++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XL - CRYSTAL STRUCTURE REFINEMENT - SHELXTL Version 2008/4 + + Copyright(c) 2008 Bruker Analytical X-ray Solutions All Rights Reserved + + udel1 started at 14:08:04 on 04-Feb-2011 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL UDEL1 in P2(1) CELL 1.54178 15.2855 9.2994 15.5097 90.000 116.573 90.000 ZERR 2.00 0.0005 0.0003 0.0005 0.000 0.002 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N F CL UNIT 82 36 8 30 6 V = 1971.75 F(000) = 956.0 Mu = 3.10 mm-1 Cell Wt = 1915.89 Rho = 1.613 TEMP -173.000 SIZE 0.036 0.039 0.44 L.S. 4 BOND $H ACTA CONF FMAP 2 PLAN -2 SIMU $CL SIMU $F ISOR DELU 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 0.078100 1.571300 FVAR 0.17966 0.56621 N1 3 1.049254 0.851248 0.424725 11.00000 0.03243 0.02587 = 0.04919 -0.00339 0.02337 0.00188 AFIX 3 H1N 2 1.011394 0.942328 0.411745 11.00000 0.03047 AFIX 0 C1 1 1.122656 0.814607 0.513489 11.00000 0.03140 0.02784 = 0.04944 0.00457 0.02211 -0.00112 C2 1 1.174942 0.702312 0.500403 11.00000 0.03694 0.03740 = 0.05671 0.00707 0.02405 0.00902 AFIX 43 H2 2 1.228004 0.652428 0.549676 11.00000 -1.20000 AFIX 0 C3 1 1.135252 0.675685 0.401126 11.00000 0.04538 0.03147 = 0.07123 0.00030 0.03610 0.00530 AFIX 43 H3 2 1.158021 0.605759 0.371275 11.00000 -1.20000 AFIX 0 C4 1 1.056888 0.768812 0.353553 11.00000 0.03755 0.02653 = 0.05370 -0.00337 0.02824 -0.00209 C5 1 0.992008 0.785497 0.254101 11.00000 0.03977 0.03653 = 0.05958 -0.01335 0.03345 -0.00727 C6 1 1.031702 0.737825 0.186343 11.00000 0.04310 0.05776 = 0.05705 -0.01353 0.02955 0.00167 C7 1 1.103474 0.815180 0.177091 11.00000 0.05104 0.06316 = 0.06588 -0.02382 0.03948 -0.01124 F1 4 1.136815 0.931859 0.229121 11.00000 0.11292 0.09105 = 0.14895 -0.07008 0.10952 -0.06131 C8 1 1.143936 0.778590 0.116829 11.00000 0.06128 0.10619 = 0.09283 -0.03864 0.05590 -0.01938 F2 4 1.214311 0.852651 0.112724 11.00000 0.13357 0.13664 = 0.17383 -0.05275 0.13455 -0.04391 C9 1 1.114127 0.647425 0.066986 11.00000 0.07322 0.12422 = 0.07401 -0.03978 0.04420 0.00093 F3 4 1.153220 0.610802 0.008784 11.00000 0.11972 0.20346 = 0.13380 -0.09297 0.09052 -0.01787 C10 1 1.047802 0.565927 0.078641 11.00000 0.08759 0.09339 = 0.08135 -0.04784 0.03896 -0.00079 F4 4 1.021030 0.438860 0.031940 11.00000 0.17866 0.14466 = 0.19726 -0.11803 0.12657 -0.04744 C11 1 1.005054 0.607218 0.137392 11.00000 0.07072 0.08406 = 0.09437 -0.04467 0.04560 -0.01837 F5 4 0.938390 0.524275 0.144912 11.00000 0.17628 0.08952 = 0.24159 -0.09198 0.15746 -0.06417 C12 1 0.897941 0.837360 0.216988 11.00000 0.03683 0.03702 = 0.04649 -0.01330 0.02388 -0.00680 N2 3 0.845160 0.865163 0.268971 11.00000 0.03208 0.03266 = 0.04010 0.00002 0.01972 0.00162 AFIX 3 H2N 2 0.862190 0.821533 0.332661 11.00000 0.03326 AFIX 0 C13 1 0.833985 0.872908 0.119929 11.00000 0.03868 0.06426 = 0.04481 -0.01037 0.02309 -0.01321 AFIX 43 H13 2 0.849944 0.867560 0.067436 11.00000 -1.20000 AFIX 0 C14 1 0.746914 0.915519 0.113790 11.00000 0.03948 0.05544 = 0.03497 -0.00464 0.01707 -0.00593 AFIX 43 H14 2 0.692369 0.947162 0.056874 11.00000 -1.20000 AFIX 0 C15 1 0.750619 0.904994 0.207449 11.00000 0.03327 0.03732 = 0.04308 -0.00171 0.01807 -0.00136 C16 1 0.675408 0.918814 0.233245 11.00000 0.03478 0.03700 = 0.03880 -0.00099 0.01881 -0.00027 C17 1 0.574821 0.942962 0.154225 11.00000 0.03399 0.05419 = 0.04051 0.00120 0.02140 0.00507 C18 1 0.533290 1.076887 0.129035 11.00000 0.03570 0.06661 = 0.04533 0.00072 0.01481 0.00777 F6 4 0.583061 1.193355 0.173601 11.00000 0.05199 0.05136 = 0.07090 -0.00059 0.01083 0.01721 C19 1 0.437410 1.095736 0.057884 11.00000 0.04057 0.09211 = 0.04618 0.00841 0.01508 0.02245 F7 4 0.399491 1.228385 0.037867 11.00000 0.05885 0.10966 = 0.07209 0.01635 0.01328 0.04474 C20 1 0.383105 0.977958 0.011460 11.00000 0.03273 0.11448 = 0.03510 0.00502 0.00860 0.00687 F8 4 0.291198 0.996298 -0.056434 11.00000 0.03740 0.17122 = 0.04597 0.00368 0.00219 0.00572 C21 1 0.420989 0.843747 0.034227 11.00000 0.04657 0.09307 = 0.04503 -0.01396 0.01878 -0.01645 F9 4 0.367889 0.727551 -0.009023 11.00000 0.06046 0.12984 = 0.06589 -0.02058 0.01240 -0.03740 C22 1 0.516709 0.825810 0.105936 11.00000 0.04011 0.06748 = 0.04203 -0.00249 0.01805 -0.00354 F10 4 0.552848 0.692873 0.127890 11.00000 0.06494 0.05369 = 0.06464 -0.00145 0.01973 -0.01384 C23 1 0.684361 0.891692 0.327496 11.00000 0.03612 0.02693 = 0.04563 0.00158 0.02290 0.00413 N3 3 0.766561 0.856323 0.405068 11.00000 0.03005 0.02583 = 0.04033 0.00400 0.01969 0.00174 C24 1 0.599684 0.886702 0.347555 11.00000 0.02781 0.05087 = 0.04512 0.00553 0.01822 0.00935 AFIX 43 H24 2 0.534109 0.911002 0.304550 11.00000 -1.20000 AFIX 0 C25 1 0.632870 0.841187 0.438364 11.00000 0.02917 0.04295 = 0.05071 0.00319 0.02424 0.00281 AFIX 43 H25 2 0.594961 0.824780 0.472035 11.00000 -1.20000 AFIX 0 C26 1 0.737926 0.821414 0.476107 11.00000 0.03153 0.02773 = 0.04149 0.00090 0.02120 -0.00031 C27 1 0.798683 0.768822 0.566686 11.00000 0.03276 0.02665 = 0.04512 0.00115 0.02304 0.00059 C28 1 0.753547 0.711130 0.627645 11.00000 0.02999 0.03650 = 0.04618 0.00893 0.01941 0.00359 C29 1 0.694620 0.589624 0.599341 11.00000 0.03225 0.05122 = 0.05042 0.00898 0.02036 -0.00752 F11 4 0.679336 0.519602 0.518825 11.00000 0.05648 0.05301 = 0.05885 -0.00651 0.02832 -0.02121 C30 1 0.653657 0.533695 0.655552 11.00000 0.03680 0.05877 = 0.06846 0.01425 0.02408 -0.01474 F12 4 0.598356 0.415271 0.627765 11.00000 0.06413 0.08148 = 0.09128 0.00767 0.04021 -0.03491 C31 1 0.671148 0.598578 0.740503 11.00000 0.04027 0.08020 = 0.05715 0.01937 0.02885 -0.00815 F13 4 0.631321 0.545471 0.795525 11.00000 0.06062 0.12244 = 0.07586 0.02258 0.04457 -0.01959 C32 1 0.730541 0.718480 0.771752 11.00000 0.04603 0.07542 = 0.04688 0.00999 0.02809 0.00492 F14 4 0.748415 0.779460 0.854617 11.00000 0.07916 0.10003 = 0.05500 -0.00377 0.04391 -0.00636 C33 1 0.770017 0.773141 0.714075 11.00000 0.03707 0.05008 = 0.04769 -0.00006 0.02376 -0.00337 F15 4 0.825333 0.891856 0.744214 11.00000 0.06670 0.05272 = 0.06023 -0.00996 0.03852 -0.01024 C34 1 0.902540 0.760928 0.608514 11.00000 0.03152 0.02746 = 0.04020 0.00039 0.01951 -0.00019 N4 3 0.956805 0.833350 0.571579 11.00000 0.03216 0.02692 = 0.04267 0.00753 0.01879 0.00215 AFIX 3 H4N 2 0.929595 0.879440 0.517619 11.00000 0.02528 AFIX 0 C35 1 0.968921 0.686489 0.689007 11.00000 0.03740 0.03540 = 0.04474 0.00617 0.02021 0.00038 AFIX 43 H35 2 0.953403 0.625161 0.729204 11.00000 -1.20000 AFIX 0 C36 1 1.062849 0.718544 0.699925 11.00000 0.03360 0.03340 = 0.04697 0.00874 0.01604 0.00109 AFIX 43 H36 2 1.122558 0.683397 0.749441 11.00000 -1.20000 AFIX 0 C37 1 1.053650 0.809826 0.626452 11.00000 0.02980 0.02462 = 0.04253 -0.00096 0.01882 -0.00135 C38 1 1.130060 0.882668 0.604276 11.00000 0.03320 0.03392 = 0.04984 0.00419 0.02327 -0.00047 C39 1 1.231686 0.856962 0.687033 11.00000 0.03500 0.05883 = 0.05506 0.00249 0.02186 -0.00748 AFIX 137 H39A 2 