 0.950 0.000 C15 C14 C16 H16 0.1789 0.6489 0.0883 43 0.950 0.000 C16 C17 C15 H17 0.2969 0.3930 0.0815 43 0.950 0.000 C17 C16 C18 H19A 0.6756 0.0697 0.0643 23 0.990 0.000 C19 N2 C20 H19B 0.5063 0.1541 0.0477 23 0.990 0.000 C19 N2 C20 H20A 0.4609 -0.0058 0.1471 23 0.990 0.000 C20 C19 C21 H20B 0.4103 0.1612 0.1734 23 0.990 0.000 C20 C19 C21 H21A 0.7080 -0.0266 0.1883 23 0.990 0.000 C21 C22 C20 H21B 0.6398 0.1331 0.2216 23 0.990 0.000 C21 C22 C20 H22A 0.5068 -0.1285 0.2644 23 0.990 0.000 C22 C21 C23 H22B 0.4338 0.0314 0.2967 23 0.990 0.000 C22 C21 C23 H23A 0.7350 -0.1442 0.3158 23 0.990 0.000 C23 C24 C22 H23B 0.6628 0.0163 0.3478 23 0.990 0.000 C23 C24 C22 H24A 0.5287 -0.2448 0.3885 23 0.990 0.000 C24 C23 C25 H24B 0.4536 -0.0843 0.4197 23 0.990 0.000 C24 C23 C25 H25A 0.7511 -0.2605 0.4439 23 0.990 0.000 C25 C26 C24 H25B 0.6777 -0.0989 0.4746 23 0.990 0.000 C25 C26 C24 H26A 0.5377 -0.3570 0.5143 23 0.990 0.000 C26 C25 C27 H26B 0.4651 -0.1957 0.5451 23 0.990 0.000 C26 C25 C27 H27A 0.6859 -0.2149 0.6021 23 0.990 0.000 C27 C26 C28 H27B 0.7589 -0.3762 0.5712 23 0.990 0.000 C27 C26 C28 H28A 0.4714 -0.3107 0.6715 23 0.990 0.000 C28 C29 C27 H28B 0.5429 -0.4719 0.6402 23 0.990 0.000 C28 C29 C27 H29A 0.7637 -0.4936 0.6976 137 0.980 0.000 C29 C28 H29A H29B 0.6037 -0.4717 0.7547 137 0.980 0.000 C29 C28 H29A H29C 0.6901 -0.3333 0.7297 137 0.980 0.000 C29 C28 H29A 03src0046 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.92101 0.00836 0.75109 1.00000 0.03789 0.03077 0.01847 0.00241 -0.00434 -0.00448 0.02973 0.00459 0.00037 0.00033 0.00014 0.00000 0.00163 0.00153 0.00130 0.00110 0.00118 0.00123 0.00062 H1A 0.85190 -0.06021 0.74691 1.00000 0.04460 0.00000 0.00000 H1B 0.90452 0.03513 0.80072 1.00000 0.04460 0.00000 0.00000 H1C 1.03115 -0.04090 0.73637 1.00000 0.04460 0.00000 0.00000 C2 0.88286 0.14986 0.70333 1.00000 0.02804 0.02267 0.02104 -0.00228 -0.00447 -0.00394 0.02399 0.00407 0.00033 0.00030 0.00014 0.00000 0.00138 0.00133 0.00129 0.00101 0.00107 0.00105 0.00055 H2A 0.77174 0.19943 0.71874 1.00000 0.02879 0.00000 0.00000 H2B 0.95029 0.22016 0.70919 1.00000 0.02879 0.00000 0.00000 C3 0.90777 0.11826 0.62496 1.00000 0.02323 0.01795 0.01786 -0.00081 -0.00402 -0.00335 0.01975 0.00377 0.00031 0.00028 0.00013 0.00000 0.00124 0.00121 0.00119 0.00093 0.00099 0.00096 0.00050 H3A 0.84029 0.04781 0.61935 1.00000 0.02370 0.00000 0.00000 H3B 1.01880 0.06810 0.60985 1.00000 0.02370 0.00000 0.00000 C4 0.87082 0.25808 0.57580 1.00000 0.02281 0.01742 0.01954 -0.00137 -0.00498 -0.00389 0.01975 0.00374 0.00031 0.00028 0.00013 0.00000 0.00124 0.00120 0.00122 0.00093 0.00100 0.00095 0.00050 H4A 0.93804 0.32881 0.58136 1.00000 0.02370 0.00000 