++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XL - CRYSTAL STRUCTURE REFINEMENT - SHELXTL Version 2008/4 + + Copyright(c) 2008 Bruker Analytical X-ray Solutions All Rights Reserved + + UDel1Mo started at 14:13:21 on 04-Feb-2011 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL UDel1Mo in P2(1) CELL 0.71073 15.2856 9.2961 15.5105 90.000 116.574 90.000 ZERR 2.00 0.0028 0.0017 0.0029 0.000 0.003 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N F CL UNIT 82 36 8 30 6 V = 1971.15 F(000) = 956.0 Mu = 0.34 mm-1 Cell Wt = 1915.89 Rho = 1.614 TEMP -173.000 SIZE 0.036 0.039 0.44 L.S. 8 BOND $H ACTA CONF FMAP 2 PLAN 20 SIMU $CL SIMU $F ISOR DELU OMIT -3 50 EADP C41 C42 SADI C41 CL1 C41 CL2 C41 CL3 C42 CL4 C42 CL5 C42 CL6 SADI CL1 CL2 CL2 CL3 CL3 CL1 CL4 CL5 CL5 CL6 CL6 CL4 WGHT 0.1023 0.1423 EXTI 0.016678 FVAR 0.18751 0.61582 N1 3 1.049162 0.851477 0.424713 11.00000 0.03528 0.02736 = 0.04451 -0.00377 0.02425 0.00212 AFIX 3 H1N 2 1.011302 0.942557 0.411732 11.00000 0.03752 AFIX 0 C1 1 1.123522 0.815457 0.514018 11.00000 0.03156 0.02653 = 0.04623 0.00354 0.02086 -0.00460 C2 1 1.174685 0.702819 0.499924 11.00000 0.03978 0.03543 = 0.05217 0.00638 0.02189 0.00927 AFIX 43 H2 2 1.227698 0.652560 0.549002 11.00000 -1.20000 AFIX 0 C3 1 1.135457 0.675887 0.402158 11.00000 0.04839 0.03042 = 0.07417 0.00418 0.03911 0.00859 AFIX 43 H3 2 1.158271 0.605547 0.372596 11.00000 -1.20000 AFIX 0 C4 1 1.056653 0.769121 0.353811 11.00000 0.03923 0.03156 = 0.04723 -0.00376 0.02730 0.00139 C5 1 0.991900 0.784841 0.254160 11.00000 0.03798 0.03597 = 0.05550 -0.01236 0.03317 -0.00850 C6 1 1.031549 0.739721 0.185181 11.00000 0.04469 0.05435 = 0.05167 -0.01007 0.02896 0.00006 C7 1 1.103695 0.816324 0.176586 11.00000 0.04810 0.06259 = 0.06853 -0.02521 0.03975 -0.00855 F1 4 1.136942 0.932748 0.229155 11.00000 0.11592 0.09066 = 0.14796 -0.07138 0.11123 -0.06214 C8 1 1.142496 0.780481 0.115972 11.00000 0.06130 0.10458 = 0.09544 -0.03528 0.06029 -0.02242 F2 4 1.213714 0.854059 0.111493 11.00000 0.13948 0.13714 = 0.17300 -0.05373 0.13462 -0.04775 C9 1 1.112803 0.648047 0.065899 11.00000 0.07497 0.12289 = 0.07330 -0.04120 0.04874 -0.00371 F3 4 1.152407 0.612072 0.008068 11.00000 0.12803 0.21142 = 0.13648 -0.09800 0.09719 -0.01952 C10 1 1.046937 0.568650 0.077011 11.00000 0.09569 0.10403 = 0.09698 -0.06152 0.05328 -0.01894 F4 4 1.022173 0.439003 0.032267 11.00000 0.17717 0.13456 = 0.20040 -0.10519 0.12526 -0.03667 C11 1 1.007502 0.607643 0.137245 11.00000 0.07707 0.08906 = 0.10315 -0.05243 0.05668 -0.02828 F5 4 0.937865 0.524956 0.144147 11.00000 0.18274 0.08942 = 0.24933 -0.09839 0.16215 -0.06399 C12 1 0.898207 0.838177 0.217208 11.00000 0.04397 0.03348 = 0.04483 -0.01045 0.02518 -0.00513 N2 3 0.845000 0.864440 0.268674 11.00000 0.03738 0.03652 = 0.03904 0.00113 0.02456 0.00213 AFIX 3 H2N 2 0.862030 0.820810 0.332364 11.00000 0.05821 AFIX 0 C13 1 0.833661 0.873275 0.119418 11.00000 0.03753 0.05878 = 0.04367 -0.00918 0.02492 -0.01265 AFIX 43 H13 2 0.849502 0.867613 0.066862 11.00000 -1.20000 AFIX 0 C14 1 0.746190 0.915962 0.113362 11.00000 0.04214 0.05453 = 0.03594 -0.00704 0.02101 -0.00456 AFIX 43 H14 2 0.691487 0.947599 0.056577 11.00000 -1.20000 AFIX 0 C15 1 0.750550 0.905073 0.207646 11.00000 0.03910 0.03060 = 0.04436 -0.00405 0.02012 -0.00226 C16 1 0.675619 0.919129 0.233114 11.00000 0.03614 0.03480 = 0.03935 -0.00276 0.02094 -0.00132 C17 1 0.575291 0.943699 0.154673 11.00000 0.03391 0.04891 = 0.03707 0.00421 0.02194 0.00528 C18 1 0.532993 1.078351 0.128461 11.00000 0.04231 0.06222 = 0.04156 -0.00039 0.01941 0.00267 F6 4 0.582935 1.193872 0.173723 11.00000 0.05360 0.04592 = 0.07170 0.00030 0.01476 0.01525 C19 1 0.437865 1.096398 0.058633 11.00000 0.04237 0.08293 = 0.05082 0.00692 0.01558 0.01752 F7 4 0.399598 1.228421 0.037673 11.00000 0.06310 0.10738 = 0.06943 0.02156 0.01538 0.04627 C20 1 0.384271 0.978642 0.012036 11.00000 0.03284 0.11578 = 0.03155 0.00627 0.00832 0.00879 F8 4 0.290972 0.996288 -0.056493 11.00000 0.03588 0.17932 = 0.04271 -0.00076 0.00179 0.00272 C21 1 0.421090 0.843559 0.033812 11.00000 0.05236 0.07916 = 0.04455 -0.01958 0.02311 -0.01685 F9 4 0.367354 0.728155 -0.009120 11.00000 0.05811 0.13142 = 0.07255 -0.02709 0.01518 -0.03249 C22 1 0.516833 0.824755 0.106394 11.00000 0.03985 0.05914 = 0.04118 -0.00349 0.01686 -0.00447 F10 4 0.552938 0.692734 0.127855 11.00000 0.06756 0.05111 = 0.06842 -0.00218 0.02414 -0.01184 C23 1 0.683999 0.891584 0.327099 11.00000 0.03527 0.02639 = 0.04528 0.00567 0.02271 0.00540 N3 3 0.766983 0.856426 0.405388 11.00000 0.03633 0.02410 = 0.03927 0.00265 0.02503 0.00156 C24 1 0.599684 0.886886 0.347519 11.00000 0.03270 0.04735 = 0.04149 0.00640 0.02191 0.00960 AFIX 43 H24 2 0.534165 0.911524 0.304543 11.00000 -1.20000 AFIX 0 C25 1 0.632527 0.841130 0.438549 11.00000 0.02839 0.04343 = 0.05453 0.00737 0.02677 0.00601 AFIX 43 H25 2 0.594542 0.825061 0.472179 11.00000 -1.20000 AFIX 0 C26 1 0.737988 0.820662 0.476220 11.00000 0.03360 0.02232 = 0.04391 0.00288 0.02292 -0.00056 C27 1 0.799012 0.769094 0.567328 11.00000 0.03507 0.02453 = 0.04398 -0.00081 0.02518 0.00026 C28 1 0.753003 0.710371 0.627605 11.00000 0.03835 0.03431 = 0.04318 0.00608 0.02466 0.00251 C29 1 0.694741 0.588494 0.599484 11.00000 0.03704 0.04925 = 0.04761 0.00722 0.02356 -0.00881 F11 4 0.679416 0.520015 0.519106 11.00000 0.05467 0.05482 = 0.06073 -0.00634 0.03018 -0.02277 C30 1 0.653955 0.534217 0.655575 11.00000 0.03835 0.05910 = 0.06570 0.01501 0.02175 -0.01270 F12 4 0.598695 0.414376 0.627884 11.00000 0.07157 0.08153 = 0.09106 0.01021 0.04084 -0.03412 C31 1 0.671121 0.599071 0.740625 11.00000 0.04226 0.08254 = 0.04978 0.01364 0.02934 -0.01076 F13 4 0.631396 0.546222 0.795253 11.00000 0.06480 0.12602 = 0.06959 0.01717 0.04360 -0.02184 C32 1 0.730860 0.720857 0.771644 11.00000 0.04897 0.06702 = 0.04678 0.01028 0.02875 0.00908 F14 4 0.748657 0.779182 0.854950 11.00000 0.08299 0.10392 = 0.05112 -0.00478 0.04483 -0.00669 C33 1 0.769483 0.772776 0.713229 11.00000 0.04528 0.04530 = 0.04932 0.00034 0.02861 -0.00368 F15 4 0.825846 0.892166 0.744351 11.00000 0.07268 0.05465 = 0.05660 -0.01012 0.04090 -0.01025 C34 1 0.902151 0.761462 0.608197 11.00000 0.03128 0.03058 = 0.03227 0.00035 0.01883 -0.00025 N4 3 0.956341 0.832553 0.571673 11.00000 0.03394 0.02818 = 0.04119 0.00766 0.01954 0.00187 AFIX 3 H4N 2 0.929131 0.878643 0.517723 11.00000 0.04315 AFIX 0 C35 1 0.969277 0.687576 0.688827 11.00000 0.03833 0.03628 = 0.04314 0.00648 0.02330 0.00404 AFIX 43 H35 2 0.954069 0.627074 0.729629 11.00000 -1.20000 AFIX 0 C36 1 1.062256 0.717982 0.698994 11.00000 0.03891 0.03264 = 0.04266 0.01226 0.01750 -0.00247 