1.244408 0.753370 0.695612 11.00000 -1.50000 H39B 2 1.234864 0.898173 0.746521 11.00000 -1.50000 H39C 2 1.280979 0.902852 0.672054 11.00000 -1.50000 AFIX 0 C40 1 1.111052 1.043689 0.592444 11.00000 0.04768 0.02936 = 0.05832 -0.00626 0.03149 -0.01031 AFIX 137 H40A 2 1.048177 1.061631 0.536345 11.00000 -1.50000 H40B 2 1.163448 1.090788 0.582954 11.00000 -1.50000 H40C 2 1.109281 1.082415 0.650408 11.00000 -1.50000 AFIX 0 PART 1 C41 1 0.534886 0.054086 0.689460 21.00000 0.07111 0.08083 = 0.08362 0.02197 0.04140 0.02785 AFIX 13 H41 2 0.477138 0.119941 0.666660 21.00000 -1.20000 AFIX 0 CL1 5 0.574707 0.050418 0.600656 21.00000 0.05553 0.07161 = 0.06978 -0.01359 0.03476 0.00504 CL2 5 0.622250 0.122063 0.796121 21.00000 0.09124 0.12200 = 0.07578 -0.01252 0.03825 0.02051 CL3 5 0.495628 -0.115481 0.705484 21.00000 0.05633 0.08460 = 0.21165 0.06659 0.06943 0.01443 PART 2 SAME C41 > CL3 C42 1 0.520519 0.009782 0.669469 -21.00000 0.07111 0.08083 = 0.08362 0.02197 0.04140 0.02785 AFIX 13 H42 2 0.461198 0.071938 0.649172 -21.00000 -1.20000 AFIX 0 CL4 5 0.583718 0.058608 0.604876 -21.00000 0.22419 0.10246 = 0.19603 0.03886 0.15278 0.03407 CL5 5 0.593904 0.033071 0.790702 -21.00000 0.16304 0.20117 = 0.09775 -0.00495 0.04122 0.09377 CL6 5 0.483770 -0.171573 0.645798 -21.00000 0.10396 0.10428 = 0.15457 0.05484 0.05905 0.05221 PART 0 HKLF 4 Covalent radii and connectivity table for UDEL1 in P2(1) C 0.770 H 0.320 N 0.700 F 0.640 CL 0.990 N1 - C1 C4 C1 - N1 C2 C38 C2 - C1 C3 C3 - C4 C2 C4 - N1 C3 C5 C5 - C12 C4 C6 C6 - C7 C11 C5 C7 - F1 C6 C8 F1 - C7 C8 - F2 C7 C9 F2 - C8 C9 - F3 C10 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 - N2 C16 C14 C16 - C15 C23 C17 C17 - C18 C22 C16 C18 - F6 C17 C19 F6 - C18 C19 - F7 C20 C18 F7 - C19 C20 - F8 C21 C19 F8 - C20 C21 - F9 C20 C22 F9 - C21 C22 - F10 C17 C21 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 - C34 C36 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 31066 Reflections read, of which 12 rejected -18 =< h =< 18, -9 =< k =< 10, -18 =< l =< 18, Max. 2-theta = 141.05 0 Systematic absence violations 0 Inconsistent equivalents 6920 Unique reflections, of which 0 suppressed R(int) = 0.0475 R(sigma) = 0.0434 Friedel opposites not merged Maximum memory for data reduction = 6195 / 68357 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 = 7717 / 825223 wR2 = 0.1519 before cycle 1 for 6920 data and 604 / 604 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint -0.0322 0.0100 DELU C41_a Cl3_a 0.0318 0.0100 DELU C42_b Cl4_b 0.0409 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 0.023 0.000 0.000 0.000 0.007 0.070 0.024 0.000 GooF = S = 1.028; Restrained GooF = 0.992 for 637 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0781 * P )^2 + 1.57 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17966 0.00038 -0.005 OSF 2 0.56658 0.01240 0.029 FVAR 2 Mean shift/esd = 0.006 Maximum = 0.123 for z Cl1_a Max. shift = 0.001 A for H42_b Max. dU = 0.000 for Cl5_b Least-squares cycle 2 Maximum vector length = 511 Memory required = 7717 / 825223 wR2 = 0.1519 before cycle 2 for 6920 data and 604 / 604 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint -0.0322 0.0100 DELU C41_a Cl3_a 0.0316 0.0100 DELU C42_b Cl4_b 0.0410 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 0.023 0.000 0.000 0.000 0.007 0.070 0.024 0.000 GooF = S = 1.028; Restrained GooF = 0.992 for 637 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0781 * P )^2 + 1.57 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17965 0.00038 -0.010 OSF 2 0.56678 0.01239 0.017 FVAR 2 Mean shift/esd = 0.004 Maximum = 0.055 for z Cl1_a Max. shift = 0.001 A for C42_b Max. dU = 0.000 for Cl5_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 7717 / 825223 wR2 = 0.1519 before cycle 3 for 6920 data and 604 / 604 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint -0.0321 0.0100 DELU C41_a Cl3_a 0.0314 0.0100 DELU C42_b Cl4_b 0.0409 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 0.022 0.000 0.000 0.000 0.007 0.070 0.024 0.000 GooF = S = 1.029; Restrained GooF = 0.992 for 637 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0781 * P )^2 + 1.57 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17965 0.00038 -0.004 OSF 2 0.56686 0.01239 0.006 FVAR 2 Mean shift/esd = 0.002 Maximum = 0.013 for z Cl1_a Max. shift = 0.000 A for H42_b Max. dU = 0.000 for F5 Least-squares cycle 4 Maximum vector length = 511 Memory required = 7717 / 825223 wR2 = 0.1519 before cycle 4 for 6920 data and 604 / 604 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint -0.0321 0.0100 DELU C41_a Cl3_a 0.0313 0.0100 DELU C42_b Cl4_b 0.0409 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 0.022 0.000 0.000 0.000 0.007 0.070 0.024 0.000 GooF = S = 1.029; Restrained GooF = 0.992 for 637 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0781 * P )^2 + 1.57 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17965 0.00038 -0.002 OSF 2 0.56686 0.01239 0.000 FVAR 2 Mean shift/esd = 0.001 Maximum = 0.007 for U23 F5 Max. shift = 0.000 A for H42_b Max. dU = 0.000 for Cl4_b Largest correlation matrix elements 0.866 U13 F2 / U33 F2 0.801 U13 F5 / U11 F5 0.758 U12 F5 / U23 F5 0.857 U13 F2 / U11 F2 0.798 z F2 / x F2 0.758 z Cl3_a / y Cl3_a 0.814 U13 F1 / U33 F1 0.798 U13 Cl4_b / U33 Cl4_b 0.752 U13 C41_a / U11 C41_a -0.812 y Cl5_b / FVAR 2 0.794 U12 F2 / U23 F2 -0.746 y Cl3_a / FVAR 2 0.811 U13 F1 / U11 F1 0.786 U13 F5 / U33 F5 0.742 y Cl6_b / z Cl3_a 0.811 U13 Cl4_b / U11 Cl4_b 0.786 U12 F1 / U23 F1 -0.739 y Cl4_b / y Cl1_a -0.807 z Cl3_a / FVAR 2 0.771 z Cl6_b / y Cl3_a 0.737 U13 F4 / U11 F4 -0.804 z Cl6_b / FVAR 2 0.760 z F1 / x F1 0.733 U13 F3 / U11 F3 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 1.2280 0.6524 0.5497 43 0.950 0.000 C2 C1 C3 H3 1.1580 0.6058 0.3713 43 0.950 0.000 C3 C4 C2 H13 0.8499 0.8676 0.0674 43 0.950 0.000 C13 C14 C12 H14 0.6924 0.9472 0.0569 43 0.950 0.000 C14 C13 C15 H24 0.5341 0.9110 0.3045 43 0.950 0.000 C24 C25 C23 H25 0.5950 0.8248 0.4720 43 0.950 0.000 C25 C24 C26 H35 0.9534 0.6252 0.7292 43 0.950 0.000 C35 C34 C36 H36 1.1226 0.6834 0.7494 43 0.950 0.000 C36 C37 C35 H39A 1.2444 0.7534 0.6956 137 0.980 0.000 C39 C38 H39A H39B 1.2349 0.8981 0.7465 137 0.980 0.000 C39 C38 H39A H39C 1.2810 0.9029 0.6721 137 0.980 0.000 C39 C38 H39A H40A 1.0482 1.0616 0.5363 137 0.980 0.000 C40 C38 H40A H40B 1.1634 1.0908 0.5829 137 0.980 0.000 C40 C38 H40A H40C 1.1093 1.0824 0.6504 137 0.980 0.000 C40 C38 H40A H41 0.4770 0.1200 0.6666 13 1.000 0.000 C41_a Cl2_a Cl1_a Cl3_a H42 0.4613 0.0718 0.6492 13 1.000 0.000 C42_b Cl5_b Cl4_b Cl6_b UDEL1 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq N1 1.04926 0.85125 0.42473 1.00000 0.03243 0.02588 0.04920 -0.00340 0.02338 0.00188 0.03393 0.00608 0.00019 0.00031 0.00021 0.00000 0.00137 0.00154 0.00155 0.00116 0.00125 0.00108 0.00061 H1N 1.01140 0.94233 0.41175 1.00000 0.03045 0.00000 