0.00000 H4B 0.75961 0.30809 0.59059 1.00000 0.02370 0.00000 0.00000 C5 0.89713 0.22433 0.49722 1.00000 0.02692 0.01660 0.02004 -0.00060 -0.00492 -0.00478 0.02104 0.00384 0.00032 0.00028 0.00013 0.00000 0.00132 0.00120 0.00124 0.00095 0.00104 0.00098 0.00051 H5A 0.82891 0.15452 0.49168 1.00000 0.02524 0.00000 0.00000 H5B 1.00796 0.17293 0.48273 1.00000 0.02524 0.00000 0.00000 C6 0.86254 0.36386 0.44729 1.00000 0.02476 0.01756 0.02011 -0.00049 -0.00607 -0.00379 0.02062 0.00381 0.00031 0.00028 0.00013 0.00000 0.00127 0.00122 0.00124 0.00096 0.00103 0.00097 0.00051 H6A 0.75150 0.41506 0.46138 1.00000 0.02475 0.00000 0.00000 H6B 0.93044 0.43401 0.45277 1.00000 0.02475 0.00000 0.00000 C7 0.89043 0.32754 0.36905 1.00000 0.02853 0.01710 0.01969 0.00069 -0.00647 -0.00460 0.02158 0.00388 0.00032 0.00028 0.00013 0.00000 0.00136 0.00121 0.00124 0.00095 0.00105 0.00099 0.00052 H7A 1.00064 0.27360 0.35554 1.00000 0.02589 0.00000 0.00000 H7B 0.82050 0.25934 0.36355 1.00000 0.02589 0.00000 0.00000 C8 0.86082 0.46555 0.31811 1.00000 0.02573 0.01687 0.01991 0.00026 -0.00733 -0.00508 0.02035 0.00378 0.00031 0.00028 0.00013 0.00000 0.00130 0.00119 0.00122 0.00094 0.00102 0.00097 0.00051 H8A 0.93291 0.53255 0.32240 1.00000 0.02442 0.00000 0.00000 H8B 0.75148 0.52111 0.33219 1.00000 0.02442 0.00000 0.00000 C9 0.88524 0.42609 0.24021 1.00000 0.02687 0.01579 0.02100 0.00091 -0.00823 -0.00379 0.02088 0.00382 0.00032 0.00028 0.00013 0.00000 0.00132 0.00118 0.00125 0.00094 0.00105 0.00097 0.00051 H9A 0.99191 0.36399 0.22731 1.00000 0.02505 0.00000 0.00000 H9B 0.80782 0.36517 0.23535 1.00000 0.02505 0.00000 0.00000 C10 0.86744 0.56402 0.18810 1.00000 0.02056 0.01522 0.01965 0.00119 -0.00747 -0.00625 0.01769 0.00354 0.00029 0.00027 0.00013 0.00000 0.00118 0.00114 0.00119 0.00091 0.00097 0.00091 0.00048 H10A 0.94715 0.62321 0.19190 1.00000 0.02122 0.00000 0.00000 H10B 0.76204 0.62777 0.20199 1.00000 0.02122 0.00000 0.00000 C11 0.88658 0.52530 0.11046 1.00000 0.01403 0.01696 0.02043 0.00104 -0.00466 -0.00560 0.01668 0.00350 0.00027 0.00027 0.00013 0.00000 0.00109 0.00114 0.00119 0.00090 0.00093 0.00088 0.00047 H11A 0.88975 0.61765 0.07894 1.00000 0.02002 0.00000 0.00000 H11B 0.98774 0.45423 0.09751 1.00000 0.02002 0.00000 0.00000 C12 0.76220 0.31223 0.09286 1.00000 0.01505 0.01285 0.01689 0.00020 -0.00346 -0.00020 0.01530 0.00352 0.00027 0.00026 0.00012 0.00000 0.00108 0.00109 0.00112 0.00086 0.00089 0.00085 0.00045 H12 0.85422 0.23584 0.09221 1.00000 0.01836 0.00000 0.00000 C13 0.60248 0.53465 0.09815 1.00000 0.01401 0.01330 0.01232 -0.00094 -0.00187 -0.00239 0.01330 0.00338 0.00027 0.00025 0.00012 0.00000 0.00105 0.00108 0.00104 0.00082 0.00085 0.00084 