AFIX 43 H36 2 1.121730 0.680852 0.747761 11.00000 -1.20000 AFIX 0 C37 1 1.053983 0.810959 0.626617 11.00000 0.03241 0.02441 = 0.03573 -0.00303 0.01762 -0.00087 C38 1 1.130162 0.883464 0.604076 11.00000 0.03475 0.03291 = 0.05351 0.00138 0.02882 -0.00067 C39 1 1.231654 0.857010 0.686835 11.00000 0.03793 0.05778 = 0.05423 -0.00095 0.02189 -0.00748 AFIX 137 H39A 2 1.243642 0.753264 0.695882 11.00000 -1.50000 H39B 2 1.235229 0.899442 0.746164 11.00000 -1.50000 H39C 2 1.281205 0.901352 0.671554 11.00000 -1.50000 AFIX 0 C40 1 1.110282 1.044683 0.591278 11.00000 0.05290 0.02819 = 0.05454 -0.00692 0.02963 -0.01549 AFIX 137 H40A 2 1.047183 1.061635 0.535248 11.00000 -1.50000 H40B 2 1.162283 1.091998 0.581231 11.00000 -1.50000 H40C 2 1.108599 1.084059 0.649127 11.00000 -1.50000 AFIX 0 PART 1 C41 1 0.534410 0.052838 0.688460 21.00000 0.07276 0.07557 = 0.08333 0.02478 0.04254 0.02569 AFIX 13 H41 2 0.476692 0.118725 0.666075 21.00000 -1.20000 AFIX 0 CL1 5 0.575009 0.052172 0.600753 21.00000 0.06584 0.07401 = 0.06635 -0.01220 0.03495 0.00506 CL2 5 0.621660 0.118583 0.796155 21.00000 0.09110 0.12596 = 0.07564 -0.01021 0.04015 0.02646 CL3 5 0.495340 -0.117058 0.703159 21.00000 0.06041 0.08272 = 0.22869 0.07162 0.07031 0.01776 PART 2 SAME C41 > Cl3 C42 1 0.518177 0.002756 0.667117 -21.00000 0.07276 0.07557 = 0.08333 0.02478 0.04254 0.02569 AFIX 13 H42 2 0.458538 0.064446 0.645985 -21.00000 -1.20000 AFIX 0 CL4 5 0.583684 0.055156 0.605618 -21.00000 0.20930 0.11671 = 0.20802 0.04517 0.16172 0.04266 CL5 5 0.588872 0.024253 0.789475 -21.00000 0.17253 0.17898 = 0.09990 -0.00411 0.04579 0.08517 CL6 5 0.482327 -0.176101 0.642645 -21.00000 0.10867 0.09051 = 0.14812 0.04416 0.05773 0.04774 PART 0 HKLF 4 Covalent radii and connectivity table for UDel1Mo in P2(1) C 0.770 H 0.320 N 0.700 F 0.640 CL 0.990 N1 - C1 C4 C1 - C2 N1 C38 C2 - C3 C1 C3 - C2 C4 C4 - N1 C3 C5 C5 - C12 C4 C6 C6 - C7 C11 C5 C7 - F1 C8 C6 F1 - C7 C8 - F2 C7 C9 F2 - C8 C9 - C10 F3 C8 F3 - C9 C10 - C9 F4 C11 F4 - C10 C11 - F5 C10 C6 F5 - C11 C12 - C5 N2 C13 N2 - C15 C12 C13 - C14 C12 C14 - C13 C15 C15 - C16 N2 C14 C16 - C15 C23 C17 C17 - C18 C22 C16 C18 - F6 C19 C17 F6 - C18 C19 - F7 C20 C18 F7 - C19 C20 - F8 C21 C19 F8 - C20 C21 - F9 C20 C22 F9 - C21 C22 - F10 C21 C17 F10 - C22 C23 - N3 C16 C24 N3 - C23 C26 C24 - C25 C23 C25 - C24 C26 C26 - C27 N3 C25 C27 - C26 C34 C28 C28 - C33 C29 C27 C29 - F11 C30 C28 F11 - C29 C30 - F12 C31 C29 F12 - C30 C31 - F13 C30 C32 F13 - C31 C32 - F14 C33 C31 F14 - C32 C33 - F15 C28 C32 F15 - C33 C34 - N4 C35 C27 N4 - C37 C34 C35 - C36 C34 C36 - C37 C35 C37 - N4 C36 C38 C38 - C1 C37 C40 C39 C39 - C38 C40 - C38 C41_a - Cl2_a Cl1_a Cl3_a Cl1_a - C41_a Cl2_a - C41_a Cl3_a - C41_a C42_b - Cl5_b Cl4_b Cl6_b Cl4_b - C42_b Cl5_b - C42_b Cl6_b - C42_b Floating origin restraints generated 22165 Reflections read, of which 3994 rejected -18 =< h =< 17, -10 =< k =< 11, -18 =< l =< 18, Max. 2-theta = 49.99 0 Systematic absence violations 0 Inconsistent equivalents 6904 Unique reflections, of which 0 suppressed R(int) = 0.0602 R(sigma) = 0.0836 Friedel opposites not merged Maximum memory for data reduction = 6195 / 69525 Default effective X-H distances for T = -173.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 7718 / 826852 wR2 = 0.1861 before cycle 1 for 6904 data and 605 / 605 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.0304 0.0100 DELU C42_b Cl6_b Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 33. 0. 0. 0. 183. 18. 402. 0. rms sigma 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.010 0.080 0.100 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.007 0.070 0.024 0.000 GooF = S = 1.023; Restrained GooF = 0.986 for 637 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1023 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.18751 0.00061 0.004 OSF 2 0.61527 0.01574 -0.035 FVAR 2 3 0.01670 0.00216 0.010 EXTI Mean shift/esd = 0.024 Maximum = 0.108 for U23 C10 Max. shift = 0.001 A for Cl5_b Max. dU = 0.000 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 7718 / 826852 wR2 = 0.1861 before cycle 2 for 6904 data and 605 / 605 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.0304 0.0100 DELU C42_b Cl6_b Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 33. 0. 0. 0. 183. 18. 402. 0. rms sigma 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.010 0.080 0.100 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.007 0.070 0.024 0.000 GooF = S = 1.023; Restrained GooF = 0.986 for 637 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1023 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.18750 0.00061 -0.022 OSF 2 0.61516 0.01576 -0.007 FVAR 2 3 0.01670 0.00216 -0.001 EXTI Mean shift/esd = 0.011 Maximum = 0.082 for U23 C10 Max. shift = 0.001 A for H40B Max. dU = 0.000 for H2N Least-squares cycle 3 Maximum vector length = 511 Memory required = 7718 / 826852 wR2 = 0.1861 before cycle 3 for 6904 data and 605 / 605 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 0.0304 0.0100 DELU C42_b Cl6_b Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 33. 0. 0. 0. 183. 18. 402. 0. rms sigma 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.010 0.080 0.100 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.007 0.070 0.024 0.000 GooF = S = 1.023; Restrained GooF = 0.986 for 637 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1023 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.18749 0.00061 -0.022 OSF 2 0.61516 0.01577 0.000 FVAR 2 3 0.01669 0.00216 -0.003 EXTI Mean shift/esd = 0.004 Maximum = 0.043 for U23 C10 Max. shift = 0.000 A for H39C Max. dU = 0.000 for C10 Least-squares cycle 4 Maximum vector length = 511 Memory required = 7718 / 826852 wR2 = 0.1861 before cycle 4 for 6904 data and 605 / 605 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.0304 0.0100 DELU C42_b Cl6_b Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 33. 0. 0. 0. 183. 18. 402. 0. rms sigma 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.010 0.080 0.100 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.007 0.070 0.024 0.000 GooF = S = 1.023; Restrained GooF = 0.986 for 637 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1023 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.18748 0.00061 -0.008 OSF 2 0.61516 0.01577 0.000 FVAR 2 3 0.01669 0.00216 -0.003 EXTI Mean shift/esd = 0.003 Maximum = 0.025 for U23 C10 Max. shift = 0.000 A for C10 Max. dU = 0.000 for C10 Least-squares cycle 5 Maximum vector length = 511 Memory required = 7718 / 826852 wR2 = 0.1861 before cycle 5 for 6904 data and 605 / 605 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 0.0304 0.0100 DELU C42_b Cl6_b Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 33. 