0.00897 C1 1.12265 0.81461 0.51349 1.00000 0.03141 0.02783 0.04946 0.00456 0.02214 -0.00111 0.03473 0.00747 0.00024 0.00038 0.00025 0.00000 0.00161 0.00179 0.00183 0.00141 0.00144 0.00128 0.00071 C2 1.17494 0.70231 0.50040 1.00000 0.03693 0.03740 0.05669 0.00706 0.02405 0.00902 0.04252 0.00865 0.00026 0.00043 0.00029 0.00000 0.00181 0.00209 0.00213 0.00165 0.00165 0.00148 0.00082 H2 1.22800 0.65242 0.54968 1.00000 0.05102 0.00000 0.00000 C3 1.13525 0.67569 0.40112 1.00000 0.04538 0.03147 0.07124 0.00031 0.03611 0.00529 0.04563 0.00912 0.00028 0.00043 0.00032 0.00000 0.00199 0.00204 0.00254 0.00168 0.00194 0.00152 0.00089 H3 1.15802 0.60577 0.37127 1.00000 0.05475 0.00000 0.00000 C4 1.05689 0.76881 0.35355 1.00000 0.03754 0.02653 0.05371 -0.00338 0.02823 -0.00210 0.03634 0.00779 0.00025 0.00038 0.00027 0.00000 0.00172 0.00177 0.00193 0.00146 0.00154 0.00140 0.00072 C5 0.99201 0.78551 0.25411 1.00000 0.03977 0.03650 0.05958 -0.01331 0.03345 -0.00725 0.04110 0.00793 0.00026 0.00041 0.00029 0.00000 0.00178 0.00211 0.00216 0.00158 0.00167 0.00145 0.00082 C6 1.03170 0.73783 0.18634 1.00000 0.04310 0.05776 0.05705 -0.01352 0.02955 0.00167 0.04997 0.00908 0.00029 0.00050 0.00031 0.00000 0.00204 0.00263 0.00229 0.00187 0.00186 0.00171 0.00096 C7 1.10348 0.81519 0.17709 1.00000 0.05105 0.06313 0.06585 -0.02379 0.03946 -0.01124 0.05505 0.00925 0.00031 0.00053 0.00033 0.00000 0.00226 0.00279 0.00258 0.00215 0.00208 0.00195 0.00109 F1 1.13681 0.93186 0.22912 1.00000 0.11290 0.09104 0.14892 -0.07005 0.10949 -0.06129 0.09863 0.00724 0.00027 0.00039 0.00030 0.00000 0.00256 0.00243 0.00311 0.00225 0.00257 0.00204 0.00134 C8 1.14394 0.77861 0.11683 1.00000 0.06126 0.10617 0.09280 -0.03860 0.05589 -0.01936 0.07876 0.01173 0.00039 0.00075 0.00044 0.00000 0.00279 0.00438 0.00373 0.00330 0.00283 0.00283 0.00168 F2 1.21431 0.85265 0.11272 1.00000 0.13349 0.13663 0.17369 -0.05270 0.13445 -0.04386 0.12343 0.00953 0.00032 0.00052 0.00035 0.00000 0.00331 0.00357 0.00410 0.00310 0.00346 0.00282 0.00172 C9 1.11412 0.64742 0.06699 1.00000 0.07320 0.12416 0.07395 -0.03971 0.04415 0.00099 0.08625 0.01287 0.00043 0.00083 0.00043 0.00000 0.00335 0.00484 0.00348 0.00341 0.00292 0.00307 0.00177 F3 1.15322 0.61081 0.00879 1.00000 0.11968 0.20330 0.13372 -0.09288 0.09045 -0.01782 0.13964 0.00954 0.00034 0.00064 0.00034 0.00000 0.00299 0.00546 0.00337 0.00364 0.00280 0.00315 0.00211 C10 1.04780 0.56593 0.07864 1.00000 0.08757 0.09327 0.08130 -0.04773 0.03893 -0.00071 0.08695 0.01237 0.00046 0.00077 0.00044 0.00000 0.00390 0.00439 0.00362 0.00340 0.00301 0.00308 0.00177 F4 1.02104 0.43886 0.03195 1.00000 0.17860 0.14456 0.19711 -0.11788 0.12647 -0.04733 0.15761 0.01113 0.00045 0.00062 0.00045 0.00000 0.00480 0.00426 0.00526 0.00417 0.00438 0.00352 0.00244 C11 1.00506 0.60721 0.13740 1.00000 0.07072 0.08398 0.09432 -0.04458 0.04556 -0.01831 0.07978 0.01145 0.00042 0.00070 0.00046 0.00000 0.00315 0.00393 0.00391 0.00320 0.00293 0.00277 0.00166 F5 0.93840 0.52426 0.14493 1.00000 0.17612 0.08941 0.24123 -0.09176 0.15719 -0.06401 0.14511 0.01054 0.00039 0.00048 0.00044 0.00000 0.00452 0.00292 0.00576 0.00344 0.00459 0.00301 0.00221 C12 0.89794 0.83736 0.21699 1.00000 0.03683 0.03701 0.04651 -0.01331 0.02389 -0.00680 0.03816 0.00728 0.00025 0.00041 0.00026 0.00000 0.00168 0.00202 0.00186 0.00154 0.00148 0.00145 0.00076 N2 0.84516 0.86517 0.26897 1.00000 0.03208 0.03265 0.04010 0.00002 0.01972 0.00162 0.03361 0.00603 0.00019 0.00031 0.00021 0.00000 0.00135 0.00163 0.00144 0.00115 0.00119 0.00113 0.00060 H2N 0.86219 0.82154 0.33266 1.00000 0.03324 0.00000 0.00921 C13 0.83399 0.87292 0.11993 1.00000 0.03867 0.06427 0.04477 -0.01037 0.02307 -0.01320 0.04760 0.00807 0.00027 0.00050 0.00028 0.00000 0.00183 0.00271 0.00193 0.00179 0.00159 0.00178 0.00093 H13 0.84994 0.86757 0.06744 1.00000 0.05712 0.00000 0.00000 C14 0.74691 0.91552 0.11379 1.00000 0.03948 0.05545 0.03497 -0.00464 0.01708 -0.00592 0.04314 0.00808 0.00028 0.00047 0.00027 0.00000 0.00183 0.00245 0.00176 0.00156 0.00150 0.00161 0.00085 H14 0.69237 0.94717 0.05687 1.00000 0.05177 0.00000 0.00000 C15 0.75062 0.90500 0.20745 1.00000 0.03325 0.03733 0.04306 -0.00172 0.01805 -0.00136 0.03751 0.00759 0.00025 0.00040 0.00026 0.00000 0.00166 0.00205 0.00188 0.00147 0.00148 0.00141 0.00076 C16 0.67541 0.91882 0.23324 1.00000 0.03478 0.03700 0.03879 -0.00097 0.01880 -0.00026 0.03598 0.00762 0.00025 0.00040 0.00025 0.00000 0.00169 0.00199 0.00177 0.00137 0.00142 0.00137 0.00074 C17 0.57482 0.94297 0.15422 1.00000 0.03398 0.05419 0.04051 0.00120 0.02139 0.00506 0.04113 0.00856 0.00027 0.00045 0.00027 0.00000 0.00176 0.00223 0.00189 0.00159 0.00153 0.00157 0.00081 C18 0.53329 1.07689 0.12904 1.00000 0.03570 0.06662 0.04532 0.00072 0.01482 0.00776 0.05045 0.00917 0.00028 0.00053 0.00029 0.00000 0.00186 0.00271 0.00208 0.00187 0.00160 0.00178 0.00094 F6 0.58306 1.19336 0.17360 1.00000 0.05198 0.05135 0.07089 -0.00059 0.01082 0.01721 0.06429 0.00576 0.00019 0.00029 0.00020 0.00000 0.00137 0.00153 0.00162 0.00122 0.00122 0.00113 0.00070 C19 0.43741 1.09575 0.05788 1.00000 0.04057 0.09209 0.04617 0.00844 0.01507 0.02245 0.06122 0.01098 0.00031 0.00064 0.00031 0.00000 0.00207 0.00333 0.00228 0.00223 0.00180 0.00216 0.00114 F7 0.39949 1.22839 0.03787 1.00000 0.05884 0.10966 0.07208 0.01634 0.01328 0.04472 0.08616 0.00757 0.00022 0.00041 0.00022 0.00000 0.00162 0.00257 0.00184 0.00170 0.00141 0.00171 0.00099 C20 0.38311 0.97796 0.01146 1.00000 0.03273 0.11446 0.03510 0.00503 0.00859 0.00689 0.06321 0.01055 0.00031 0.00069 0.00031 0.00000 0.00203 0.00363 0.00206 0.00227 0.00168 0.00222 0.00119 F8 0.29120 0.99630 -0.05643 1.00000 0.03740 0.17116 0.04598 0.00368 0.00219 0.00570 0.09099 0.00653 0.00019 0.00047 0.00020 0.00000 0.00132 0.00372 0.00145 0.00179 0.00112 0.00171 0.00117 C21 0.42099 0.84375 0.03423 1.00000 0.04656 0.09307 0.04505 -0.01395 0.01879 -0.01645 0.06219 0.00934 0.00033 0.00067 0.00031 0.00000 0.00219 0.00335 0.00217 0.00227 0.00182 0.00222 0.00113 F9 0.36789 0.72755 -0.00902 1.00000 0.06046 0.12982 0.06589 -0.02059 0.01241 -0.03739 0.09130 0.00607 0.00022 0.00045 0.00023 0.00000 0.00174 0.00307 0.00178 0.00184 0.00143 0.00188 0.00109 C22 0.51671 0.82581 0.10593 1.00000 0.04011 0.06746 0.04202 -0.00251 0.01805 -0.00354 0.04998 0.00875 0.00029 0.00055 0.00028 0.00000 0.00189 0.00265 0.00195 0.00187 0.00157 0.00181 0.00091 F10 0.55285 0.69288 0.12789 1.00000 0.06493 0.05368 0.06465 -0.00145 0.01973 -0.01385 0.06454 0.00561 0.00020 0.00030 0.00020 0.00000 0.00158 0.00160 0.00156 0.00120 0.00129 0.00123 0.00069 C23 0.68436 0.89170 0.32750 1.00000 0.03611 0.02694 0.04562 0.00158 0.02289 0.00413 0.03450 0.00761 0.00025 0.00037 0.00026 0.00000 0.00168 0.00176 0.00180 0.00139 0.00147 0.00133 0.00071 N3 0.76656 0.85633 0.40507 1.00000 0.03005 0.02583 0.04033 0.00399 0.01970 0.00174 0.03060 0.00584 0.00019 0.00029 0.00020 0.00000 0.00127 0.00148 