0.00044 C14 0.53434 0.68715 0.10139 1.00000 0.01869 0.01185 0.02070 -0.00211 -0.00274 -0.00326 0.01706 0.00363 0.00028 0.00026 0.00013 0.00000 0.00115 0.00109 0.00119 0.00088 0.00095 0.00087 0.00047 H14 0.59359 0.76022 0.10592 1.00000 0.02047 0.00000 0.00000 C15 0.37592 0.72541 0.09764 1.00000 0.02064 0.01202 0.02237 -0.00225 -0.00317 -0.00086 0.01870 0.00372 0.00029 0.00027 0.00013 0.00000 0.00120 0.00111 0.00124 0.00090 0.00098 0.00090 0.00049 H15 0.32455 0.82783 0.09993 1.00000 0.02244 0.00000 0.00000 C16 0.28780 0.61721 0.09049 1.00000 0.01431 0.01670 0.02127 -0.00235 -0.00296 0.00011 0.01784 0.00370 0.00028 0.00027 0.00013 0.00000 0.00109 0.00117 0.00121 0.00092 0.00093 0.00088 0.00048 H16 0.17892 0.64885 0.08826 1.00000 0.02141 0.00000 0.00000 C17 0.35572 0.46602 0.08664 1.00000 0.01596 0.01330 0.02007 -0.00152 -0.00302 -0.00256 0.01647 0.00362 0.00028 0.00026 0.00013 0.00000 0.00111 0.00111 0.00117 0.00088 0.00093 0.00087 0.00046 H17 0.29691 0.39304 0.08145 1.00000 0.01977 0.00000 0.00000 C18 0.51538 0.42763 0.09085 1.00000 0.01588 0.01157 0.01366 -0.00120 -0.00331 -0.00154 0.01375 0.00341 0.00027 0.00025 0.00012 0.00000 0.00108 0.00106 0.00107 0.00082 0.00087 0.00085 0.00044 C19 0.57914 0.14284 0.08225 1.00000 0.02129 0.00795 0.02327 -0.00516 -0.00585 -0.00129 0.01719 0.00349 0.00029 0.00025 0.00013 0.00000 0.00118 0.00105 0.00123 0.00088 0.00098 0.00086 0.00048 H19A 0.67557 0.06970 0.06429 1.00000 0.02063 0.00000 0.00000 H19B 0.50626 0.15406 0.04771 1.00000 0.02063 0.00000 0.00000 C20 0.50156 0.08371 0.15421 1.00000 0.01888 0.01053 0.02424 -0.00192 -0.00537 -0.00450 0.01737 0.00351 0.00028 0.00026 0.00013 0.00000 0.00115 0.00108 0.00125 0.00090 0.00098 0.00087 0.00048 H20A 0.46087 -0.00579 0.14712 1.00000 0.02084 0.00000 0.00000 H20B 0.41028 0.16118 0.17340 1.00000 0.02084 0.00000 0.00000 C21 0.61031 0.04136 0.20930 1.00000 0.02028 0.01835 0.02279 0.00142 -0.00639 -0.00566 0.02003 0.00375 0.00030 0.00028 0.00013 0.00000 0.00121 0.00122 0.00126 0.00097 0.00101 0.00095 0.00050 H21A 0.70804 -0.02663 0.18827 1.00000 0.02403 0.00000 0.00000 H21B 0.63977 0.13313 0.22165 1.00000 0.02403 0.00000 0.00000 C22 0.53357 -0.03563 0.27704 1.00000 0.02213 0.01921 0.02261 0.00189 -0.00536 -0.00541 0.02113 0.00387 0.00030 0.00029 0.00014 0.00000 0.00124 0.00124 0.00128 0.00097 0.00103 0.00097 0.00051 H22A 0.50678 -0.12849 0.26442 1.00000 0.02536 0.00000 0.00000 H22B 0.43384 0.03138 0.29669 1.00000 0.02536 0.00000 0.00000 C23 0.63555 -0.07613 0.33488 1.00000 0.02177 0.02064 0.02434 0.00176 -0.00461 -0.00460 0.02232 0.00398 0.00031 0.00029 0.00014 0.00000 0.00125 0.00128 0.00132 0.00101 0.00105 0.00099 0.00053 H23A 0.73496 -0.14419 0.31576 1.00000 0.02678 0.00000 0.00000 H23B 0.66275 0.01631 0.34776 1.00000 0.02678 0.00000 0.00000 C24 0.55420 -0.15174 0.40159 1.00000 0.02129 0.02231 0.02351 0.00432 -0.00504 -0.00369 0.02270 0.00411 0.00031 0.00030 0.00014 0.00000 0.00124 0.00129 0.00130 0.00101 0.00104 0.00099 0.00053 H24A 0.52867 -0.24479 0.38849 1.00000 0.02724 0.00000 0.00000 H24B 0.45356 -0.08428 0.41972 1.00000 0.02724 0.00000 0.00000 C25 0.65113 -0.19145 0.46149 1.00000 0.02110 0.02210 0.02398 0.00220 -0.00486 -0.00341 0.02264 0.00406 0.00031 0.00030 0.00014 0.00000 0.00124 0.00129 0.00131 0.00101 0.00105 0.00100 0.00053 H25A 0.75107 -0.26049 0.44394 1.00000 0.02717 0.00000 0.00000 H25B 0.67772 -0.09888 0.47456 1.00000 0.02717 0.00000 0.00000 C26 0.56491 -0.26507 0.52770 1.00000 0.02267 0.02088 0.02426 0.00150 -0.00260 -0.00187 0.02337 0.00417 0.00031 0.00030 0.00014 0.00000 0.00128 0.00129 0.00133 0.00101 0.00106 0.00100 0.00054 H26A 0.53768 -0.35703 0.51429 1.00000 0.02804 0.00000 0.00000 H26B 0.46510 -0.19565 0.54507 1.00000 0.02804 0.00000 0.00000 C27 0.65902 -0.30675 0.58838 1.00000 0.02410 0.01863 0.02254 0.00099 -0.00327 -0.00028 0.02261 0.00411 0.00031 0.00029 0.00014 0.00000 0.00130 0.00124 0.00129 0.00098 0.00105 0.00099 0.00053 H27A 0.68594 -0.21491 0.60210 1.00000 0.02713 0.00000 0.00000 H27B 0.75890 -0.37625 0.57119 1.00000 0.02713 0.00000 0.00000 C28 0.57075 -0.38058 0.65405 1.00000 0.02779 0.02606 0.02482 0.00249 0.00047 0.00069 0.02808 0.00468 0.00034 0.00032 0.00015 0.00000 0.00142 0.00142 0.00140 0.00109 0.00113 0.00111 0.00060 H28A 0.47140 -0.31067 0.67154 1.00000 0.03370 0.00000 0.00000 H28B 0.54286 -0.47186 0.64023 1.00000 0.03370 0.00000 0.00000 C29 0.66554 -0.42365 0.71439 1.00000 0.04644 0.02945 0.02064 0.00124 -0.00442 0.00287 0.03412 0.00501 0.00039 0.00034 0.00015 0.00000 0.00182 0.00154 0.00138 0.00113 0.00128 0.00131 0.00069 H29A 0.76372 -0.49362 0.69763 1.00000 0.05118 0.00000 0.00000 H29B 0.60371 -0.47171 0.75468 1.00000 0.05118 0.00000 0.00000 H29C 0.69013 -0.33330 0.72966 1.00000 0.05118 0.00000 0.00000 Br1 0.17116 0.15755 0.04692 1.00000 0.02039 0.01847 0.03859 -0.00651 -0.00409 -0.00448 0.02553 0.00039 0.00003 0.00003 0.00002 0.00000 0.00014 0.00014 0.00017 0.00010 0.00011 0.00009 0.00009 N1 0.75650 0.45779 0.09909 1.00000 0.01435 0.01347 0.01668 -0.00002 -0.00438 -0.00265 0.01468 0.00291 0.00023 0.00022 0.00010 0.00000 0.00093 0.00094 0.00097 0.00074 0.00077 0.00074 0.00039 N2 0.62079 0.28936 0.08768 1.00000 0.01599 0.00906 0.01719 -0.00248 -0.00371 -0.00091 0.01409 0.00288 0.00023 0.00021 0.00010 0.00000 0.00094 0.00089 0.00096 0.00072 0.00077 0.00072 0.00039 O1 0.03655 0.11361 -0.09404 1.00000 