0. 0. 0. 183. 18. 402. 0. rms sigma 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.010 0.080 0.100 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.007 0.070 0.024 0.000 GooF = S = 1.023; Restrained GooF = 0.986 for 637 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1023 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.18748 0.00061 -0.001 OSF 2 0.61516 0.01577 0.000 FVAR 2 3 0.01669 0.00216 0.001 EXTI Mean shift/esd = 0.002 Maximum = 0.015 for U23 C10 Max. shift = 0.000 A for H39C Max. dU = 0.000 for C10 Least-squares cycle 6 Maximum vector length = 511 Memory required = 7718 / 826852 wR2 = 0.1861 before cycle 6 for 6904 data and 605 / 605 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint 0.0304 0.0100 DELU C42_b Cl6_b Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 33. 0. 0. 0. 183. 18. 402. 0. rms sigma 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.010 0.080 0.100 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.007 0.070 0.024 0.000 GooF = S = 1.023; Restrained GooF = 0.986 for 637 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1023 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.18748 0.00061 0.001 OSF 2 0.61516 0.01577 0.001 FVAR 2 3 0.01669 0.00216 0.002 EXTI Mean shift/esd = 0.001 Maximum = 0.009 for U23 C10 Max. shift = 0.000 A for H39C Max. dU = 0.000 for C10 Least-squares cycle 7 Maximum vector length = 511 Memory required = 7718 / 826852 wR2 = 0.1861 before cycle 7 for 6904 data and 605 / 605 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint 0.0304 0.0100 DELU C42_b Cl6_b Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 33. 0. 0. 0. 183. 18. 402. 0. rms sigma 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.010 0.080 0.100 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.007 0.070 0.024 0.000 GooF = S = 1.023; Restrained GooF = 0.986 for 637 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1023 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.18748 0.00061 0.001 OSF 2 0.61518 0.01577 0.001 FVAR 2 3 0.01670 0.00216 0.001 EXTI Mean shift/esd = 0.001 Maximum = 0.006 for U23 C10 Max. shift = 0.000 A for H39C Max. dU = 0.000 for C10 Least-squares cycle 8 Maximum vector length = 511 Memory required = 7718 / 826852 wR2 = 0.1861 before cycle 8 for 6904 data and 605 / 605 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint 0.0304 0.0100 DELU C42_b Cl6_b Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 33. 0. 0. 0. 183. 18. 402. 0. rms sigma 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.010 0.080 0.100 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.007 0.070 0.024 0.000 GooF = S = 1.023; Restrained GooF = 0.986 for 637 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1023 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.18748 0.00061 0.000 OSF 2 0.61517 0.01577 0.000 FVAR 2 3 0.01670 0.00216 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.004 for U23 C10 Max. shift = 0.000 A for C10 Max. dU = 0.000 for C10 Largest correlation matrix elements -0.835 y Cl5_b / FVAR 2 -0.792 y Cl2_a / FVAR 2 0.765 z Cl3_a / y Cl3_a -0.834 y Cl4_b / y Cl1_a -0.791 z Cl6_b / FVAR 2 0.763 U13 F1 / U33 F1 -0.831 z Cl3_a / FVAR 2 0.791 y Cl6_b / z Cl3_a 0.753 U13 F5 / U33 F5 0.830 U13 F2 / U33 F2 0.789 z Cl6_b / y Cl3_a 0.742 U12 F1 / U23 F1 0.817 U13 F2 / U11 F2 -0.777 y Cl3_a / FVAR 2 0.742 y Cl5_b / z Cl3_a -0.816 U22 Cl4_b / U22 Cl1_a 0.772 U13 F1 / U11 F1 -0.740 z Cl4_b / z Cl1_a 0.806 U13 Cl4_b / U11 Cl4_b 0.770 U13 F5 / U11 F5 0.739 z F2 / x F2 0.800 U13 Cl4_b / U33 Cl4_b 0.765 y Cl5_b / y Cl2_a -0.739 y Cl6_b / FVAR 2 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 1.2277 0.6525 0.5490 43 0.950 0.000 C2 C3 C1 H3 1.1583 0.6055 0.3726 43 0.950 0.000 C3 C2 C4 H13 0.8495 0.8676 0.0669 43 0.950 0.000 C13 C14 C12 H14 0.6915 0.9475 0.0566 43 0.950 0.000 C14 C13 C15 H24 0.5342 0.9116 0.3045 43 0.950 0.000 C24 C25 C23 H25 0.5945 0.8250 0.4722 43 0.950 0.000 C25 C24 C26 H35 0.9541 0.6271 0.7296 43 0.950 0.000 C35 C36 C34 H36 1.1217 0.6808 0.7478 43 0.950 0.000 C36 C37 C35 H39A 1.2436 0.7533 0.6959 137 0.980 0.000 C39 C38 H39A H39B 1.2352 0.8995 0.7461 137 0.980 0.000 C39 C38 H39A H39C 1.2812 0.9013 0.6715 137 0.980 0.000 C39 C38 H39A H40A 1.0473 1.0617 0.5352 137 0.980 0.000 C40 C38 H40A H40B 1.1624 1.0920 0.5813 137 0.980 0.000 C40 C38 H40A H40C 1.1086 1.0840 0.6491 137 0.980 0.000 C40 C38 H40A H41 0.4767 0.1187 0.6660 13 1.000 0.000 C41_a Cl2_a Cl1_a Cl3_a H42 0.4586 0.0645 0.6460 13 1.000 0.000 C42_b Cl5_b Cl4_b Cl6_b UDel1Mo in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq N1 1.04917 0.85146 0.42473 1.00000 0.03529 0.02738 0.04459 -0.00372 0.02432 0.00205 0.03334 0.00849 0.00028 0.00043 0.00028 0.00000 0.00220 0.00214 0.00221 0.00182 0.00184 0.00176 0.00092 H1N 1.01131 0.94254 0.41175 1.00000 0.03666 0.00000 0.01332 C1 1.12353 0.81547 0.51402 1.00000 0.03168 0.02648 0.04636 0.00360 0.02098 -0.00455 0.03353 0.01018 0.00034 0.00052 0.00035 0.00000 0.00255 0.00246 0.00258 0.00214 0.00210 0.00204 0.00106 C2 1.17469 0.70281 0.49995 1.00000 0.03990 0.03548 0.05227 0.00639 0.02190 0.00932 0.04207 0.01169 0.00038 0.00057 0.00039 0.00000 0.00300 0.00286 0.00305 0.00249 0.00245 0.00231 0.00125 H2 1.22769 0.65253 0.54904 1.00000 0.05048 0.00000 0.00000 C3 1.13549 0.67588 0.40215 1.00000 0.04831 0.03058 0.07386 0.00426 0.03891 0.00860 0.04660 0.01281 0.00040 0.00059 0.00044 0.00000 0.00321 0.00275 0.00371 0.00259 0.00289 0.00241 0.00134 H3 1.15831 0.60555 0.37259 1.00000 0.05592 0.00000 0.00000 C4 1.05667 0.76916 0.35380 1.00000 0.03944 0.03143 0.04754 -0.00357 0.02753 0.00153 0.03646 0.01116 0.00037 0.00054 0.00037 0.00000 0.00272 0.00261 0.00263 0.00230 0.00221 0.00227 0.00112 C5 0.99193 0.78483 0.25419 1.00000 0.03808 0.03608 0.05537 -0.01229 0.03313 -0.00842 0.03862 0.01079 0.00037 0.00055 0.00038 0.00000 0.00267 0.00295 0.00294 0.00233 0.00228 0.00221 0.00117 C6 1.03153 0.73968 0.18518 1.00000 0.04471 0.05431 0.05173 -0.00995 0.02904 0.00004 0.04746 0.01228 0.00041 0.00066 0.00041 0.00000 0.00317 0.00331 0.00318 0.00266 0.00267 0.00252 0.00132 C7 1.10369 0.81632 0.17659 1.00000 0.04817 0.06274 0.06833 -0.02519 0.03969 -0.00865 0.05466 0.01278 0.00043 0.00072 0.00044 0.00000 0.00334 0.00375 0.00381 0.00315 0.00294 0.00283 0.00155 F1 1.13695 0.93275 0.22916 1.00000 0.11597 0.09063 0.14780 -0.07135 0.11117 -0.06204 0.09868 0.00934 0.00035 0.00049 0.00036 0.00000 0.00358 0.00315 0.00394 0.00295 0.00333 0.00273 0.00170 C8 1.14252 0.78043 0.11597 1.00000 0.06133 0.10420 0.09548 -0.03512 0.06022 -0.02208 0.07763 0.01581 0.00052 0.00095 0.00056 0.00000 0.00408 0.00567 0.00515 0.00443 0.00391 0.00396 0.00219 F2 1.21373 0.85406 0.11152 1.00000 0.13908 0.13706 0.17251 -0.05360 0.13421 -0.04752 0.12550 0.01205 0.00042 0.00066 0.00043 0.00000 0.00456 0.00452 0.00524 0.00402 0.00450 0.00378 0.00220 C9 1.11286 0.64795 0.06597 1.00000 0.07500 0.12179 0.07272 -0.04037 0.04847 -0.00320 0.08409 0.01688 0.00057 0.00105 0.00054 0.00000 0.00493 0.00613 0.00480 0.00455 0.00404 0.00412 0.00230 F3 1.15245 0.61205 0.00812 1.00000 0.12770 0.21030 0.13604 -0.09741 0.09684 -0.01944 0.14391 0.01228 0.00044 0.00080 0.00043 0.00000 0.00408 0.00702 0.00428 0.00473 0.00361 0.00425 0.00269 C10 1.04702 0.56856 0.07712 1.00000 0.09533 0.10268 0.09604 -0.05996 0.05266 -0.01789 0.09434 0.01703 0.00064 0.00106 0.00062 0.00000 0.00601 0.00616 0.00572 0.00531 0.00452 0.00474 0.00264 F4 1.02218 0.43898 0.03229 1.00000 0.17699 0.13410 0.20048 -0.10500 0.12556 -0.03682 0.15519 0.01409 0.00055 0.00074 0.00054 0.00000 0.00600 0.00483 0.00648 0.00491 0.00534 0.00422 0.00278 C11 1.00751 0.60759 0.13729 1.00000 0.07683 0.08846 0.10214 -0.05173 0.05607 -0.02768 0.08317 0.01546 0.00057 0.00092 0.00060 0.00000 0.00484 0.00533 0.00560 0.00462 0.00422 0.00411 0.00237 F5 0.93786 0.52492 0.14417 1.00000 0.18246 0.08910 0.24832 -0.09788 0.16159 -0.06371 0.14897 0.01311 0.00049 0.00058 0.00053 0.00000 0.00598 0.00355 0.00730 0.00435 0.00582 0.00386 0.00276 C12 0.89820 0.83813 0.21722 1.00000 0.04391 0.03345 0.04504 -0.01034 0.02528 -0.00494 0.03879 0.01056 0.00037 0.00056 0.00036 0.00000 0.00273 0.00276 0.00281 0.00238 0.00222 0.00230 0.00115 N2 0.84500 0.86446 0.26868 1.00000 0.03745 0.03656 0.03905 0.00115 0.02452 0.00221 0.03492 0.00865 0.00028 0.00044 0.00029 0.00000 0.00222 0.00241 0.00220 0.00190 0.00185 0.00189 0.00095 H2N 0.86203 0.82083 0.33237 1.00000 0.05743 0.00000 0.01702 C13 0.83369 0.87323 0.11940 1.00000 0.03751 0.05864 0.04365 -0.00931 0.02493 -0.01263 0.04408 0.01095 0.00037 0.00064 0.00038 0.00000 0.00279 0.00349 0.00278 0.00262 0.00227 0.00260 0.00129 H13 0.84954 0.86759 0.06685 1.00000 0.05289 0.00000 0.00000 C14 0.74619 0.91592 0.11337 1.00000 0.04219 0.05460 0.03600 -0.00691 0.02101 -0.00454 0.04295 0.01145 0.00040 0.00062 0.00038 0.00000 0.00293 0.00346 0.00268 0.00248 0.00227 0.00254 0.00128 H14 0.69147 0.94753 0.05659 1.00000 0.05154 0.00000 0.00000 C15 0.75058 0.90508 0.20767 1.00000 0.03903 0.03076 0.04421 -0.00407 0.02000 -0.00226 0.03748 0.01062 0.00037 0.00054 0.00036 0.00000 0.00268 0.00272 0.00287 0.00232 0.00230 0.00224 0.00116 C16 0.67562 0.91914 0.23313 1.00000 0.03610 0.03470 0.03930 -0.00260 0.02084 -0.00126 0.03522 0.01054 0.00036 0.00054 0.00035 0.00000 0.00261 0.00279 0.00262 0.00217 0.00207 0.00216 0.00112 C17 0.57529 0.94373 0.15468 1.00000 0.03395 0.04884 0.03702 0.00423 0.02187 0.00533 0.03770 0.01158 0.00037 0.00059 0.00036 0.00000 0.00265 0.00280 0.00275 0.00234 0.00217 0.00228 0.00115 C18 0.53300 1.07827 0.12847 1.00000 0.04228 0.06219 0.04170 -0.00031 0.01937 0.00276 0.04851 0.01242 0.00041 0.00071 0.00039 0.00000 0.00295 0.00345 0.00297 0.00272 0.00234 0.00260 0.00131 F6 0.58296 1.19388 0.17375 1.00000 0.05347 0.04596 0.07160 0.00039 0.01463 0.01541 0.06198 0.00759 0.00025 0.00037 0.00026 0.00000 0.00203 0.00186 0.00223 0.00171 0.00171 0.00159 0.00095 C19 0.43785 1.09641 0.05863 1.00000 0.04236 0.08285 0.05058 0.00700 0.01548 0.01767 0.06058 0.01451 0.00045 0.00083 0.00044 0.00000 0.00316 0.00410 0.00349 0.00326 0.00261 0.00299 0.00158 F7 0.39960 1.22840 0.03770 1.00000 0.06296 0.10704 0.06946 0.02130 0.01535 0.04597 0.08514 0.00953 0.00029 0.00051 0.00027 0.00000 0.00238 0.00323 0.00248 0.00228 0.00195 0.00235 0.00131 C20 0.38426 0.97863 0.01202 1.00000 0.03280 0.11545 0.03164 0.00633 0.00830 0.00869 0.06224 0.01424 0.00044 0.00092 0.00041 0.00000 0.00321 0.00442 0.00308 0.00324 0.00247 0.00314 0.00161 F8 0.29097 0.99627 -0.05651 1.00000 0.03578 0.17902 0.04269 -0.00073 0.00178 0.00271 0.09171 0.00800 0.00025 0.00059 0.00024 0.00000 0.00192 0.00495 0.00200 0.00245 0.00154 0.00232 0.00157 C21 0.42109 0.84351 0.03383 1.00000 0.05248 0.07928 0.04457 -0.01948 0.02319 -0.01680 0.05822 0.01258 0.00046 0.00084 0.00041 0.00000 0.00333 0.00392 0.00325 0.00308 0.00261 0.00295 0.00149 F9 0.36736 0.72818 -0.00911 1.00000 0.05826 0.13098 0.07238 -0.02702 0.01534 -0.03269 0.09238 0.00797 0.00028 0.00057 0.00029 0.00000 0.00249 0.00395 0.00257 0.00261 0.00201 0.00253 0.00144 C22 0.51681 0.82472 0.10636 1.00000 0.03995 0.05899 0.04123 -0.00342 0.01694 -0.00457 0.04717 0.01157 0.00040 0.00070 0.00038 0.00000 0.00282 0.00332 0.00293 0.00268 0.00223 0.00253 0.00130 F10 0.55294 0.69275 0.12784 1.00000 0.06744 0.05112 0.06819 -0.00224 0.02401 -0.01188 0.06461 0.00744 0.00027 0.00039 0.00026 0.00000 0.00234 0.00203 0.00225 0.00177 0.00184 0.00177 0.00098 C23 0.68401 0.89159 0.32713 1.00000 0.03542 0.02631 0.04515 0.00566 0.02265 0.00543 0.03390 0.01066 0.00035 0.00051 0.00036 0.00000 0.00266 0.00243 0.00262 0.00217 0.00218 0.00213 0.00108 N3 0.76698 0.85641 0.40539 1.00000 0.03653 0.02419 0.03927 0.00269 0.02515 0.00161 0.03028 0.00817 0.00027 0.00040 0.00027 0.00000 0.00213 0.00203 0.00210 0.00168 0.00178 0.00173 0.00087 C24 0.59970 0.88692 0.34751 1.00000 0.03269 0.04730 0.04144 0.00624 0.02182 0.00950 0.03852 0.01148 0.00037 0.00059 0.00037 0.00000 0.00256 0.00311 0.00276 0.00245 0.00215 0.00236 0.00120 H24 0.53418 0.91160 0.30454 1.00000 0.04623 0.00000 0.00000 C25 0.63253 0.84111 0.43854 1.00000 0.02832 0.04344 0.05441 0.00720 0.02654 0.00591 0.03906 0.01121 0.00035 0.00058 0.00037 0.00000 0.00247 0.00304 0.00303 0.00259 0.00225 0.00234 0.00119 H25 0.59453 0.82500 0.47215 1.00000 0.04688 0.00000 0.00000 C26 0.73798 0.82068 0.47623 1.00000 0.03358 0.02228 0.04400 0.00289 0.02293 -0.00055 0.03121 0.01019 0.00034 0.00050 0.00035 0.00000 0.00247 0.00235 0.00253 0.00209 0.00203 0.00201 0.00104 C27 0.79901 0.76907 0.56732 1.00000 0.03518 0.02442 0.04386 -0.00076 0.02514 0.00029 0.03171 0.01050 0.00035 0.00051 0.00035 0.00000 0.00242 0.00236 0.00260 0.00211 0.00209 0.00205 0.00103 C28 0.75301 0.71038 0.62762 1.00000 0.03824 0.03446 0.04320 0.00606 0.02466 0.00248 0.03624 0.01110 0.00036 0.00053 0.00037 0.00000 0.00277 0.00264 0.00270 0.00216 0.00231 0.00215 0.00111 C29 0.69474 0.58846 0.59945 1.00000 0.03715 0.04891 0.04790 0.00717 0.02365 -0.00873 0.04293 0.01153 0.00037 0.00064 0.00039 0.00000 0.00290 0.00317 0.00305 0.00256 0.00247 0.00239 0.00127 F11 0.67941 0.52001 0.51910 1.00000 0.05461 0.05483 0.06056 -0.00630 0.03008 -0.02264 0.05505 0.00664 0.00023 0.00036 0.00024 0.00000 0.00204 0.00199 