0.00141 0.00108 0.00114 0.00105 0.00057 C24 0.59968 0.88670 0.34755 1.00000 0.02781 0.05088 0.04512 0.00554 0.01822 0.00935 0.04056 0.00823 0.00025 0.00044 0.00027 0.00000 0.00156 0.00229 0.00192 0.00162 0.00144 0.00150 0.00082 H24 0.53411 0.91100 0.30455 1.00000 0.04867 0.00000 0.00000 C25 0.63287 0.84119 0.43836 1.00000 0.02917 0.04294 0.05070 0.00319 0.02423 0.00280 0.03856 0.00793 0.00024 0.00042 0.00026 0.00000 0.00157 0.00211 0.00195 0.00162 0.00148 0.00145 0.00077 H25 0.59496 0.82479 0.47203 1.00000 0.04627 0.00000 0.00000 C26 0.73793 0.82142 0.47611 1.00000 0.03152 0.02772 0.04148 0.00090 0.02119 -0.00031 0.03176 0.00717 0.00023 0.00037 0.00024 0.00000 0.00155 0.00173 0.00165 0.00134 0.00133 0.00127 0.00066 C27 0.79868 0.76883 0.56669 1.00000 0.03276 0.02665 0.04512 0.00115 0.02304 0.00058 0.03274 0.00750 0.00024 0.00038 0.00025 0.00000 0.00155 0.00169 0.00177 0.00136 0.00141 0.00130 0.00068 C28 0.75355 0.71113 0.62765 1.00000 0.02999 0.03651 0.04618 0.00893 0.01941 0.00359 0.03667 0.00791 0.00024 0.00040 0.00026 0.00000 0.00162 0.00193 0.00185 0.00144 0.00147 0.00135 0.00073 C29 0.69462 0.58962 0.59934 1.00000 0.03225 0.05121 0.05040 0.00897 0.02036 -0.00752 0.04392 0.00831 0.00025 0.00047 0.00028 0.00000 0.00172 0.00231 0.00210 0.00172 0.00160 0.00157 0.00086 F11 0.67934 0.51961 0.51883 1.00000 0.05647 0.05303 0.05885 -0.00651 0.02831 -0.02121 0.05517 0.00494 0.00018 0.00028 0.00017 0.00000 0.00137 0.00147 0.00140 0.00109 0.00113 0.00111 0.00061 C30 0.65365 0.53370 0.65555 1.00000 0.03680 0.05875 0.06843 0.01426 0.02405 -0.01473 0.05447 0.00954 0.00029 0.00052 0.00034 0.00000 0.00195 0.00270 0.00254 0.00202 0.00188 0.00180 0.00103 F12 0.59836 0.41528 0.62777 1.00000 0.06412 0.08148 0.09130 0.00767 0.04021 -0.03490 0.07693 0.00634 0.00021 0.00035 0.00023 0.00000 0.00168 0.00212 0.00205 0.00159 0.00158 0.00151 0.00089 C31 0.67115 0.59859 0.74051 1.00000 0.04027 0.08018 0.05715 0.01938 0.02885 -0.00814 0.05657 0.01020 0.00029 0.00059 0.00032 0.00000 0.00201 0.00310 0.00241 0.00206 0.00187 0.00199 0.00108 F13 0.63132 0.54548 0.79552 1.00000 0.06064 0.12244 0.07587 0.02259 0.04459 -0.01956 0.08108 0.00702 0.00020 0.00042 0.00022 0.00000 0.00165 0.00271 0.00180 0.00175 0.00147 0.00169 0.00095 C32 0.73054 0.71849 0.77175 1.00000 0.04604 0.07541 0.04688 0.01000 0.02810 0.00492 0.05338 0.00998 0.00031 0.00055 0.00030 0.00000 0.00211 0.00303 0.00215 0.00192 0.00179 0.00193 0.00101 F14 0.74841 0.77946 0.85462 1.00000 0.07915 0.10004 0.05500 -0.00376 0.04391 -0.00636 0.07288 0.00647 0.00022 0.00038 0.00019 0.00000 0.00179 0.00230 0.00148 0.00142 0.00141 0.00163 0.00080 C33 0.77002 0.77315 0.71407 1.00000 0.03707 0.05006 0.04768 -0.00007 0.02376 -0.00337 0.04315 0.00840 0.00027 0.00047 0.00028 0.00000 0.00179 0.00229 0.00198 0.00164 0.00161 0.00162 0.00083 F15 0.82533 0.89186 0.74421 1.00000 0.06671 0.05270 0.06023 -0.00996 0.03853 -0.01024 0.05610 0.00531 0.00019 0.00029 0.00018 0.00000 0.00149 0.00147 0.00142 0.00111 0.00124 0.00115 0.00060 C34 0.90254 0.76093 0.60852 1.00000 0.03153 0.02745 0.04020 0.00039 0.01952 -0.00018 0.03177 0.00721 0.00023 0.00037 0.00024 0.00000 0.00151 0.00168 0.00172 0.00132 0.00135 0.00129 0.00066 N4 0.95681 0.83335 0.57158 1.00000 0.03215 0.02693 0.04265 0.00753 0.01877 0.00215 0.03315 0.00622 0.00020 0.00032 0.00021 0.00000 0.00134 0.00144 0.00149 0.00119 0.00119 0.00109 0.00058 H4N 0.92960 0.87944 0.51762 1.00000 0.02531 0.00000 0.00857 C35 0.96892 0.68649 0.68901 1.00000 0.03741 0.03538 0.04476 0.00619 0.02022 0.00038 0.03850 0.00784 0.00025 0.00040 0.00026 0.00000 0.00176 0.00205 0.00193 0.00148 0.00155 0.00145 0.00077 H35 0.95340 0.62517 0.72920 1.00000 0.04620 0.00000 0.00000 C36 1.06285 0.71855 0.69993 1.00000 0.03358 0.03341 0.04696 0.00874 0.01603 0.00109 0.03872 0.00794 0.00026 0.00040 0.00027 0.00000 0.00168 0.00196 0.00193 0.00146 0.00148 0.00138 0.00077 H36 1.12256 0.68340 0.74944 1.00000 0.04647 0.00000 0.00000 C37 1.05365 0.80983 0.62645 1.00000 0.02981 0.02460 0.04255 -0.00096 0.01884 -0.00134 0.03133 0.00697 0.00023 0.00035 0.00024 0.00000 0.00151 0.00169 0.00175 0.00128 0.00137 0.00120 0.00068 C38 1.13006 0.88267 0.60428 1.00000 0.03319 0.03392 0.04984 0.00419 0.02327 -0.00046 0.03723 0.00797 0.00025 0.00040 0.00027 0.00000 0.00162 0.00193 0.00193 0.00147 0.00151 0.00141 0.00075 C39 1.23169 0.85697 0.68703 1.00000 0.03500 0.05884 0.05508 0.00249 0.02188 -0.00749 0.04899 0.00858 0.00027 0.00050 0.00029 0.00000 0.00175 0.00269 0.00218 0.00189 0.00165 0.00172 0.00095 H39A 1.24442 0.75338 0.69559 1.00000 0.07349 0.00000 0.00000 H39B 1.23485 0.89814 0.74653 1.00000 0.07349 0.00000 0.00000 H39C 1.28098 0.90290 0.67207 1.00000 0.07349 0.00000 0.00000 C40 1.11105 1.04369 0.59244 1.00000 0.04766 0.02935 0.05832 -0.00626 0.03148 -0.01030 0.04221 0.00813 0.00028 0.00040 0.00029 0.00000 0.00203 0.00192 0.00224 0.00160 0.00179 0.00152 0.00083 H40A 1.04817 1.06163 0.53635 1.00000 0.06332 0.00000 0.00000 H40B 1.16344 1.09079 0.58294 1.00000 0.06332 0.00000 0.00000 H40C 1.10929 1.08242 0.65041 1.00000 0.06332 0.00000 0.00000 C41_a 0.53479 0.05413 0.68944 0.56686 0.07140 0.08052 0.08369 0.02192 0.04165 0.02812 0.07594 0.02341 0.00101 0.00127 0.00074 0.01239 0.00473 0.00644 0.00453 0.00421 0.00392 0.00424 0.00224 H41_a 0.47704 0.11999 0.66663 0.56686 0.09113 0.01239 0.00000 Cl1_a 0.57471 0.05038 0.60070 0.56686 0.05556 0.07171 0.06985 -0.01361 0.03475 0.00509 0.06321 0.00716 0.00025 0.00052 0.00025 0.01239 0.00164 0.00258 0.00193 0.00175 0.00139 0.00137 0.00118 Cl2_a 0.62224 0.12204 0.79609 0.56686 0.09128 0.12209 0.07581 -0.01235 0.03829 0.02059 0.09605 0.01046 0.00033 0.00068 0.00029 0.01239 0.00221 0.00393 0.00183 0.00200 0.00156 0.00223 0.00158 Cl3_a 0.49562 -0.11550 0.70546 0.56686 0.05635 0.08467 0.21181 0.06670 0.06944 0.01445 0.11408 0.01777 0.00025 0.00061 0.00068 0.01239 0.00154 0.00289 0.00616 0.00350 0.00252 0.00159 0.00263 C42_b 0.52064 0.00968 0.66948 0.43314 0.07140 0.08052 0.08369 0.02192 0.04165 0.02812 0.07594 0.03066 0.00137 0.00171 0.00094 0.01239 0.00473 0.00644 0.00453 0.00421 0.00392 0.00424 0.00224 H42_b 0.46132 0.07183 0.64919 0.43314 0.09113 0.01239 0.00000 Cl4_b 0.58371 0.05865 0.60475 0.43314 0.22446 0.10219 0.19628 0.03900 0.15323 0.03386 0.15227 0.02538 0.00086 0.00120 0.00078 0.01239 0.01104 0.00647 0.00863 0.00616 0.00860 0.00606 0.00463 Cl5_b 0.59388 0.03298 0.79076 0.43314 0.16300 0.20063 0.09787 -0.00462 0.04147 0.09351 0.16012 0.02963 0.00090 0.00169 0.00049 0.01239 0.00764 0.01081 0.00346 0.00473 0.00395 0.00744 0.00473 Cl6_b 0.48375 -0.17162 0.64575 0.43314 0.10394 0.10414 0.15437 0.05471 0.05897 0.05215 0.12037 0.02319 0.00045 0.00089 0.00080 0.01239 0.00345 0.00386 0.00624 0.00383 0.00352 0.00277 0.00237 Final Structure Factor Calculation for UDEL1 in P2(1) Total number of l.s. parameters = 604 Maximum vector length = 511 Memory required = 7115 / 26068 wR2 = 0.1519 before