0.04209 0.03875 0.04301 0.00031 -0.01181 -0.01098 0.04043 0.00364 0.00029 0.00027 0.00013 0.00000 0.00134 0.00131 0.00135 0.00105 0.00110 0.00102 0.00054 H20 -0.02744 0.04858 -0.08595 1.00000 0.06065 0.04229 0.00416 0.00387 0.00211 0.00000 0.00000 H10 0.06252 0.12138 -0.05263 1.00000 0.06065 0.03840 0.00482 0.00461 0.00141 0.00000 0.00000 Final Structure Factor Calculation for 03src0046 in P-1 Total number of l.s. parameters = 306 Maximum vector length = 511 Memory required = 4686 / 24017 wR2 = 0.1137 before cycle 16 for 6555 data and 0 / 306 parameters Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.043 0.036 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.048; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0317 * P )^2 + 2.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0465 for 5755 Fo > 4sig(Fo) and 0.0558 for all 6555 data wR2 = 0.1137, GooF = S = 1.048, Restrained GooF = 1.049 for all data Occupancy sum of asymmetric unit = 33.00 for non-hydrogen and 53.00 for hydrogen atoms Principal mean square atomic displacements U 0.0402 0.0315 0.0175 C1 0.0286 0.0230 0.0204 C2 0.0236 0.0182 0.0175 C3 0.0232 0.0189 0.0172 C4 0.0270 0.0198 0.0164 C5 0.0254 0.0190 0.0174 C6 0.0288 0.0197 0.0163 C7 0.0268 0.0178 0.0164 C8 0.0284 0.0191 0.0151 C9 0.0243 0.0155 0.0133 C10 0.0218 0.0165 0.0117 C11 0.0177 0.0169 0.0112 C12 0.0144 0.0133 0.0122 C13 0.0211 0.0186 0.0115 C14 0.0227 0.0218 0.0116 C15 0.0215 0.0194 0.0126 C16 0.0201 0.0161 0.0132 C17 0.0166 0.0133 0.0114 C18 0.0255 0.0196 0.0065 C19 0.0245 0.0182 0.0094 C20 0.0252 0.0181 0.0168 C21 0.0251 0.0209 0.0174 C22 0.0263 0.0216 0.0190 C23 0.0293 0.0216 0.0172 C24 0.0272 0.0219 0.0189 C25 0.0291 0.0221 0.0189 C26 0.0288 0.0224 0.0166 C27 0.0407 0.0219 0.0216 C28 0.0556 0.0271 0.0197 C29 0.0396 0.0205 0.0165 Br1 0.0174 0.0138 0.0129 N1 0.0181 0.0156 0.0086 N2 0.0475 0.0379 0.0359 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.027 0.050 0.072 0.094 0.117 0.142 0.172 0.214 0.282 1.000 Number in group 669. 646. 667. 644. 659. 667. 636. 652. 654. 661. GooF 1.034 1.123 1.087 1.027 1.039 0.991 1.029 0.999 0.981 1.155 K 1.816 1.156 1.079 1.050 1.009 1.007 0.996 0.993 0.999 1.006 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.06 1.16 1.33 1.66 inf Number in group 680. 636. 653. 652. 657. 667. 647. 653. 649. 