0.00203 0.00164 0.00160 0.00162 0.00089 C30 0.65393 0.53423 0.65559 1.00000 0.03838 0.05897 0.06563 0.01485 0.02181 -0.01274 0.05487 0.01311 0.00042 0.00072 0.00047 0.00000 0.00312 0.00372 0.00348 0.00287 0.00275 0.00274 0.00147 F12 0.59868 0.41437 0.62788 1.00000 0.07146 0.08159 0.09080 0.01009 0.04072 -0.03409 0.07963 0.00842 0.00029 0.00045 0.00029 0.00000 0.00262 0.00283 0.00274 0.00223 0.00219 0.00221 0.00125 C31 0.67111 0.59910 0.74063 1.00000 0.04212 0.08233 0.04969 0.01370 0.02919 -0.01046 0.05482 0.01346 0.00041 0.00078 0.00042 0.00000 0.00319 0.00424 0.00327 0.00286 0.00268 0.00296 0.00151 F13 0.63138 0.54624 0.79525 1.00000 0.06473 0.12586 0.06946 0.01727 0.04361 -0.02162 0.08161 0.00876 0.00027 0.00054 0.00027 0.00000 0.00246 0.00359 0.00235 0.00240 0.00198 0.00245 0.00127 C32 0.73085 0.72084 0.77166 1.00000 0.04900 0.06717 0.04689 0.01030 0.02888 0.00901 0.05158 0.01352 0.00043 0.00070 0.00041 0.00000 0.00335 0.00393 0.00315 0.00274 0.00267 0.00273 0.00140 F14 0.74865 0.77917 0.85495 1.00000 0.08286 0.10394 0.05114 -0.00476 0.04482 -0.00663 0.07378 0.00837 0.00029 0.00049 0.00025 0.00000 0.00260 0.00310 0.00205 0.00201 0.00193 0.00234 0.00113 C33 0.76949 0.77281 0.71323 1.00000 0.04541 0.04562 0.04911 0.00042 0.02852 -0.00353 0.04396 0.01203 0.00040 0.00064 0.00039 0.00000 0.00312 0.00310 0.00300 0.00253 0.00255 0.00257 0.00125 F15 0.82584 0.89218 0.74435 1.00000 0.07274 0.05455 0.05659 -0.01020 0.04093 -0.01031 0.05682 0.00707 0.00026 0.00038 0.00023 0.00000 0.00224 0.00200 0.00201 0.00161 0.00176 0.00173 0.00088 C34 0.90217 0.76145 0.60820 1.00000 0.03132 0.03069 0.03237 0.00035 0.01886 -0.00028 0.02974 0.00992 0.00033 0.00052 0.00032 0.00000 0.00229 0.00243 0.00248 0.00206 0.00196 0.00208 0.00101 N4 0.95634 0.83259 0.57168 1.00000 0.03401 0.02820 0.04106 0.00763 0.01956 0.00192 0.03339 0.00870 0.00028 0.00044 0.00029 0.00000 0.00215 0.00203 0.00228 0.00192 0.00183 0.00176 0.00091 H4N 0.92913 0.87868 0.51773 1.00000 0.04281 0.00000 0.01552 C35 0.96928 0.68759 0.68884 1.00000 0.03848 0.03627 0.04313 0.00655 0.02333 0.00397 0.03741 0.01090 0.00036 0.00056 0.00036 0.00000 0.00275 0.00279 0.00290 0.00228 0.00231 0.00230 0.00116 H35 0.95406 0.62710 0.72964 1.00000 0.04489 0.00000 0.00000 C36 1.06228 0.71797 0.69903 1.00000 0.03902 0.03261 0.04273 0.01221 0.01767 -0.00244 0.03835 0.01097 0.00038 0.00053 0.00036 0.00000 0.00274 0.00281 0.00285 0.00223 0.00227 0.00220 0.00120 H36 1.12174 0.68085 0.74781 1.00000 0.04602 0.00000 0.00000 C37 1.05400 0.81098 0.62661 1.00000 0.03252 0.02452 0.03592 -0.00315 0.01787 -0.00087 0.03003 0.00973 0.00034 0.00049 0.00033 0.00000 0.00238 0.00235 0.00252 0.00201 0.00202 0.00194 0.00102 C38 1.13014 0.88346 0.60406 1.00000 0.03479 0.03268 0.05339 0.00132 0.02877 -0.00073 0.03691 0.01112 0.00036 0.00055 0.00037 0.00000 0.00257 0.00262 0.00288 0.00233 0.00225 0.00222 0.00112 C39 1.23166 0.85701 0.68682 1.00000 0.03789 0.05786 0.05429 -0.00092 0.02199 -0.00731 0.04950 0.01148 0.00038 0.00069 0.00039 0.00000 0.00279 0.00372 0.00323 0.00288 0.00242 0.00264 0.00140 H39A 1.24364 0.75327 0.69588 1.00000 0.07425 0.00000 0.00000 H39B 1.23525 0.89947 0.74615 1.00000 0.07425 0.00000 0.00000 H39C 1.28120 0.90133 0.67152 1.00000 0.07425 0.00000 0.00000 C40 1.11031 1.04468 0.59130 1.00000 0.05283 0.02817 0.05442 -0.00692 0.02956 -0.01554 0.04306 0.01097 0.00041 0.00054 0.00039 0.00000 0.00330 0.00257 0.00322 0.00241 0.00263 0.00239 0.00128 H40A 1.04725 1.06168 0.53522 1.00000 0.06460 0.00000 0.00000 H40B 1.16237 1.09199 0.58134 1.00000 0.06460 0.00000 0.00000 H40C 1.10856 1.08402 0.64912 1.00000 0.06460 0.00000 0.00000 C41_a 0.53442 0.05279 0.68844 0.61517 0.07279 0.07568 0.08359 0.02480 0.04282 0.02576 0.07443 0.02511 0.00099 0.00131 0.00079 0.01577 0.00619 0.00718 0.00535 0.00526 0.00459 0.00537 0.00259 H41_a 0.47669 0.11866 0.66604 0.61517 0.08931 0.01577 0.00000 Cl1_a 0.57502 0.05216 0.60075 0.61517 0.06590 0.07357 0.06629 -0.01212 0.03494 0.00507 0.06658 0.00957 0.00043 0.00071 0.00032 0.01577 0.00276 0.00392 0.00265 0.00266 0.00210 0.00244 0.00171 Cl2_a 0.62167 0.11864 0.79615 0.61517 0.09107 0.12576 0.07567 -0.01022 0.04027 0.02644 0.09640 0.01394 0.00039 0.00089 0.00033 0.01577 0.00301 0.00501 0.00235 0.00258 0.00201 0.00292 0.00212 Cl3_a 0.49536 -0.11706 0.70316 0.61517 0.06028 0.08298 0.22836 0.07167 0.07031 0.01769 0.12173 0.02342 0.00034 0.00079 0.00091 0.01577 0.00229 0.00377 0.00866 0.00486 0.00361 0.00225 0.00361 C42_b 0.51820 0.00277 0.66713 0.38483 0.07279 0.07568 0.08359 0.02480 0.04282 0.02576 0.07443 0.03758 0.00164 0.00210 0.00108 0.01577 0.00619 0.00718 0.00535 0.00526 0.00459 0.00537 0.00259 H42_b 0.45856 0.06446 0.64601 0.38483 0.08931 0.01577 0.00000 Cl4_b 0.58363 0.05518 0.60557 0.38483 0.20837 0.11751 0.20752 0.04525 0.16119 0.04262 0.15238 0.03423 0.00131 0.00185 0.00110 0.01577 0.01596 0.01133 0.01240 0.01035 0.01256 0.00957 0.00684 Cl5_b 0.58894 0.02440 0.78951 0.38483 0.17229 0.17910 0.09979 -0.00395 0.04561 0.08565 0.15607 0.04073 0.00130 0.00225 0.00065 0.01577 0.01121 0.01360 0.00504 0.00616 0.00541 0.01027 0.00632 Cl6_b 0.48231 -0.17605 0.64265 0.38483 0.10869 0.09070 0.14807 0.04426 0.05772 0.04761 0.11571 0.03244 0.00069 0.00128 0.00108 0.01577 0.00548 0.00519 0.00858 0.00511 0.00516 0.00397 0.00322 Final Structure Factor Calculation for UDel1Mo in P2(1) Total number of l.s. parameters = 605 Maximum vector length = 511 Memory required = 7115 / 26068 wR2 = 0.1861 before cycle 9 for 6904 data and 2 / 605 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint 0.0304 0.0100 DELU C42_b Cl6_b Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 33. 0. 0. 0. 183. 18. 402. 