cycle 5 for 6920 data and 2 / 604 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint -0.0321 0.0100 DELU C41_a Cl3_a 0.0312 0.0100 DELU C42_b Cl4_b 0.0409 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 0.022 0.000 0.000 0.000 0.007 0.070 0.024 0.000 GooF = S = 1.028; Restrained GooF = 0.992 for 637 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0781 * P )^2 + 1.57 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0548 for 6145 Fo > 4sig(Fo) and 0.0616 for all 6920 data wR2 = 0.1519, GooF = S = 1.028, Restrained GooF = 0.992 for all data Flack x parameter = 0.0536 with esd 0.0233 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 0.0497 0.0301 0.0220 N1 0.0504 0.0303 0.0234 C1 0.0590 0.0410 0.0275 C2 0.0719 0.0383 0.0267 C3 0.0550 0.0279 0.0261 C4 0.0671 0.0310 0.0252 C5 0.0712 0.0496 0.0291 C6 0.0897 0.0454 0.0300 C7 0.2170 0.0443 0.0346 F1 may be split into 1.1494 0.9201 0.2373 and 1.1242 0.9436 0.2210 0.1401 0.0643 0.0318 C8 0.2354 0.1033 0.0316 F2 0.1479 0.0764 0.0344 C9 0.2677 0.1193 0.0319 F3 0.1401 0.0876 0.0332 C10 0.2970 0.1369 0.0389 F4 0.1341 0.0619 0.0434 C11 0.3030 0.0861 0.0462 F5 may be split into 0.9532 0.5141 0.1557 and 0.9236 0.5345 0.1341 0.0563 0.0310 0.0272 C12 0.0404 0.0332 0.0272 N2 0.0715 0.0403 0.0310 C13 0.0576 0.0380 0.0339 C14 0.0436 0.0371 0.0318 C15 0.0395 0.0367 0.0317 C16 0.0554 0.0411 0.0269 C17 0.0690 0.0485 0.0338 C18 0.0987 0.0599 0.0343 F6 0.1007 0.0512 0.0318 C19 0.1382 0.0894 0.0309 F7 0.1151 0.0459 0.0287 C20 0.1714 0.0720 0.0295 F8 0.0991 0.0488 0.0388 C21 0.1462 0.0896 0.0380 F9 0.0680 0.0423 0.0397 C22 0.0863 0.0631 0.0443 F10 0.0464 0.0325 0.0246 C23 0.0416 0.0257 0.0245 N3 0.0553 0.0434 0.0229 C24 0.0520 0.0418 0.0219 C25 0.0421 0.0280 0.0252 C26 0.0457 0.0266 0.0259 C27 0.0516 0.0312 0.0272 C28 0.0637 0.0442 0.0239 C29 0.0760 0.0570 0.0325 F11 0.0872 0.0549 0.0213 C30 0.1159 0.0898 0.0251 F12 0.0948 0.0523 0.0227 C31 0.1395 0.0785 0.0252 F13 0.0788 0.0487 0.0327 C32 0.1020 0.0793 0.0373 F14 0.0509 0.0480 0.0305 C33 0.0768 0.0475 0.0441 F15 0.0404 0.0279 0.0270 C34 0.0457 0.0300 0.0237 N4 0.0479 0.0367 0.0309 C35 0.0535 0.0335 0.0291 C36 0.0426 0.0272 0.0242 C37 0.0509 0.0341 0.0267 C38 0.0634 0.0539 0.0297 C39 0.0623 0.0401 0.0243 C40 0.1109 0.0696 0.0474 C41_a 0.0857 0.0643 0.0397 Cl1_a 0.1405 0.0843 0.0634 Cl2_a 0.2458 0.0573 0.0391 Cl3_a may be split into 0.5056 -0.1063 0.7193 and 0.4857 -0.1247 0.6917 0.1109 0.0696 0.0474 C42_b 0.2639 0.1069 0.0860 Cl4_b 0.2987 0.0978 0.0839 Cl5_b may be split into 0.6002 0.0507 0.7855 and 0.5876 0.0152 0.7960 0.1901 0.1215 0.0495 Cl6_b Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.025 0.033 0.041 0.051 0.063 0.079 0.104 0.153 1.000 Number in group 705. 692. 744. 661. 687. 667. 691. 692. 690. 691. GooF 1.039 1.036 0.996 1.036 1.051 0.979 1.004 1.000 1.119 1.020 K 1.436 1.064 1.020 1.050 1.041 1.026 1.021 1.012 0.997 1.005 Resolution(A) 0.82 0.87 0.90 0.94 0.99 1.06 1.14 1.26 1.44 1.80 inf Number in group 730. 659. 709. 685. 678. 699. 683. 689. 690. 698. GooF 0.881 0.930 0.907 0.918 0.889 0.956 0.984 1.019 1.157 1.489 K 1.009 1.047 1.032 1.037 1.005 1.012 0.992 0.982 0.992 1.014 R1 0.161 0.126 0.099 0.082 0.064 0.055 0.051 0.052 0.047 0.043 Recommended weighting scheme: WGHT 0.0806 1.5202 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 5 -3 4 87.66 15.19 7.50 0.023 1.55 3 -2 4 71.45 12.08 6.78 0.020 2.07 6 -2 4 25.68 0.60 5.36 0.005 1.52 2 0 3 309.47 170.97 4.87 0.077 3.22 3 2 4 79.20 26.75 4.86 0.030 2.07 2 -3 1 683.72 394.83 4.85 0.117 2.67 3 -4 2 105.01 43.99 4.83 0.039 1.88 2 3 1 612.12 392.32 4.56 0.117 2.67 0 0 6 78.91 18.20 4.31 0.025 2.31 2 -3 5 95.92 43.82 4.24 0.039 1.82 2 -5 0 61.45 21.94 4.15 0.028 1.79 4 0 1 228.82 137.34 4.12 0.069 3.02 4 -3 3 943.46 650.18 4.11 0.150 1.85 1 -6 4 32.52 7.01 4.11 0.016 1.38 2 -3 7 16.34 1.03 4.07 0.006 1.50 0 -2 3 213.09 350.27 3.99 0.110 3.28 -2 -1 7 116.78 62.41 3.82 0.047 2.12 1 0 3 384.35 572.49 3.77 0.141 3.88 -11 3 7 31.64 1.96 3.74 0.008 1.25 -6 0 7 684.02 476.62 3.69 0.129 2.00 -1 -6 5 17.02 0.66 3.68 0.005 1.38 -5 -3 4 122.84 63.42 3.68 0.047 2.10 7 0 4 226.97 140.51 3.68 0.070 1.45 8 0 6 16.77 0.06 3.62 0.001 1.15 6 2 4 27.84 2.92 3.61 0.010 1.52 -1 0 6 123.22 68.47 3.61 0.049 2.47 -2 1 7 76.87 36.87 3.61 0.036 2.12 2 0 9 15.64 0.65 3.56 0.005 1.38 -6 -8 7 22.55 2.65 3.55 0.010 1.01 4 -3 4 23.71 5.57 3.53 0.014 1.69 6 0 3 58.08 20.81 3.51 0.027 1.76 3 -2 3 388.86 268.15 3.50 0.096 2.33 4 3 3 928.86 665.25 3.50 0.152 1.85 2 0 12 81.77 41.83 3.45 0.038 1.06 -4 2 1 142.96 87.86 3.45 0.055 2.91 -5 0 6 525.52 360.38 3.44 0.112 2.36 -9 -2 18 18.90 56.37 3.44 0.044 0.85 -6 1 3 124.97 74.47 3.41 0.051 2.45 -8 -1 3 269.60 181.33 3.37 0.079 1.86 7 1 5 150.69 73.17 3.37 0.050 1.33 0 -1 16 37.08 12.42 3.36 0.021 0.86 4 1 4 1637.47 1218.54 3.36 0.206 1.98 1 -3 2 917.48 1258.90 3.35 0.209 2.68 7 5 3 73.54 36.91 3.32 0.036 1.20 -1 7 4 209.88 135.58 3.31 0.069 1.25 -1 -3 1 113.71 191.56 3.29 0.081 3.02 -7 -2 5 554.48 767.48 3.29 0.163 1.91 -7 -5 1 70.88 37.70 3.23 0.036 1.38 -13 0 6 45.41 16.47 3.22 0.024 1.18 1 0 8 167.49 73.59 3.20 0.051 1.63 Bond lengths and angles N1 - Distance Angles C1 1.3741 (0.0046) C4 1.3910 (0.0045) 109.73 (0.29) H1N 0.9943 123.68 123.82 N1 - C1 C4 C1 - Distance Angles N1 1.3741 (0.0046) C2 1.3841 (0.0050) 107.85 (0.32) C38 1.5012 (0.0051) 121.36 (0.30) 130.50 (0.33) C1 - N1 C2 C2 - Distance Angles C1 1.3841 (0.0050) C3 1.4017 (0.0059) 107.44 (0.33) H2 0.9500 126.28 126.28 C2 - C1 C3 C3 - Distance Angles C4 1.3922 (0.0054) C2 1.4017 (0.0059) 108.62 (0.33) H3 0.9500 125.69 125.69 C3 - C4 C2 C4 - Distance Angles N1 1.3910 (0.0045) C3 1.3922 (0.0054) 106.26 (0.34) C5 1.4206 (0.0055) 122.40 (0.31) 131.34 (0.35) C4 - N1 C3 C5 - Distance Angles C12 1.3751 (0.0052) C4 1.4206 (0.0055) 125.74 (0.32) C6 1.4965 (0.0049) 119.10 (0.35) 115.13 (0.32) C5 - C12 C4 C6 - Distance Angles C7 1.3721 (0.0060) C11 1.3931 (0.0069) 116.91 (0.40) C5 1.4965 (0.0049) 120.82 (0.38) 121.97 (0.42) C6 - C7 C11 C7 - Distance Angles F1 1.3115 (0.0053) C6 1.3721 (0.0060) 118.57 (0.36) C8 1.3745 (0.0060) 117.00 (0.41) 124.43 (0.44) C7 - F1 C6 F1 - Distance Angles C7 1.3115 (0.0053) F1 - C8 - Distance Angles F2 1.3025 (0.0063) C7 1.3745 (0.0060) 122.35 (0.49) C9 1.4065 (0.0087) 120.22 (0.45) 117.05 (0.50) C8 - F2 C7 F2 - Distance Angles C8 1.3025 (0.0063) F2 - C9 - Distance Angles F3 1.3306 (0.0059) C10 1.3411 (0.0097) 122.88 (0.59) C8 1.4065 (0.0087) 117.47 (0.60) 119.65 (0.45) C9 - F3 C10 F3 - Distance Angles C9 1.3306 (0.0059) F3 - C10 - Distance Angles C9 1.3411 (0.0097) F4 1.3503 (0.0073) 119.22 (0.53) C11 1.3919 (0.0078) 122.47 (0.55) 118.31 (0.65) C10 - C9 F4 F4 - Distance Angles C10 1.3503 (0.0073) F4 - C11 - Distance Angles F5 1.3242 (0.0072) C10 1.3919 (0.0078) 120.14 (0.51) C6 1.3931 (0.0069) 120.58 (0.46) 119.27 (0.55) C11 - F5 C10 F5 - Distance Angles C11 1.3242 (0.0072) F5 - C12 - Distance Angles C5 1.3751 (0.0052) N2 1.3963 (0.0043) 126.11 (0.34) C13 1.4193 (0.0056) 128.38 (0.33) 105.52 (0.30) C12 - C5 N2 N2 - Distance Angles C15 1.3792 (0.0045) C12 1.3963 (0.0043) 110.33 (0.29) H2N 0.9890 121.83 122.60 N2 - C15 C12 C13 - Distance Angles C14 1.3506 (0.0055) C12 1.4193 (0.0056) 109.43 (0.33) H13 0.9500 125.29 125.29 C13 - C14 C12 C14 - Distance Angles C13 1.3506 (0.0055) C15 1.4316 (0.0051) 108.54 (0.34) H14 0.9500 125.73 125.73 C14 - C13 C15 C15 - Distance Angles N2 1.3792 (0.0045) C16 1.3819 (0.0049) 125.07 (0.33) C14 1.4316 (0.0051) 105.90 (0.30) 128.83 (0.33) C15 - N2 C16 C16 - Distance Angles C15 1.3819 (0.0049) C23 1.4284 (0.0050) 124.65 (0.32) C17 1.4935 (0.0052) 117.44 (0.32) 117.29 (0.30) C16 - C15 C23 C17 - Distance Angles C18 1.3729 (0.0062) C22 1.3935 (0.0060) 116.99 (0.36) C16 1.4935 (0.0052) 123.04 (0.37) 119.88 (0.36) C17 - C18 C22 C18 - Distance Angles F6 1.3263 (0.0055) C17 1.3729 (0.0062) 120.54 (0.34) C19 1.3963 (0.0057) 117.64 (0.43) 121.81 (0.45) C18 - F6 C17 F6 - Distance Angles C18 1.3263 (0.0055) F6 - C19 - Distance Angles F7 1.3390 (0.0062) C20 1.3684 (0.0079) 121.17 (0.39) C18 1.3963 (0.0057) 119.43 (0.49) 119.38 (0.47) C19 - F7 C20 F7 - Distance Angles C19 1.3390 (0.0062) F7 - C20 - Distance Angles F8 1.3372 (0.0049) C21 1.3545 (0.0080) 119.93 (0.51) C19 1.3684 (0.0079) 119.25 (0.51) 120.82 (0.39) C20 - F8 C21 F8 - Distance Angles C20 1.3372 (0.0049) F8 - C21 - Distance Angles F9 1.3376 (0.0062) C20 1.3545 (0.0080) 121.39 (0.43) C22 1.3963 (0.0062) 119.18 (0.53) 119.42 (0.46) C21 - F9 C20 F9 - Distance Angles C21 1.3376 (0.0062) F9 - C22 - Distance Angles F10 1.3346 (0.0057) C17 1.3935 (0.0061) 119.70 (0.35) C21 1.3963 (0.0062) 118.72 (0.43) 121.57 (0.47) C22 - F10 C17 F10 - Distance Angles C22 1.3346 (0.0057) F10 - C23 - Distance Angles N3 1.3349 (0.0045) C16 1.4284 (0.0050) 125.91 (0.30) C24 1.4610 (0.0047) 111.51 (0.30) 122.35 (0.31) C23 - N3 C16 N3 - Distance Angles C23 1.3349 (0.0045) C26 1.3936 (0.0042) 105.55 (0.26) N3 - C23 C24 - Distance Angles C25 1.3345 (0.0052) C23 1.4610 (0.0047) 106.27 (0.30) H24 0.9500 126.87 126.87 C24 - C25 C23 C25 - Distance Angles C24 1.3345 (0.0052) C26 1.4540 (0.0046) 107.15 (0.29) H25 0.9500 126.42 126.42 C25 - C24 C26 C26 - Distance Angles C27 1.3813 (0.0049) N3 1.3936 (0.0042) 125.48 (0.29) C25 1.4540 (0.0046) 124.97 (0.30) 109.46 (0.28) C26 - C27 N3 C27 - Distance Angles C26 1.3813 (0.0049) C34 1.4230 (0.0045) 125.97 (0.30) C28 1.4971 (0.0045) 118.63 (0.29) 115.40 (0.30) C27 - C26 C34 C28 - Distance Angles C33 1.3751 (0.0055) C29 1.3882 (0.0054) 117.36 (0.33) C27 1.4971 (0.0046) 122.02 (0.34) 120.60 (0.34) C28 - C33 C29 C29 - Distance Angles F11 1.3330 (0.0049) C30 1.3824 (0.0056) 117.91 (0.37) C28 1.3882 (0.0054) 120.72 (0.32) 121.31 (0.40) C29 - F11 C30 F11 - Distance Angles C29 1.3330 (0.0049) F11 - C30 - Distance Angles F12 1.3368 (0.0052) C31 1.3625 (0.0072) 119.92 (0.37) C29 1.3824 (0.0056) 120.40 (0.44) 119.67 (0.40) C30 - F12 C31 F12 - Distance Angles C30 1.3368 (0.0052) F12 - C31 - Distance Angles F13 1.3444 (0.0045) C30 1.3625 (0.0071) 120.16 (0.43) C32 1.3815 (0.0069) 119.14 (0.44) 120.70 (0.36) C31 - F13 C30 F13 - Distance Angles C31 1.3444 (0.0045) F13 - C32 - Distance Angles F14 1.3167 (0.0052) C33 1.3805 (0.0054) 120.93 (0.43) C31 1.3815 (0.0069) 120.45 (0.37) 118.62 (0.40) C32 - F14 C33 F14 - Distance Angles C32 1.3167 (0.0052) F14 - C33 - Distance Angles F15 1.3411 (0.0048) C28 1.3751 (0.0055) 119.80 (0.32) C32 1.3805 (0.0054) 117.86 (0.37) 122.33 (0.39) C33 - F15 C28 F15 - Distance Angles C33 1.3411 (0.0049) F15 - C34 - Distance Angles N4 1.3766 (0.0043) C35 1.3907 (0.0050) 106.48 (0.28) C27 1.4230 (0.0045) 122.82 (0.31) 130.70 (0.31) C34 - N4 C35 N4 - Distance Angles C37 1.3551 (0.0043) C34 1.3766 (0.0043) 110.61 (0.28) H4N 0.8635 127.30 121.84 N4 - C37 C34 C35 - Distance Angles C34 1.3907 (0.0050) C36 1.4005 (0.0050) 107.42 (0.31) H35 0.9500 126.29 126.29 C35 - C34 C36 C36 - Distance Angles C37 1.3768 (0.0049) C35 1.4005 (0.0050) 108.15 (0.31) H36 0.9500 125.92 125.92 C36 - C37 C35 C37 - Distance Angles N4 1.3551 (0.0043) C36 1.3768 (0.0049) 107.32 (0.29) C38 1.5168 (0.0046) 121.41 (0.30) 131.23 (0.31) C37 - N4 C36 C38 - Distance Angles C1 1.5012 (0.0051) C37 1.5168 (0.0046) 106.37 (0.29) C40 1.5207 (0.0055) 111.82 (0.31) 110.01 (0.28) C39 1.5277 (0.0052) 110.11 (0.30) 109.65 (0.29) 108.85 (0.33) C38 - C1 C37 C40 C39 - Distance Angles C38 1.5277 (0.0052) 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 1.5207 (0.0055) 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 1.7156 (0.0099) Cl1_a 1.7375 (0.0099) 111.89 (0.68) Cl3_a 1.7441 (0.0097) 111.38 (0.62) 111.05 (0.65) H41_a 1.0000 107.42 107.42 107.42 C41_a - Cl2_a Cl1_a Cl3_a Cl1_a - Distance Angles C41_a 1.7375 (0.0099) Cl1_a - Cl2_a - Distance Angles C41_a 1.7156 (0.0100) Cl2_a - Cl3_a - Distance Angles C41_a 1.7441 (0.0097) Cl3_a - C42_b - Distance Angles Cl5_b 1.7189 (0.0118) Cl4_b 1.7350 (0.0121) 109.98 (0.91) Cl6_b 1.7636 (0.0118) 109.86 (0.85) 109.80 (0.88) H42_b 1.0000 109.06 109.06 109.06 C42_b - Cl5_b Cl4_b Cl6_b Cl4_b - Distance Angles C42_b 1.7350 (0.0121) Cl4_b - Cl5_b - Distance Angles C42_b 1.7189 (0.0118) Cl5_b - Cl6_b - Distance Angles C42_b 1.7636 (0.0118) Cl6_b - Selected torsion angles -3.26 ( 0.37) C4 - N1 - C1 - C2 -177.61 ( 0.30) C4 - N1 - C1 - C38 3.01 ( 0.40) N1 - C1 - C2 - C3 176.66 ( 0.35) C38 - C1 - C2 - C3 -1.68 ( 0.44) C1 - C2 - C3 - C4 2.18 ( 0.37) C1 - N1 - C4 - C3 -178.50 ( 0.32) C1 - N1 - C4 - C5 -0.28 ( 0.41) C2 - C3 - C4 - N1 -179.51 ( 0.37) C2 - C3 - C4 - C5 -25.76 ( 0.57) N1 - C4 - C5 - C12 153.37 ( 0.41) C3 - C4 - C5 - C12 155.80 ( 0.34) N1 - C4 - C5 - C6 -25.07 ( 0.60) C3 - C4 - C5 - C6 110.15 ( 0.48) C12 - C5 - C6 - C7 -71.30 ( 0.56) C4 - C5 - C6 - C7 -76.27 ( 0.62) C12 - C5 - C6 - C11 102.28 ( 0.53) C4 - C5 - C6 - C11 -173.75 ( 0.54) C11 - C6 - C7 - F1 0.14 ( 0.73) C5 - C6 - C7 - F1 5.93 ( 0.82) C11 - C6 - C7 - C8 179.82 ( 0.52) C5 - C6 - C7 - C8 2.04 ( 0.96) F1 - C7 - C8 - F2 -177.64 ( 0.60) C6 - C7 - C8 - F2 174.90 ( 0.57) F1 - C7 - C8 - C9 -4.78 ( 0.93) C6 - C7 - C8 - C9 -6.70 ( 1.02) F2 - C8 - C9 - F3 -179.72 ( 0.60) C7 - C8 - C9 - F3 174.04 ( 0.70) F2 - C8 - C9 - C10 1.02 ( 1.02) C7 - C8 - C9 - C10 2.05 ( 1.15) F3 - C9 - C10 - F4 -178.73 ( 0.68) C8 - C9 - C10 - F4 -177.97 ( 0.66) F3 - C9 - C10 - C11 1.25 ( 1.13) C8 - C9 - C10 - C11 178.59 ( 0.71) C9 - C10 - C11 - F5 -1.43 ( 1.11) F4 - C10 - C11 - F5 -0.05 ( 1.09) C9 - C10 - C11 - C6 179.92 ( 0.63) F4 - C10 - C11 - C6 178.02 ( 0.61) C7 - C6 - C11 - F5 4.20 ( 0.92) C5 - C6 - C11 - F5 -3.34 ( 0.87) C7 - C6 - C11 - C10 -177.16 ( 0.55) C5 - C6 - C11 - C10 -8.85 ( 0.61) C4 - C5 - C12 - N2 169.54 ( 0.36) C6 - C5 - C12 - N2 171.59 ( 0.39) C4 - C5 - C12 - C13 -10.03 ( 0.63) C6 - C5 - C12 - C13 -175.09 ( 0.36) C5 - C12 - N2 - C15 4.55 ( 0.41) C13 - C12 - N2 - C15 177.94 ( 0.40) C5 - C12 - C13 - C14 -1.70 ( 0.46) N2 - C12 - C13 - C14 -1.64 ( 0.49) C12 - C13 - C14 - C15 169.70 ( 0.35) C12 - N2 - C15 - C16 -5.52 ( 0.40) C12 - N2 - C15 - C14 4.37 ( 0.45) C13 - C14 - C15 - N2 -170.61 ( 0.40) C13 - C14 - C15 - C16 -0.96 ( 0.60) N2 - C15 - C16 - C23 173.13 ( 0.38) C14 - C15 - C16 - C23 -171.68 ( 0.35) N2 - C15 - C16 - C17 2.41 ( 0.61) C14 - C15 - C16 - C17 -96.90 ( 0.46) C15 - C16 - C17 - C18 91.68 ( 0.46) C23 - C16 - C17 - C18 86.64 ( 0.46) C15 - C16 - C17 - C22 -84.77 ( 0.44) C23 - C16 - C17 - C22 178.15 ( 0.37) C22 - C17 - C18 - F6 1.60 ( 0.59) C16 - C17 - C18 - F6 -0.40 ( 0.59) C22 - C17 - C18 - C19 -176.95 ( 0.37) C16 - C17 - C18 - C19 -0.40 ( 0.63) F6 - C18 - C19 - F7 178.19 ( 0.39) C17 - C18 - C19 - F7 -178.85 ( 0.40) F6 - C18 - C19 - C20 -0.26 ( 0.67) C17 - C18 - C19 - C20 1.36 ( 0.67) F7 - C19 - C20 - F8 179.79 ( 0.39) C18 - C19 - C20 - F8 -177.93 ( 0.44) F7 - C19 - C20 - C21 0.50 ( 0.69) C18 - C19 - C20 - C21 -0.89 ( 0.68) F8 - C20 - C21 - F9 178.40 ( 0.42) C19 - C20 - C21 - F9 -179.35 ( 0.37) F8 - C20 - C21 - C22 -0.06 ( 0.69) C19 - C20 - C21 - C22 -179.47 ( 0.36) C18 - C17 - C22 - F10 -2.80 ( 0.55) C16 - C17 - C22 - F10 0.85 ( 0.58) C18 - C17 - C22 - C21 177.51 ( 0.35) C16 - C17 - C22 - C21 1.18 ( 0.61) F9 - C21 - C22 - F10 179.67 ( 0.39) C20 - C21 - C22 - F10 -179.13 ( 0.38) F9 - C21 - C22 - C17 -0.63 ( 0.64) C20 - C21 - C22 - C17 3.50 ( 0.60) C15 - C16 - C23 - N3 174.23 ( 0.35) C17 - C16 - C23 - N3 -170.50 ( 0.37) C15 - C16 - C23 - C24 0.23 ( 0.52) C17 - C16 - C23 - C24 -172.04 ( 0.34) C16 - C23 - N3 - C26 2.51 ( 0.39) C24 - C23 - N3 - C26 -2.63 ( 0.45) N3 - C23 - C24 - C25 172.15 ( 0.35) C16 - C23 - C24 - C25 1.51 ( 0.43) C23 - C24 - C25 - C26 175.28 ( 0.35) C23 - N3 - C26 - C27 -1.53 ( 0.38) C23 - N3 - C26 - C25 -176.90 ( 0.37) C24 - C25 - C26 - C27 -0.07 ( 0.42) C24 - C25 - C26 - N3 9.86 ( 0.59) N3 - C26 - C27 - C34 -173.81 ( 0.34) C25 - C26 - C27 - C34 -168.77 ( 0.32) N3 - C26 - C27 - C28 7.56 ( 0.56) C25 - C26 - C27 - C28 -116.80 ( 0.41) C26 - C27 - C28 - C33 64.43 ( 0.47) C34 - C27 - C28 - C33 64.67 ( 0.48) C26 - C27 - C28 - C29 -114.11 ( 0.37) C34 - C27 - C28 - C29 -176.67 ( 0.35) C33 - C28 - C29 - F11 1.93 ( 0.53) C27 - C28 - C29 - F11 0.37 ( 0.56) C33 - C28 - C29 - C30 178.97 ( 0.37) C27 - C28 - C29 - C30 -1.82 ( 0.61) F11 - C29 - C30 - F12 -178.95 ( 0.37) C28 - C29 - C30 - F12 177.13 ( 0.40) F11 - C29 - C30 - C31 0.00 ( 0.65) C28 - C29 - C30 - C31 -1.34 ( 0.69) F12 - C30 - C31 - F13 179.70 ( 0.40) C29 - C30 - C31 - F13 178.02 ( 0.41) F12 - C30 - C31 - C32 -0.94 ( 0.70) C29 - C30 - C31 - C32 0.42 ( 0.66) F13 - C31 - C32 - F14 -178.95 ( 0.43) C30 - C31 - C32 - F14 -179.18 ( 0.41) F13 - C31 - C32 - C33 1.45 ( 0.68) C30 - C31 - C32 - C33 -179.11 ( 0.33) C29 - C28 - C33 - F15 2.31 ( 0.55) C27 - C28 - C33 - F15 0.17 ( 0.57) C29 - C28 - C33 - C32 -178.41 ( 0.36) C27 - C28 - C33 - C32 -1.37 ( 0.62) F14 - C32 - C33 - F15 178.22 ( 0.39) C31 - C32 - C33 - F15 179.33 ( 0.38) F14 - C32 - C33 - C28 -1.07 ( 0.63) C31 - C32 - C33 - C28 14.43 ( 0.57) C26 - C27 - C34 - N4 -166.90 ( 0.33) C28 - C27 - C34 - N4 -165.81 ( 0.39) C26 - C27 - C34 - C35 12.86 ( 0.56) C28 - C27 - C34 - C35 -1.30 ( 0.40) C35 - C34 - N4 - C37 178.51 ( 0.31) C27 - C34 - N4 - C37 1.19 ( 0.41) N4 - C34 - C35 - C36 -178.60 ( 0.36) C27 - C34 - C35 - C36 -0.69 ( 0.43) C34 - C35 - C36 - C37 0.88 ( 0.40) C34 - N4 - C37 - C36 -177.18 ( 0.31) C34 - N4 - C37 - C38 -0.10 ( 0.41) C35 - C36 - C37 - N4 177.70 ( 0.36) C35 - C36 - C37 - C38 77.65 ( 0.38) N1 - C1 - C38 - C37 -95.27 ( 0.41) C2 - C1 - C38 - C37 -42.46 ( 0.42) N1 - C1 - C38 - C40 144.62 ( 0.37) C2 - C1 - C38 - C40 -163.61 ( 0.31) N1 - C1 - C38 - C39 23.47 ( 0.52) C2 - C1 - C38 - C39 -70.70 ( 0.39) N4 - C37 - C38 - C1 111.77 ( 0.42) C36 - C37 - C38 - C1 50.59 ( 0.45) N4 - C37 - C38 - C40 -126.95 ( 0.41) C36 - C37 - C38 - C40 170.27 ( 0.33) N4 - C37 - C38 - C39 -7.27 ( 0.55) C36 - C37 - C38 - C39 FMAP and GRID set by program FMAP 2 1 77 GRID -1.351 -2 -1 1.351 2 1 R1 = 0.0591 for 3840 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.63 at 0.8788 0.6129 0.0628 [ 1.45 A from F5 ] Deepest hole -0.35 at 0.9740 0.4742 0.2039 [ 0.95 A from F5 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 6618 / 58427 Molecule 1 scale 0.369 inches = 0.937 cm per Angstrom F5 F8 C20 F9 F13 F7 F10 F6 C21 CL2 C19 CL5 F12 CL4 CL1 C22 CL3 C18 CL6 F*L3 C17 F10 F7 CL6 CL6 F9 C24 CL1 CL4 C25 C16 F8 CL5 F12 *** C23 CL2 C14 C15 F13 C30 F11 C31 C29 C26 F3 N3 C13 C32 C28 N2 1 F14 C33 C27 C12 F2 F15 F5 C34 C11 F4 F1 C5 N4 C6 C10 N4 C35 C4 N1 C7 C9 C8 F3 F4 C37 F1 C36 C40 C1 C3 F2 C38 F15 N2 C2 N3 C39 N3 F13 CL2 F8 F6 CL3 Atom Peak x y z Sof Height Distances and Angles N1 0.00 1.0493 0.8512 0.4247 1.000 3.6 0 H1N 0.994 0 C1 1.374 123.7 0 C4 1.391 123.8 109.7 0 N2 2.974 59.6 156.1 79.0 0 H2N 2.577 65.0 137.3 88.1 18.8 0 N4 3.177 77.6 72.2 139.7 86.7 69.7 0 H4N 2.801 64.5 86.3 140.0 74.0 58.5 15.0 0 H40A 2.617 47.3 76.5 164.7 101.0 96.5 55.1 52.5 H1N 0.00 1.0114 0.9423 0.4117 1.000 3.9 0 N1 0.994 0 N2 2.616 101.2 C1 0.11 1.1227 0.8146 0.5135 1.000 3.4 0 N1 1.374 0 C2 1.384 107.8 0 C38 1.501 121.4 130.5 C2 0.00 1.1749 0.7023 0.5004 1.000 3.2 0 C1 1.384 0 H2 0.950 126.3 0 C3 1.402 107.4 126.3 H2 0.11 1.2280 0.6524 0.5497 1.000 3.0 0 C2 0.950 19 N3 2.834 126.4 C3 0.08 1.1352 0.6757 0.4011 1.000 3.2 0 C2 1.402 0 H3 0.950 125.7 0 C4 1.392 108.6 125.7 H3 0.00 1.1580 0.6058 0.3713 1.000 3.1 0 C3 0.950 26 F15 2.764 165.6 C4 0.09 1.0569 0.7688 0.3536 1.000 3.5 0 N1 1.391 0 C3 1.392 106.3 0 C5 1.421 122.4 131.3 C5 0.12 0.9920 0.7855 0.2541 1.000 3.6 0 C4 1.421 0 C6 1.497 115.1 0 C12 1.375 125.7 119.1 C6 0.03 1.0317 0.7378 0.1863 1.000 3.7 0 C5 1.497 0 C7 1.372 120.8 0 C11 1.393 122.0 116.9 C7 0.09 1.1035 0.8152 0.1771 1.000 4.0 0 C6 1.372 0 F1 1.312 118.6 0 C8 1.374 124.4 117.0 F1 0.00 1.1368 0.9319 0.2291 1.000 4.4 0 C7 1.312 0 F2 2.668 61.5 28 H35 2.520 129.9 146.1 C8 0.05 1.1439 0.7786 0.1168 1.000 4.1 0 C7 1.374 0 F2 1.302 122.3 0 C9 1.407 117.0 120.2 F2 0.00 1.2143 0.8527 0.1127 1.000 4.4 0 F1 2.668 0 C8 1.302 59.1 0 F3 2.680 119.9 60.8 24 F13 2.794 90.4 147.4 146.4 39 CL2 3.111 113.1 97.2 71.8 83.5 C9 0.02 1.1141 0.6474 0.0670 1.000 3.7 0 C8 1.407 0 F3 1.331 117.5 0 C10 1.341 119.6 122.9 F3 0.23 1.1532 0.6108 0.0088 1.000 3.8 0 F2 2.680 0 C9 1.331 61.2 0 F4 2.724 119.5 58.4 9 H13 2.543 162.8 128.5 71.2 39 CL2 3.414 60.0 88.2 114.3 104.0 C10 0.00 1.0478 0.5659 0.0786 1.000 3.3 0 C9 1.341 0 F4 1.350 119.2 0 C11 1.392 122.5 118.3 F4 0.08 1.0210 0.4389 0.0319 1.000 3.0 0 F3 2.724 0 C10 1.350 59.5 0 F5 2.698 120.2 60.8 26 F15 3.235 89.7 69.0 70.7 C11 0.00 1.0051 0.6072 0.1374 1.000 3.3 0 C6 1.393 0 C10 1.392 119.3 0 F5 1.324 120.6 120.1 0 1 1.751 107.5 106.1 54.0 F5 0.17 0.9384 0.5243 0.1449 1.000 2.9 0 F4 2.698 0 C11 1.324 60.8 0 1 1.447 83.6 78.2 16 F8 3.156 116.5 139.4 61.6 C12 0.09 0.8979 0.8374 0.2170 1.000 3.7 0 C5 1.375 0 N2 