661. GooF 1.041 1.006 0.972 0.907 0.879 0.892 0.839 0.847 1.150 1.670 K 0.992 1.009 1.008 1.009 1.006 1.011 1.011 1.016 1.007 1.000 R1 0.122 0.096 0.087 0.071 0.052 0.049 0.038 0.033 0.038 0.044 Recommended weighting scheme: WGHT 0.0322 2.4967 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/su Fc/Fc(max) Resolution(A) -2 3 3 4125.25 3224.75 5.28 0.473 2.07 2 5 4 910.70 629.58 5.18 0.209 1.74 1 0 5 184.90 341.33 5.04 0.154 3.67 -4 0 1 551.81 354.35 5.02 0.157 2.07 -2 2 2 119.30 234.89 4.86 0.128 2.63 1 0 7 829.91 1177.67 4.78 0.286 2.69 1 0 6 996.65 1342.46 4.67 0.305 3.11 -1 -1 7 369.43 190.49 4.59 0.115 2.35 2 -4 5 254.79 141.50 4.35 0.099 1.66 0 -3 6 158.08 78.62 4.33 0.074 2.09 2 3 2 3699.57 2958.47 4.20 0.453 2.71 0 0 11 567.18 381.09 4.16 0.162 1.70 2 -2 5 155.98 70.03 4.15 0.070 2.33 -1 -3 5 1170.50 846.99 4.02 0.242 2.21 4 2 1 62.42 134.28 4.01 0.096 2.12 -4 0 3 1040.66 1378.35 3.96 0.309 1.91 2 -1 7 422.11 598.04 3.94 0.204 2.28 1 5 4 534.16 374.84 3.91 0.161 1.75 3 0 7 150.40 80.38 3.87 0.075 2.14 2 2 9 107.03 51.52 3.85 0.060 1.95 0 4 3 300.68 198.49 3.80 0.117 2.14 0 1 8 201.19 310.64 3.79 0.147 2.30 2 3 9 798.52 604.51 3.78 0.205 1.80 3 1 8 88.00 37.95 3.77 0.051 2.02 -1 -1 6 188.07 107.97 3.68 0.086 2.66 -4 3 3 31.02 82.45 3.68 0.076 1.50 4 0 3 21.82 64.63 3.67 0.067 2.12 2 7 6 1599.15 1289.51 3.66 0.299 1.24 3 -2 5 191.65 290.97 3.60 0.142 1.99 2 -2 4 408.92 283.54 3.55 0.140 2.49 -2 1 2 50.91 107.01 3.53 0.086 3.21 -4 0 4 1075.85 1345.09 3.48 0.305 1.82 -3 2 0 97.29 49.49 3.47 0.059 2.20 0 1 4 117.30 64.16 3.46 0.067 4.25 10 6 9 157.96 263.25 3.46 0.135 0.81 10 6 8 234.42 378.55 3.44 0.162 0.82 0 4 4 4927.77 4191.36 3.42 0.539 2.06 -2 5 5 153.17 90.61 3.41 0.079 1.42 10 0 14 -6.37 46.59 3.36 0.057 0.78 3 2 10 217.12 139.22 3.36 0.098 1.69 -4 2 2 3244.87 2687.43 3.36 0.432 1.71 -1 5 2 58.67 20.94 3.36 0.038 1.66 0 -5 4 866.73 678.67 3.33 0.217 1.63 1 3 10 998.66 802.57 3.27 0.236 1.68 0 0 10 497.55 368.67 3.22 0.160 1.88 1 1 8 584.69 442.87 3.20 0.175 2.36 3 -2 4 583.23 738.82 3.16 0.226 2.08 -3 -1 3 3540.95 4183.37 3.13 0.538 2.43 4 0 4 76.33 132.50 3.12 0.096 2.07 9 6 14 82.62 144.87 3.11 0.100 0.81 Bond lengths and angles C1 - Distance Angles C2 1.5230 (0.0037) H1A 0.9800 109.47 H1B 0.9800 109.47 109.47 H1C 0.9800 109.47 109.47 109.47 C1 - C2 H1A H1B C2 - Distance Angles C3 1.5205 (0.0035) C1 1.5230 (0.0037) 112.83 (0.22) H2A 0.9900 109.02 109.02 H2B 0.9900 109.02 109.02 107.80 C2 - C3 C1 H2A C3 - Distance Angles C2 1.5205 (0.0035) C4 1.5251 (0.0034) 113.98 (0.21) H3A 0.9900 108.76 108.76 H3B 0.9900 108.76 108.76 107.65 C3 - C2 C4 H3A C4 - Distance Angles C3 1.5251 (0.0034) C5 1.5285 (0.0034) 113.27 (0.20) H4A 0.9900 108.92 108.92 H4B 0.9900 108.92 108.92 107.74 C4 - C3 C5 H4A C5 - Distance Angles C4 1.5285 (0.0034) C6 1.5287 (0.0034) 113.77 (0.20) H5A 0.9900 108.81 108.81 H5B 0.9900 108.81 108.81 107.68 C5 - C4 C6 H5A C6 - Distance Angles C7 1.5275 (0.0034) C5 1.5287 (0.0034) 112.85 (0.20) H6A 0.9900 109.02 109.02 H6B 0.9900 109.02 109.02 