0. rms sigma 0.000 0.000 0.000 0.023 0.000 0.000 0.000 0.010 0.080 0.100 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.007 0.070 0.024 0.000 GooF = S = 1.023; Restrained GooF = 0.986 for 637 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1023 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0659 for 4580 Fo > 4sig(Fo) and 0.1073 for all 6904 data wR2 = 0.1861, GooF = S = 1.023, Restrained GooF = 0.986 for all data Flack x parameter = 0.0303 with esd 0.1190 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 63.00 for non-hydrogen and 18.00 for hydrogen atoms Principal mean square atomic displacements U 0.0463 0.0318 0.0219 N1 0.0470 0.0337 0.0199 C1 0.0545 0.0437 0.0281 C2 0.0756 0.0391 0.0251 C3 0.0503 0.0343 0.0248 C4 0.0638 0.0302 0.0218 C5 0.0631 0.0486 0.0308 C6 0.0914 0.0460 0.0265 C7 0.2189 0.0424 0.0348 F1 may be split into 1.1497 0.9209 0.2373 and 1.1242 0.9446 0.2210 0.1385 0.0670 0.0274 C8 0.2379 0.1017 0.0369 F2 0.1449 0.0776 0.0298 C9 0.2774 0.1263 0.0280 F3 0.1594 0.0887 0.0349 C10 0.2819 0.1394 0.0443 F4 0.1491 0.0582 0.0422 C11 0.3129 0.0918 0.0422 F5 may be split into 0.9527 0.5146 0.1552 and 0.9230 0.5352 0.1332 0.0529 0.0368 0.0267 C12 0.0439 0.0362 0.0247 N2 0.0665 0.0393 0.0264 C13 0.0575 0.0407 0.0306 C14 0.0454 0.0375 0.0296 C15 0.0416 0.0340 0.0300 C16 0.0515 0.0373 0.0243 C17 0.0627 0.0423 0.0405 C18 0.0925 0.0596 0.0338 F6 0.0896 0.0569 0.0352 C19 0.1369 0.0874 0.0311 F7 0.1164 0.0432 0.0271 C20 0.1791 0.0681 0.0279 F8 0.0904 0.0484 0.0358 C21 0.1449 0.0921 0.0402 F9 0.0601 0.0429 0.0385 C22 0.0822 0.0667 0.0449 F10 0.0474 0.0305 0.0238 C23 0.0440 0.0243 0.0225 N3 0.0538 0.0375 0.0242 C24 0.0583 0.0400 0.0189 C25 0.0450 0.0278 0.0209 C26 0.0459 0.0256 0.0237 C27 0.0479 0.0333 0.0274 C28 0.0588 0.0466 0.0233 C29 0.0775 0.0578 0.0299 F11 0.0869 0.0520 0.0258 C30 0.1199 0.0895 0.0295 F12 0.0913 0.0520 0.0212 C31 0.1399 0.0767 0.0282 F13 0.0735 0.0470 0.0343 C32 0.1061 0.0822 0.0330 F14 0.0529 0.0465 0.0325 C33 0.0807 0.0502 0.0396 F15 0.0351 0.0307 0.0234 C34 0.0446 0.0315 0.0240 N4 0.0484 0.0333 0.0306 C35 0.0539 0.0392 0.0219 C36 0.0372 0.0294 0.0235 C37 0.0544 0.0329 0.0233 C38 0.0603 0.0546 0.0335 C39 0.0628 0.0460 0.0203 C40 0.1100 0.0651 0.0483 C41_a 0.0844 0.0690 0.0463 Cl1_a 0.1467 0.0833 0.0592 Cl2_a 0.2650 0.0538 0.0464 Cl3_a may be split into 0.5058 -0.1078 0.7180 and 0.4850 -0.1263 0.6883 0.1100 0.0651 0.0483 C42_b 0.2723 0.1007 0.0842 Cl4_b may be split into 0.5979 0.0622 0.6130 and 0.5693 0.0481 0.5981 0.2821 0.1007 0.0854 Cl5_b may be split into 0.5956 0.0402 0.7844 and 0.5823 0.0086 0.7946 0.1729 0.1249 0.0493 Cl6_b Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.017 0.026 0.034 0.042 0.052 0.064 0.080 0.104 0.152 1.000 Number in group 724. 698. 720. 685. 664. 676. 688. 680. 676. 693. GooF 0.948 1.029 1.030 1.014 1.049 1.104 0.986 1.027 1.038 1.002 K 1.258 1.110 1.017 1.016 1.022 1.026 1.020 1.036 1.012 1.006 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.26 1.44 1.80 inf Number in group 697. 714. 665. 706. 689. 671. 692. 689. 687. 694. GooF 0.896 0.952 1.006 0.983 0.946 0.927 0.980 1.030 1.098 1.340 K 1.034 1.001 1.004 1.023 1.006 1.013 1.019 1.028 1.009 1.009 R1 0.309 0.279 0.230 0.181 0.123 0.086 0.069 0.066 0.051 0.049 Recommended weighting scheme: WGHT 0.1027 0.1433 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) 3 2 4 85.78 23.62 6.29 0.029 2.07 5 3 4 65.56 12.15 5.60 0.021 1.55 1 0 2 155.38 85.13 5.05 0.054 5.30 2 3 1 694.61 439.17 4.56 0.124 2.67 0 0 2 433.90 765.41 4.31 0.163 6.94 4 3 4 34.97 1.25 4.23 0.007 1.69 7 0 4 281.25 164.07 4.21 0.076 1.45 -5 3 4 106.32 56.98 4.17 0.045 2.10 3 4 2 93.19 49.54 4.16 0.041 1.88 2 0 3 269.06 168.79 4.11 0.077 3.22 0 2 3 215.32 348.70 3.99 0.110 3.28 1 0 8 187.19 92.40 3.99 0.057 1.63 0 0 6 82.78 37.43 3.87 0.036 2.31 -4 2 1 176.70 103.34 3.86 0.060 2.91 1 0 3 335.43 556.76 3.69 0.139 3.88 -7 5 1 63.75 23.17 3.57 0.028 1.38 2 5 3 396.19 273.10 3.38 0.097 1.61 -2 0 1 362.65 255.23 3.32 0.094 7.63 2 0 10 41.14 9.67 3.31 0.018 1.25 4 3 3 938.14 672.20 3.30 0.153 1.85 4 0 3 233.66 150.95 3.28 0.072 2.30 -2 -9 7 189.45 97.55 3.27 0.058 0.93 -7 2 5 512.60 744.41 3.27 0.161 1.91 -4 5 8 149.54 236.79 3.24 0.091 1.34 -6 1 15 15.12 84.21 3.24 0.054 1.03 -2 1 7 102.73 64.08 3.23 0.047 2.12 2 5 0 43.63 21.40 3.19 0.027 1.79 -9 0 10 682.66 482.49 3.17 0.130 1.38 1 3 2 846.99 1193.17 3.14 0.204 2.68 3 1 1 2215.62 1622.90 3.13 0.238 3.56 1 4 0 201.47 135.54 3.12 0.069 2.29 -5 4 5 362.41 256.14 3.12 0.094 1.74 -17 2 8 -29.20 41.43 3.12 0.038 0.88 1 0 10 44.50 80.79 3.08 0.053 1.32 -10 3 1 103.22 43.90 3.03 0.039 1.29 2 3 5 82.16 48.43 3.02 0.041 1.82 1 9 5 26.20 78.04 3.00 0.052 0.96 -3 8 6 768.24 548.70 3.00 0.138 1.06 6 -2 4 31.43 3.26 2.97 0.011 1.52 2 0 2 2230.71 3082.42 2.96 0.327 4.05 5 4 5 66.65 109.47 2.95 0.062 1.33 8 -7 3 30.14 86.21 2.93 0.055 0.97 0 0 9 64.97 34.60 2.93 0.035 1.54 -4 0 3 35.94 14.93 2.93 0.023 3.63 -1 0 6 132.36 64.72 2.92 0.047 2.47 4 -3 3 907.53 668.20 2.92 0.152 1.85 3 2 3 358.30 260.43 2.91 0.095 2.33 5 4 4 358.86 504.28 2.91 0.132 1.42 4 -8 6 85.58 20.53 2.89 0.027 0.94 -11 0 11 739.40 533.16 2.89 0.136 1.19 Bond lengths and angles N1 - Distance Angles C1 1.3833 (0.0063) C4 1.3863 (0.0063) 109.78 (0.40) H1N 0.9940 123.50 123.83 N1 - C1 C4 C1 - Distance Angles C2 1.3816 (0.0070) N1 1.3833 (0.0063) 107.15 (0.44) C38 1.4945 (0.0070) 131.43 (0.46) 121.00 (0.42) C1 - C2 N1 C2 - Distance Angles C3 1.3818 (0.0078) C1 1.3816 (0.0070) 108.22 (0.46) H2 0.9500 125.89 125.89 C2 - C3 C1 C3 - Distance Angles C2 1.3818 (0.0078) C4 1.3990 (0.0075) 108.83 (0.48) H3 0.9500 125.59 125.59 C3 - C2 C4 C4 - Distance Angles N1 1.3863 (0.0063) C3 1.3990 (0.0075) 105.89 (0.46) C5 1.4212 (0.0072) 122.79 (0.43) 131.31 (0.49) C4 - N1 C3 C5 - Distance Angles C12 1.3754 (0.0071) C4 1.4212 (0.0072) 125.39 (0.45) C6 1.5060 (0.0072) 118.62 (0.47) 115.99 (0.44) C5 - C12 C4 C6 - Distance Angles C7 1.3688 (0.0082) C11 1.3966 (0.0091) 115.93 (0.56) C5 1.5060 (0.0072) 121.46 (0.51) 121.97 (0.57) C6 - C7 C11 C7 - Distance Angles F1 1.3130 (0.0070) C8 1.3589 (0.0085) 117.68 (0.57) C6 1.3688 (0.0082) 118.26 (0.50) 124.05 (0.59) C7 - F1 C8 F1 - Distance Angles C7 1.3130 (0.0070) F1 - C8 - Distance Angles F2 1.3137 (0.0080) C7 1.3589 (0.0084) 122.49 (0.65) C9 1.4175 (0.0112) 119.58 (0.61) 117.40 (0.66) C8 - F2 C7 F2 - Distance Angles C8 1.3137 (0.0080) F2 - C9 - Distance Angles C10 1.3203 (0.0118) F3 1.3297 (0.0079) 123.49 (0.79) C8 1.4175 (0.0112) 119.34 (0.63) 117.16 (0.78) C9 - C10 F3 F3 - Distance Angles C9 1.3297 (0.0079) F3 - C10 - Distance Angles C9 1.3203 (0.0118) F4 1.3573 (0.0100) 118.95 (0.73) C11 1.3681 (0.0106) 122.42 (0.75) 118.50 (0.87) C10 - C9 F4 F4 - Distance Angles C10 1.3573 (0.0100) F4 - C11 - Distance Angles F5 1.3554 (0.0091) C10 1.3681 (0.0106) 120.35 (0.67) C6 1.3966 (0.0091) 119.04 (0.60) 120.32 (0.75) C11 - F5 C10 F5 - Distance Angles C11 1.3554 (0.0091) F5 - C12 - Distance Angles C5 1.3754 (0.0071) N2 1.3925 (0.0062) 126.22 (0.47) C13 1.4291 (0.0075) 128.33 (0.47) 105.41 (0.44) C12 - C5 N2 N2 - Distance Angles C15 1.3781 (0.0064) C12 1.3925 (0.0062) 110.82 (0.41) H2N 0.9890 121.67 122.69 N2 - C15 C12 C13 - Distance Angles C14 1.3576 (0.0075) C12 1.4291 (0.0075) 109.31 (0.47) H13 0.9500 125.35 125.35 C13 - C14 C12 C14 - Distance Angles C13 1.3576 (0.0075) C15 1.4374 (0.0070) 108.25 (0.47) H14 0.9500 125.87 125.87 C14 - C13 C15 C15 - Distance Angles C16 1.3749 (0.0070) N2 1.3781 (0.0064) 125.46 (0.47) C14 1.4374 (0.0070) 128.31 (0.47) 106.01 (0.43) C15 - C16 N2 C16 - Distance Angles C15 1.3749 (0.0070) C23 1.4285 (0.0069) 124.77 (0.45) C17 1.4883 (0.0073) 117.78 (0.44) 116.82 (0.43) C16 - C15 C23 C17 - Distance Angles C18 1.3829 (0.0081) C22 1.4090 (0.0080) 116.86 (0.49) C16 1.4883 (0.0073) 123.68 (0.50) 119.39 (0.48) C17 - C18 C22 C18 - Distance Angles F6 1.3235 (0.0072) C19 1.3811 (0.0082) 118.19 (0.58) C17 1.3829 (0.0082) 119.70 (0.46) 122.06 (0.60) C18 - F6 C19 F6 - Distance Angles C18 1.3235 (0.0072) F6 - C19 - Distance Angles F7 1.3353 (0.0079) C20 1.3647 (0.0101) 120.98 (0.54) C18 1.3811 (0.0082) 119.72 (0.64) 119.31 (0.63) C19 - F7 C20 F7 - Distance Angles C19 1.3353 (0.0079) F7 - C20 - Distance Angles F8 1.3543 (0.0065) C21 1.3560 (0.0100) 118.80 (0.69) C19 1.3647 (0.0101) 119.36 (0.68) 121.82 (0.55) C20 - F8 C21 F8 - Distance Angles C20 1.3543 (0.0065) F8 - C21 - Distance Angles F9 1.3335 (0.0079) C20 1.3560 (0.0100) 121.74 (0.60) C22 1.4015 (0.0085) 119.29 (0.66) 118.92 (0.60) C21 - F9 C20 F9 - Distance Angles C21 1.3335 (0.0079) F9 - C22 - Distance Angles F10 1.3253 (0.0071) C21 1.4015 (0.0085) 119.02 (0.55) C17 1.4090 (0.0080) 119.95 (0.47) 121.01 (0.60) C22 - F10 C21 F10 - Distance Angles C22 1.3253 (0.0071) F10 - C23 - Distance Angles N3 1.3459 (0.0061) C16 1.4285 (0.0069) 125.60 (0.44) C24 1.4586 (0.0070) 111.39 (0.42) 122.82 (0.43) C23 - N3 C16 N3 - Distance Angles C23 1.3459 (0.0061) C26 1.3964 (0.0060) 105.35 (0.38) N3 - C23 C24 - Distance Angles C25 1.3389 (0.0070) C23 1.4586 (0.0070) 106.70 (0.43) H24 0.9500 126.65 126.65 C24 - C25 C23 C25 - Distance Angles C24 1.3389 (0.0070) C26 1.4605 (0.0069) 106.82 (0.43) H25 0.9500 126.59 126.59 C25 - C24 C26 C26 - Distance Angles C27 1.3847 (0.0067) N3 1.3964 (0.0060) 125.39 (0.42) C25 1.4605 (0.0069) 124.93 (0.44) 109.64 (0.41) C26 - C27 N3 C27 - Distance Angles C26 1.3847 (0.0067) C34 1.4139 (0.0066) 125.59 (0.43) C28 1.5017 (0.0067) 118.16 (0.43) 116.20 (0.43) C27 - C26 C34 C28 - Distance Angles C33 1.3654 (0.0073) C29 1.3859 (0.0074) 117.85 (0.47) C27 1.5017 (0.0067) 121.15 (0.47) 120.98 (0.47) C28 - C33 C29 C29 - Distance Angles F11 1.3236 (0.0064) C30 1.3739 (0.0081) 118.76 (0.51) C28 1.3859 (0.0074) 120.54 (0.45) 120.68 (0.55) C29 - F11 C30 F11 - Distance Angles C29 1.3236 (0.0064) F11 - C30 - Distance Angles F12 1.3471 (0.0071) C31 1.3646 (0.0092) 119.73 (0.53) C29 1.3739 (0.0081) 119.92 (0.60) 120.32 (0.55) C30 - F12 C31 F12 - Distance Angles C30 1.3471 (0.0072) F12 - C31 - Distance Angles F13 1.3372 (0.0064) C30 1.3646 (0.0092) 120.29 (0.58) C32 1.3976 (0.0089) 119.42 (0.58) 120.28 (0.51) C31 - F13 C30 F13 - Distance Angles C31 1.3372 (0.0064) F13 - C32 - Distance Angles F14 1.3124 (0.0067) C33 1.3720 (0.0076) 122.94 (0.58) C31 1.3976 (0.0089) 119.30 (0.51) 117.75 (0.54) C32 - F14 C33 F14 - Distance Angles C32 1.3124 (0.0067) F14 - C33 - Distance Angles F15 1.3544 (0.0067) C28 1.3654 (0.0073) 120.40 (0.46) C32 1.3720 (0.0076) 116.50 (0.50) 123.10 (0.54) C33 - F15 C28 F15 - Distance Angles C33 1.3544 (0.0067) F15 - C34 - Distance Angles N4 1.3651 (0.0060) C35 1.3929 (0.0068) 105.76 (0.40) C27 1.4139 (0.0066) 123.47 (0.43) 130.77 (0.44) C34 - N4 C35 N4 - Distance Angles C37 1.3626 (0.0061) C34 1.3651 (0.0060) 111.55 (0.40) H4N 0.8634 126.67 121.60 N4 - C37 C34 C35 - Distance Angles C36 1.3872 (0.0071) C34 1.3929 (0.0068) 107.91 (0.43) H35 0.9500 126.05 126.05 C35 - C36 C34 C36 - Distance Angles C37 1.3778 (0.0065) C35 1.3872 (0.0071) 108.62 (0.45) H36 0.9500 125.69 125.69 C36 - C37 C35 C37 - Distance Angles N4 1.3626 (0.0061) C36 1.3778 (0.0065) 106.12 (0.42) C38 1.5150 (0.0069) 122.01 (0.41) 131.87 (0.44) C37 - N4 C36 C38 - Distance Angles C1 1.4945 (0.0070) C37 1.5150 (0.0068) 106.85 (0.40) C40 1.5243 (0.0075) 111.60 (0.43) 109.79 (0.40) C39 1.5277 (0.0074) 109.62 (0.41) 109.33 (0.42) 109.61 (0.45) C38 - C1 C37 C40 C39 - Distance Angles C38 1.5277 (0.0073) H39A 0.9800 109.47 H39B 0.9800 109.47 109.47 H39C 0.9800 109.47 109.47 109.47 C39 - C38 H39A H39B C40 - Distance Angles C38 1.5243 (0.0075) H40A 0.9800 109.47 H40B 0.9800 109.47 109.47 H40C 0.9800 109.47 109.47 109.47 C40 - C38 H40A H40B C41_a - Distance Angles Cl2_a 1.7178 (0.0102) Cl1_a 1.7293 (0.0101) 111.74 (0.68) Cl3_a 1.7389 (0.0099) 111.02 (0.63) 111.43 (0.67) H41_a 1.0000 107.47 107.47 107.47 C41_a - Cl2_a Cl1_a Cl3_a Cl1_a - Distance Angles C41_a 1.7293 (0.0101) Cl1_a - Cl2_a - Distance Angles C41_a 1.7178 (0.0103) Cl2_a - Cl3_a - Distance Angles C41_a 1.7389 (0.0100) Cl3_a - C42_b - Distance Angles Cl5_b 1.7251 (0.0129) Cl4_b 1.7333 (0.0132) 109.95 (1.04) Cl6_b 1.7385 (0.0128) 109.45 (0.95) 110.60 (1.04) H42_b 1.0000 108.94 108.94 108.94 C42_b - Cl5_b Cl4_b Cl6_b Cl4_b - Distance Angles C42_b 1.7333 (0.0132) Cl4_b - Cl5_b - Distance Angles C42_b 1.7251 (0.0129) Cl5_b - Cl6_b - Distance Angles C42_b 1.7385 (0.0129) Cl6_b - Selected torsion angles -3.83 ( 0.52) C4 - N1 - C1 - C2 -177.21 ( 0.43) C4 - N1 - C1 - C38 3.47 ( 0.56) N1 - C1 - C2 - C3 175.90 ( 0.50) C38 - C1 - C2 - C3 -1.88 ( 0.62) C1 - C2 - C3 - C4 2.65 ( 0.53) C1 - N1 - C4 - C3 -178.18 ( 0.46) C1 - N1 - C4 - C5 -0.45 ( 0.59) C2 - C3 - C4 - N1 -179.53 ( 0.54) C2 - C3 - C4 - C5 -24.81 ( 0.80) N1 - C4 - C5 - C12 154.13 ( 0.57) C3 - C4 - C5 - C12 154.63 ( 0.48) N1 - C4 - C5 - C6 -26.42 ( 0.85) C3 - C4 - C5 - C6 110.02 ( 0.64) C12 - C5 - C6 - C7 -69.46 ( 0.75) C4 - C5 - C6 - C7 -79.51 ( 0.80) C12 - C5 - C6 - C11 101.01 ( 0.73) C4 - C5 - C6 - C11 -172.15 ( 0.70) C11 - C6 - C7 - F1 -1.14 ( 0.93) C5 - C6 - C7 - F1 8.68 ( 1.04) C11 - C6 - C7 - C8 179.69 ( 0.67) C5 - C6 - C7 - C8 2.85 ( 1.22) F1 - C7 - C8 - F2 -177.98 ( 0.76) C6 - C7 - C8 - F2 174.40 ( 0.71) F1 - C7 - C8 - C9 -6.42 ( 1.17) C6 - C7 - C8 - C9 174.37 ( 0.91) F2 - C8 - C9 - C10 2.56 ( 1.30) C7 - C8 - C9 - C10 -6.96 ( 1.26) F2 - C8 - C9 - F3 -178.77 ( 0.75) C7 - C8 - C9 - F3 4.26 ( 1.52) F3 - C9 - C10 - F4 -177.16 ( 0.85) C8 - C9 - C10 - F4 179.82 ( 0.87) F3 - C9 - C10 - C11 -1.59 ( 1.51) C8 - C9 - C10 - C11 177.93 ( 0.92) C9 - C10 - C11 - F5 -6.48 ( 1.46) F4 - C10 - C11 - F5 4.09 ( 1.51) C9 - C10 - C11 - C6 179.68 ( 0.81) F4 - C10 - C11 - C6 178.83 ( 0.75) C7 - C6 - C11 - F5 7.87 ( 1.16) C5 - C6 - C11 - F5 -7.24 ( 1.16) C7 - C6 - C11 - C10 -178.21 ( 0.75) C5 - C6 - C11 - C10 -10.84 ( 0.84) C4 - C5 - C12 - N2 169.73 ( 0.49) C6 - C5 - C12 - N2 171.60 ( 0.53) C4 - C5 - C12 - C13 -7.84 ( 0.84) C6 - C5 - C12 - C13 -174.46 ( 0.49) C5 - C12 - N2 - C15 3.56 ( 0.55) C13 - C12 - N2 - C15 177.02 ( 0.53) C5 - C12 - C13 - C14 -0.94 ( 0.61) N2 - C12 - C13 - C14 -1.87 ( 0.64) C12 - C13 - C14 - C15 170.32 ( 0.49) C12 - N2 - C15 - C16 -4.67 ( 0.55) C12 - N2 - C15 - C14 -170.82 ( 0.54) C13 - C14 - C15 - C16 3.98 ( 0.60) C13 - C14 - C15 - N2 -0.94 ( 0.82) N2 - C15 - C16 - C23 172.92 ( 0.50) C14 - C15 - C16 - C23 -171.47 ( 0.47) N2 - C15 - C16 - C17 2.39 ( 0.82) C14 - C15 - C16 - C17 -96.48 ( 0.64) C15 - C16 - C17 - C18 92.22 ( 0.63) C23 - C16 - C17 - C18 86.70 ( 0.63) C15 - C16 - C17 - C22 -84.59 ( 0.61) C23 - C16 - C17 - C22 177.48 ( 0.50) C22 - C17 - C18 - F6 0.60 ( 0.81) C16 - C17 - C18 - F6 0.29 ( 0.83) C22 - C17 - C18 - C19 -176.60 ( 0.53) C16 - C17 - C18 - C19 1.04 ( 0.89) F6 - C18 - C19 - F7 178.28 ( 0.53) C17 - C18 - C19 - F7 -178.92 ( 0.56) F6 - C18 - C19 - C20 -1.68 ( 0.94) C17 - C18 - C19 - C20 0.07 ( 0.94) F7 - C19 - C20 - F8 -179.97 ( 0.55) C18 - C19 - C20 - F8 -178.47 ( 0.62) F7 - C19 - C20 - C21 1.49 ( 0.99) C18 - C19 - C20 - C21 -1.23 ( 0.93) F8 - C20 - C21 - F9 177.31 ( 0.59) C19 - C20 - C21 - F9 -178.46 ( 0.50) F8 - C20 - C21 - C22 0.08 ( 0.98) C19 - C20 - C21 - C22 2.65 ( 0.85) F9 - C21 - C22 - F10 179.95 ( 0.55) C20 - C21 - C22 - F10 -178.82 ( 0.51) F9 - C21 - C22 - C17 -1.52 ( 0.89) C20 - C21 - C22 - C17 179.84 ( 0.50) C18 - C17 - C22 - F10 -3.14 ( 0.77) C16 - C17 - C22 - F10 1.32 ( 0.79) C18 - C17 - C22 - C21 178.34 ( 0.50) C16 - C17 - C22 - C21 4.16 ( 0.81) C15 - C16 - C23 - N3 174.78 ( 0.47) C17 - C16 - C23 - N3 -170.55 ( 0.51) C15 - C16 - C23 - C24 0.07 ( 0.71) C17 - C16 - C23 - C24 -172.06 ( 0.46) C16 - C23 - N3 - C26 3.17 ( 0.53) C24 - C23 - N3 - C26 -3.04 ( 0.61) N3 - C23 - C24 - C25 172.34 ( 0.47) C16 - C23 - C24 - C25 1.49 ( 0.57) C23 - C24 - C25 - C26 175.79 ( 0.47) C23 - N3 - C26 - C27 -2.20 ( 0.51) C23 - N3 - C26 - C25 -177.64 ( 0.50) C24 - C25 - C26 - C27 0.37 ( 0.56) C24 - C25 - C26 - N3 8.67 ( 0.80) N3 - C26 - C27 - C34 -173.64 ( 0.46) C25 - C26 - C27 - C34 -168.81 ( 0.43) N3 - C26 - C27 - C28 8.88 ( 0.75) C25 - C26 - C27 - C28 -117.46 ( 0.57) C26 - C27 - C28 - C33 64.82 ( 0.65) C34 - C27 - C28 - C33 64.47 ( 0.66) C26 - C27 - C28 - C29 -113.25 ( 0.54) C34 - C27 - C28 - C29 -177.29 ( 0.48) C33 - C28 - C29 - F11 0.85 ( 0.75) C27 - C28 - C29 - F11 1.00 ( 0.79) C33 - C28 - C29 - C30 179.13 ( 0.51) C27 - C28 - C29 - C30 -0.68 ( 0.84) F11 - C29 - C30 - F12 -179.00 ( 0.50) C28 - C29 - C30 - F12 177.65 ( 0.54) F11 - C29 - C30 - C31 -0.67 ( 0.90) C28 - C29 - C30 - C31 -1.66 ( 0.94) F12 - C30 - C31 - F13 -179.99 ( 0.55) C29 - C30 - C31 - F13 177.96 ( 0.55) F12 - C30 - C31 - C32 -0.37 ( 0.95) C29 - C30 - C31 - C32 1.52 ( 0.88) F13 - C31 - C32 - F14 -178.10 ( 0.57) C30 - C31 - C32 - F14 -179.34 ( 0.55) F13 - C31 - C32 - C33 1.04 ( 0.90) C30 - C31 - C32 - C33 -179.98 ( 0.48) C29 - C28 - C33 - F15 1.88 ( 0.78) C27 - C28 - C33 - F15 -0.30 ( 0.81) C29 - C28 - C33 - C32 -178.43 ( 0.51) C27 - C28 - C33 - C32 -1.91 ( 0.84) F14 - C32 - C33 - F15 178.99 ( 0.52) C31 - C32 - C33 - F15 178.40 ( 0.53) F14 - C32 - C33 - C28 -0.70 ( 0.86) C31 - C32 - C33 - C28 14.93 ( 0.78) C26 - C27 - C34 - N4 -167.54 ( 0.44) C28 - C27 - C34 - N4 -165.52 ( 0.53) C26 - C27 - C34 - C35 12.00 ( 0.77) C28 - C27 - C34 - C35 -1.84 ( 0.55) C35 - C34 - N4 - C37 177.80 ( 0.43) C27 - C34 - N4 - C37 0.65 ( 0.56) N4 - C34 - C35 - C36 -178.95 ( 0.51) C27 - C34 - C35 - C36 0.72 ( 0.57) C34 - C35 - C36 - C37 2.28 ( 0.54) C34 - N4 - C37 - C36 -177.27 ( 0.42) C34 - N4 - C37 - C38 -1.79 ( 0.54) C35 - C36 - C37 - N4 177.70 ( 0.50) C35 - C36 - C37 - C38 -94.42 ( 0.59) C2 - C1 - C38 - C37 77.14 ( 0.53) N1 - C1 - C38 - C37 145.57 ( 0.53) C2 - C1 - C38 - C40 -42.88 ( 0.60) N1 - C1 - C38 - C40 23.94 ( 0.74) C2 - C1 - C38 - C39 -164.50 ( 0.44) N1 - C1 - C38 - C39 -70.36 ( 0.54) N4 - C37 - C38 - C1 110.21 ( 0.58) C36 - C37 - C38 - C1 50.81 ( 0.62) N4 - C37 - C38 - C40 -128.62 ( 0.56) C36 - C37 - C38 - C40 171.08 ( 0.46) N4 - C37 - C38 - C39 -8.35 ( 0.74) C36 - C37 - C38 - C39 FMAP and GRID set by program FMAP 2 1 75 GRID -1.389 -2 -1 1.389 2 1 R1 = 0.0908 for 3701 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.49 at 0.0435 0.0648 0.0607 [ 1.78 A from F4 ] Deepest hole -0.35 at 0.9718 0.4654 0.2002 [ 0.96 A from F5 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 6655 / 56685 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9565 0.5648 -0.0607 1.00000 0.05 0.49 1.78 F4 1.96 C10 2.44 C9 2.65 F1 Q2 1 0.8821 0.6107 0.0642 1.00000 0.05 0.48 1.40 F5 1.74 C11 2.44 H13 2.47 C10 Q3 1 0.9894 0.6626 0.0023 1.00000 0.05 0.34 1.40 C10 1.70 C9 2.05 C11 2.14 F4 Q4 1 0.9601 0.6807 0.0679 1.00000 0.05 0.29 1.20 C11 1.64 C10 1.74 C6 1.99 F5 Q5 1 1.0680 0.7379 0.0045 1.00000 0.05 0.28 1.22 C9 1.64 C8 1.73 F3 2.04 C10 Q6 1 1.0669 0.9906 0.1639 1.00000 0.05 0.26 1.22 F1 1.70 C7 2.22 H35 2.45 C6 Q7 1 0.5438 1.1617 0.1153 1.00000 0.05 0.26 0.84 C18 0.89 F6 1.58 C19 2.08 F7 Q8 1 0.8772 0.9180 0.0611 1.00000 0.05 0.25 0.66 H13 1.40 C13 2.04 F3 2.41 C12 Q9 1 1.1064 0.7013 -0.0568 1.00000 0.05 0.25 1.25 F3 1.93 C9 2.59 C8 2.77 F2 Q10 1 0.9356 0.8161 0.4967 1.00000 0.05 0.25 0.70 H4N 1.07 N4 2.02 C37 2.07 C34 Q11 1 0.7419 0.1565 0.8574 1.00000 0.05 0.24 1.69 CL2 1.94 F2 1.99 C8 2.00 C9 Q12 1 0.6084 0.0064 0.5211 1.00000 0.05 0.23 1.58 CL4 1.59 CL1 1.82 H25 2.14 C25 Q13 1 0.6862 0.0599 0.8569 1.00000 0.05 0.22 1.15 CL2 1.42 CL5 2.47 F3 2.61 C41 Q14 1 0.8052 0.9617 0.1222 1.00000 0.05 0.22 0.94 C13 0.95 C14 1.58 H13 1.58 H14 Q15 1 0.6550 0.4674 0.6029 1.00000 0.05 0.22 1.03 C30 1.20 F12 1.29 C29 1.58 F11 Q16 1 0.3233 0.8396 -0.0337 1.00000 0.05 0.22 1.20 F9 1.39 C21 1.53 F8 1.57 C20 Q17 1 1.1385 0.9568 0.0438 1.00000 0.05 0.21 1.50 F2 1.97 C8 2.20 F4 2.68 C7 Q18 1 0.8512 0.8914 -0.0415 1.00000 0.05 0.21 1.71 H13 1.93 F4 1.97 F14 2.12 F3 Q19 1 0.4483 0.5205 0.0782 1.00000 0.05 0.21 2.15 F10 2.32 H14 2.36 CL5 2.37 F9 Q20 1 0.8194 0.7999 0.3716 1.00000 0.05 0.20 1.09 H2N 1.25 N3 1.90 N2 2.04 H40B Shortest distances between peaks (including symmetry equivalents) 11 13 1.23 1 3 1.26 3 4 1.29 2 4 1.34 5 9 1.37 3 5 1.38 8 18 1.48 1 6 1.63 8 14 1.79 1 17 1.88 10 20 1.96 2 17 2.12 1 5 2.23 1 4 2.25 5 17 2.25 2 3 2.29 4 5 2.33 3 9 2.37 4 8 2.52 6 17 2.57 1 9 2.59 3 17 2.60 4 18 2.64 8 9 2.65 1 2 2.68 13 19 2.69 4 17 2.70 6 8 2.70 9 17 2.76 13 18 2.78 3 6 2.82 5 11 2.83 3 18 2.86 2 8 2.86 1 8 2.89 9 11 2.95 14 18 3.00 11 18 3.00 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 0.02: 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. 0.09: 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 0.02: Generate idealized H-atoms 1.34: Structure factors and derivatives 8.09: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.06: Apply other restraints 1.67: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.08: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + udel1mo finished at 14:13:33 Total CPU time: 11.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++