107.80 C6 - C7 C5 H6A C7 - Distance Angles C8 1.5242 (0.0034) C6 1.5275 (0.0034) 113.72 (0.21) H7A 0.9900 108.82 108.82 H7B 0.9900 108.82 108.82 107.68 C7 - C8 C6 H7A C8 - Distance Angles C7 1.5242 (0.0034) C9 1.5323 (0.0035) 112.79 (0.21) H8A 0.9900 109.03 109.03 H8B 0.9900 109.03 109.03 107.80 C8 - C7 C9 H8A C9 - Distance Angles C10 1.5282 (0.0033) C8 1.5323 (0.0035) 113.22 (0.20) H9A 0.9900 108.93 108.93 H9B 0.9900 108.93 108.93 107.75 C9 - C10 C8 H9A C10 - Distance Angles C9 1.5282 (0.0033) C11 1.5304 (0.0033) 113.42 (0.20) H10A 0.9900 108.89 108.89 H10B 0.9900 108.89 108.89 107.72 C10 - C9 C11 H10A C11 - Distance Angles N1 1.4712 (0.0029) C10 1.5304 (0.0033) 111.48 (0.19) H11A 0.9900 109.33 109.33 H11B 0.9900 109.33 109.33 107.97 C11 - N1 C10 H11A C12 - Distance Angles N2 1.3304 (0.0030) N1 1.3358 (0.0030) 110.40 (0.20) H12 0.9500 124.80 124.80 C12 - N2 N1 C13 - Distance Angles N1 1.3927 (0.0029) C18 1.3968 (0.0032) 106.66 (0.19) C14 1.3970 (0.0032) 131.49 (0.21) 121.83 (0.21) C13 - N1 C18 C14 - Distance Angles C15 1.3801 (0.0034) C13 1.3970 (0.0032) 116.08 (0.22) H14 0.9500 121.96 121.96 C14 - C15 C13 C15 - Distance Angles C14 1.3801 (0.0034) C16 1.4115 (0.0034) 122.09 (0.22) H15 0.9500 118.95 118.95 C15 - C14 C16 C16 - Distance Angles C17 1.3865 (0.0033) C15 1.4115 (0.0034) 121.84 (0.22) H16 0.9500 119.08 119.08 C16 - C17 C15 C17 - Distance Angles C16 1.3865 (0.0033) C18 1.3926 (0.0032) 115.95 (0.22) H17 0.9500 122.03 122.03 C17 - C16 C18 C18 - Distance Angles C17 1.3926 (0.0032) C13 1.3968 (0.0032) 122.21 (0.21) N2 1.3990 (0.0028) 131.45 (0.21) 106.32 (0.20) C18 - C17 C13 C19 - Distance Angles N2 1.4788 (0.0029) C20 1.5198 (0.0035) 111.15 (0.19) H19A 0.9900 109.40 109.40 H19B 0.9900 109.40 109.40 108.02 C19 - N2 C20 H19A C20 - Distance Angles C19 1.5198 (0.0035) C21 1.5251 (0.0034) 114.35 (0.20) H20A 0.9900 108.67 108.67 H20B 0.9900 108.67 108.67 107.60 C20 - C19 C21 H20A C21 - Distance Angles C22 1.5244 (0.0035) C20 1.5251 (0.0034) 112.24 (0.21) H21A 0.9900 109.16 109.16 H21B 0.9900 109.16 109.16 107.87 C21 - C22 C20 H21A C22 - Distance Angles C21 1.5244 (0.0035) C23 1.5251 (0.0035) 114.40 (0.21) H22A 0.9900 108.66 108.66 H22B 0.9900 108.66 108.66 107.60 C22 - C21 C23 H22A C23 - Distance Angles C24 1.5204 (0.0036) C22 1.5251 (0.0035) 112.65 (0.22) H23A 0.9900 109.06 109.06 H23B 0.9900 109.06 109.06 107.82 C23 - C24 C22 H23A C24 - Distance Angles C23 1.5204 (0.0036) C25 1.5276 (0.0036) 114.36 (0.22) H24A 0.9900 108.67 108.67 H24B 0.9900 108.67 108.67 107.60 C24 - C23 C25 H24A C25 - Distance Angles C26 1.5234 (0.0036) C24 1.5276 (0.0036) 112.81 (0.22) H25A 0.9900 109.03 109.03 H25B 0.9900 109.03 109.03 107.80 C25 - C26 C24 H25A C26 - Distance Angles C25 1.5234 (0.0036) C27 1.5250 (0.0037) 114.06 (0.22) H26A 0.9900 108.74 108.74 H26B 0.9900 108.74 108.74 107.64 C26 - C25 C27 H26A C27 - Distance Angles C26 1.5250 (0.0037) C28 1.5251 (0.0037) 113.20 (0.23) H27A 0.9900 108.94 108.94 H27B 0.9900 108.94 108.94 107.75 C27 - C26 C28 H27A C28 - Distance Angles C29 1.5243 (0.0040) C27 1.5251 (0.0037) 113.17 (0.25) H28A 0.9900 108.95 108.95 H28B 0.9900 108.95 108.95 107.76 C28 - C29 C27 H28A C29 - Distance Angles C28 1.5243 (0.0040) H29A 0.9800 109.47 H29B 0.9800 109.47 109.47 H29C 0.9800 109.47 109.47 109.47 C29 - C28 H29A H29B N1 - Distance Angles C12 1.3358 (0.0030) C13 1.3927 (0.0029) 108.28 (0.19) C11 1.4712 (0.0029) 126.35 (0.20) 125.23 (0.19) N1 - C12 C13 N2 - Distance Angles C12 1.3304 (0.0030) C18 1.3990 (0.0028) 108.34 (0.19) C19 1.4788 (0.0029) 126.32 (0.19) 125.30 (0.19) N2 - C12 C18 O1 - Distance Angles H20 0.8868 (0.0182) H10 0.8785 (0.0182) 105.56 (3.11) O1 - H20 FMAP and GRID set by program FMAP 2 1 41 GRID -2.632 -2 -1 2.632 2 1 R1 = 0.0533 for 6555 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.26 at 0.1449 0.1794 0.0063 [ 0.85 A from BR1 ] Deepest hole -1.10 at 0.1942 0.1382 0.0800 [ 0.70 A from BR1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 4570 / 46241 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1449 0.1794 0.0063 1.00000 0.05 1.26 0.85 BR1 1.63 H10 2.36 H11A 2.47 O1 Q2 1 0.1121 0.0890 0.0896 1.00000 0.05 0.51 1.10 BR1 1.61 H20 2.28 H1B 2.38 H12 Q3 1 0.0735 0.0821 0.0300 1.00000 0.05 0.46 1.31 BR1 1.59 H20 1.60 H10 2.33 H12 Q4 1 0.2402 0.2292 0.0039 1.00000 0.05 0.42 1.16 BR1 2.31 H11A 2.33 H14 2.39 H17 Q5 1 0.5601 0.0604 0.1796 1.00000 0.05 0.36 0.76 C20 0.77 C21 1.41 H21A 1.42 H20A Q6 1 0.4501 0.4272 0.0783 1.00000 0.05 0.36 0.67 C18 0.82 C17 1.44 H17 1.77 N2 Q7 1 0.8714 0.3463 0.4116 1.00000 0.05 0.35 0.70 C6 0.83 C7 1.37 H6A 1.41 H6B Q8 1 0.6114 -0.3470 0.6193 1.00000 0.05 0.35 0.76 C28 0.77 C27 1.39 H28B 1.43 H27B Q9 1 0.1094 0.2208 0.0968 1.00000 0.05 0.34 1.15 BR1 2.17 H11B 2.24 H12 2.48 H17 Q10 1 0.8758 0.5463 0.1491 1.00000 0.05 0.34 0.77 C10 0.77 C11 1.42 H10B 1.43 H11A Shortest distances between peaks (including symmetry equivalents) 1 4 1.03 1 3 1.20 2 9 1.22 2 3 1.26 1 2 1.73 1 9 1.76 4 9 1.93 3 9 1.99 3 4 2.16 2 4 2.26 3 3 2.64 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.73: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 4.38: Structure factors and derivatives 11.77: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.91: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 14:43:29 Total CPU time: 18.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++