1.396 126.1 0 C13 1.419 128.4 105.5 N2 0.00 0.8452 0.8652 0.2690 1.000 3.6 0 N1 2.974 0 H1N 2.616 19.1 0 C12 1.396 78.1 86.9 0 H2N 0.989 57.2 62.9 122.6 0 C15 1.379 165.3 146.4 110.3 121.8 0 N3 2.859 91.9 87.3 164.4 42.3 82.1 33 H40C 2.861 69.1 85.9 89.5 44.1 121.6 75.6 H2N 0.12 0.8622 0.8215 0.3327 1.000 3.4 0 N1 2.577 0 N2 0.989 103.9 0 N3 2.230 121.4 120.3 C13 0.13 0.8340 0.8729 0.1199 1.000 3.9 0 C12 1.419 0 H13 0.950 125.3 0 C14 1.351 109.4 125.3 H13 0.12 0.8499 0.8676 0.0674 1.000 4.0 0 C13 0.950 5 F3 2.543 113.2 C14 0.00 0.7469 0.9155 0.1138 1.000 4.0 0 C13 1.351 0 H14 0.950 125.7 0 C15 1.432 108.5 125.7 H14 0.11 0.6924 0.9472 0.0569 1.000 4.1 0 C14 0.950 14 F7 2.534 108.6 17 F9 2.754 126.3 124.9 C15 0.00 0.7506 0.9050 0.2075 1.000 3.7 0 N2 1.379 0 C14 1.432 105.9 0 C16 1.382 125.1 128.8 C16 0.00 0.6754 0.9188 0.2332 1.000 3.6 0 C15 1.382 0 C17 1.494 117.4 0 C23 1.428 124.7 117.3 C17 0.11 0.5748 0.9430 0.1542 1.000 3.7 0 C16 1.494 0 C18 1.373 123.0 0 C22 1.393 119.9 117.0 C18 0.00 0.5333 1.0769 0.1290 1.000 4.1 0 C17 1.373 0 F6 1.326 120.5 0 C19 1.396 121.8 117.6 F6 0.00 0.5831 1.1934 0.1736 1.000 4.5 0 C18 1.326 0 F7 2.670 62.2 29 H39A 2.568 137.4 160.4 17 F9 2.982 86.9 83.7 95.2 42 CL3 3.185 118.9 81.7 86.5 138.6 51 CL6 3.610 113.1 90.4 81.9 153.4 15.5 C19 0.00 0.4374 1.0957 0.0579 1.000 4.2 0 C18 1.396 0 F7 1.339 119.4 0 C20 1.368 119.4 121.2 F7 0.06 0.3995 1.2284 0.0379 1.000 4.6 0 F6 2.670 0 C19 1.339 60.8 0 F8 2.715 120.0 59.3 10 H14 2.535 132.0 160.7 106.2 18 F10 2.987 95.2 81.4 76.9 82.8 C20 0.07 0.3831 0.9780 0.0115 1.000 3.8 0 C19 1.368 0 F8 1.337 119.2 0 C21 1.355 120.8 119.9 F8 0.06 0.2912 0.9963 -0.0564 1.000 3.9 0 F7 2.715 0 C20 1.337 60.3 0 F9 2.718 120.0 59.7 30 H39B 2.926 129.4 119.8 83.4 7 F5 3.156 117.4 157.7 117.0 79.7 C21 0.05 0.4210 0.8438 0.0342 1.000 3.4 0 C20 1.355 0 F9 1.338 121.4 0 C22 1.396 119.4 119.2 F9 0.10 0.3679 0.7276 -0.0090 1.000 3.0 0 F8 2.718 0 C21 1.338 59.0 0 F10 2.690 119.8 60.9 11 H14 2.754 138.2 162.7 101.9 12 F6 2.982 96.3 100.8 94.9 81.4 40 CL2 3.383 110.9 89.6 67.8 81.5 152.4 C22 0.00 0.5167 0.8258 0.1059 1.000 3.3 0 C17 1.393 0 C21 1.396 121.6 0 F10 1.335 119.7 118.7 F10 0.05 0.5528 0.6929 0.1279 1.000 2.9 0 F9 2.690 0 C22 1.335 61.2 14 F7 2.987 83.2 84.9 49 CL5 3.371 73.0 103.6 146.1 40 CL2 3.437 65.7 88.2 147.5 15.5 C23 0.00 0.6844 0.8917 0.3275 1.000 3.4 0 C16 1.428 0 N3 1.335 125.9 0 C24 1.461 122.4 111.5 N3 0.00 0.7666 0.8563 0.4051 1.000 3.2 0 N2 2.859 0 H2N 2.230 17.4 0 C23 1.335 82.2 98.4 0 C26 1.394 167.1 150.8 105.5 0 N4 2.907 94.3 79.4 169.4 79.8 0 H4N 2.326 83.6 70.6 156.1 92.2 14.1 32 H40B 2.664 77.9 64.4 118.6 89.3 70.1 76.8 1 H2 2.834 100.3 108.2 84.0 90.9 86.8 79.7 156.5 C24 0.00 0.5997 0.8867 0.3476 1.000 3.2 0 C23 1.461 0 H24 0.950 126.9 0 C25 1.335 106.3 126.9 H24 0.00 0.5341 0.9110 0.3045 1.000 3.3 0 C24 0.950 25 F13 2.618 164.9 23 F12 2.666 118.4 61.6 C25 0.10 0.6329 0.8412 0.4384 1.000 2.9 0 C24 1.335 0 H25 0.950 126.4 0 C26 1.454 107.2 126.4 H25 0.00 0.5950 0.8248 0.4720 1.000 2.8 0 C25 0.950 23 F12 2.783 113.7 35 CL1 3.005 121.5 76.1 45 CL4 3.052 119.3 78.1 2.6 C26 0.00 0.7379 0.8214 0.4761 1.000 2.9 0 N3 1.394 0 C25 1.454 109.5 0 C27 1.381 125.5 125.0 C27 0.00 0.7987 0.7688 0.5667 1.000 2.7 0 C26 1.381 0 C28 1.497 118.6 0 C34 1.423 126.0 115.4 C28 0.10 0.7535 0.7111 0.6276 1.000 2.3 0 C27 1.497 0 C29 1.388 120.6 0 C33 1.375 122.0 117.4 C29 0.00 0.6946 0.5896 0.5993 1.000 1.9 0 C28 1.388 0 F11 1.333 120.7 0 C30 1.382 121.3 117.9 F11 0.08 0.6793 0.5196 0.5188 1.000 1.8 0 C29 1.333 0 F12 2.683 61.6 44 H42 2.576 124.9 107.1 34 H41 2.951 119.0 109.1 7.6 52 CL6 3.194 140.2 83.5 45.3 52.8 37 CL1 3.487 98.3 69.3 38.7 39.8 48.3 43 CL3 3.537 146.5 97.6 31.8 39.4 16.2 48.2 47 CL4 3.616 97.7 69.7 38.6 39.4 49.2 1.1 48.9 C30 0.00 0.6537 0.5337 0.6556 1.000 1.6 0 C29 1.382 0 F12 1.337 120.4 0 C31 1.363 119.7 119.9 F12 0.02 0.5984 0.4153 0.6278 1.000 1.2 0 F11 2.683 0 C30 1.337 60.1 0 F13 2.705 120.3 60.2 21 H24 2.666 154.0 111.6 58.4 22 H25 2.783 115.7 142.1 111.4 53.8 46 CL4 3.332 108.7 149.0 121.5 90.0 68.6 36 CL1 3.418 109.6 151.0 121.8 88.6 66.7 2.0 37 CL1 3.570 66.0 96.4 122.3 92.3 54.8 105.0 103.7 C31 0.06 0.6711 0.5986 0.7405 1.000 1.6 0 C30 1.363 0 F13 1.344 120.2 0 C32 1.382 120.7 119.1 F13 0.04 0.6313 0.5455 0.7955 1.000 1.3 0 F12 2.705 0 C31 1.344 59.8 0 F14 2.704 119.8 60.0 21 H24 2.618 60.1 113.0 154.5 4 F2 2.794 87.4 92.3 93.7 111.5 50 CL6 3.566 85.0 69.5 75.9 78.7 161.7 C32 0.00 0.7305 0.7185 0.7718 1.000 2.0 0 C31 1.382 0 F14 1.317 120.5 0 C33 1.380 118.6 120.9 F14 0.06 0.7484 0.7795 0.8546 1.000 2.1 0 F13 2.704 0 C32 1.317 60.4 0 F15 2.685 120.6 60.3 48 CL5 3.166 101.8 102.4 89.4 38 CL2 3.623 115.2 106.2 80.4 13.6 C33 0.08 0.7700 0.7731 0.7141 1.000 2.4 0 C28 1.375 0 C32 1.380 122.3 0 F15 1.341 119.8 117.9 F15 0.00 0.8253 0.8919 0.7442 1.000 2.8 0 F14 2.685 0 C33 1.341 60.9 2 H3 2.764 152.5 126.4 6 F4 3.235 71.5 121.8 111.4 C34 0.00 0.9025 0.7609 0.6085 1.000 2.7 0 C27 1.423 0 N4 1.377 122.8 0 C35 1.391 130.7 106.5 N4 0.08 0.9568 0.8334 0.5716 1.000 3.1 0 N1 3.177 0 N3 2.907 87.0 0 C34 1.377 150.2 81.7 0 H4N 0.864 57.0 41.1 121.8 0 C37 1.355 75.4 161.3 110.6 127.3 0 H40A 2.727 52.0 99.4 157.2 59.2 74.8 31 H40A 3.013 63.5 78.6 87.2 89.8 87.9 115.4 H4N 0.15 0.9296 0.8794 0.5176 1.000 3.3 0 N1 2.801 0 N3 2.326 109.4 0 N4 0.864 108.0 124.8 C35 0.09 0.9689 0.6865 0.6890 1.000 2.4 0 C34 1.391 0 H35 0.950 126.3 0 C36 1.401 107.4 126.3 H35 0.07 0.9534 0.6252 0.7292 1.000 2.1 0 C35 0.950 3 F1 2.520 157.3 C36 0.07 1.0628 0.7185 0.6999 1.000 2.7 0 C35 1.401 0 H36 0.950 125.9 0 C37 1.377 108.2 125.9 H36 0.00 1.1226 0.6834 0.7494 1.000 2.5 0 C36 0.950 C37 0.00 1.0537 0.8098 0.6265 1.000 3.1 0 N4 1.355 0 C36 1.377 107.3 0 C38 1.517 121.4 131.2 C38 0.00 1.1301 0.8827 0.6043 1.000 3.5 0 C1 1.501 0 C37 1.517 106.4 0 C39 1.528 110.1 109.7 0 C40 1.521 111.8 110.0 108.8 C39 0.00 1.2317 0.8570 0.6870 1.000 3.4 0 C38 1.528 0 H39A 0.980 109.5 0 H39B 0.980 109.5 109.5 0 H39C 0.980 109.5 109.5 109.5 H39A 0.11 1.2444 0.7534 0.6956 1.000 3.0 0 C39 0.980 13 F6 2.568 113.1 H39B 0.09 1.2349 0.8981 0.7465 1.000 3.4 0 C39 0.980 15 F8 2.926 166.6 H39C 0.14 1.2810 0.9029 0.6721 1.000 3.6 0 C39 0.980 41 CL3 3.089 143.9 C40 0.00 1.1110 1.0437 0.5924 1.000 4.0 0 C38 1.521 0 H40A 0.980 109.5 0 H40B 0.980 109.5 109.5 0 H40C 0.980 109.5 109.5 109.5 H40A 0.00 1.0482 1.0616 0.5363 1.000 4.1 0 N1 2.617 0 N4 2.727 72.9 0 C40 0.980 99.6 94.4 27 N4 3.013 105.4 151.2 114.0 H40B 0.05 1.1634 1.0908 0.5829 1.000 4.2 0 C40 0.980 20 N3 2.664 137.2 H40C 0.00 1.1093 1.0824 0.6504 1.000 4.0 0 C40 0.980 8 N2 2.861 129.6 1 0.63 0.8788 0.6129 0.0628 1.000 3.3 0 C11 1.751 0 F5 1.447 47.8 Code Atom x y z Height Symmetry Transformation 1 H2 0.7720 1.1524 0.4503 4.1 2.0000-X 0.5000+Y 1.0000-Z 2 H3 0.8420 1.1058 0.6287 3.7 2.0000-X 0.5000+Y 1.0000-Z 3 F1 0.8632 0.4319 0.7709 1.3 2.0000-X -0.5000+Y 1.0000-Z 4 F2 0.7857 0.3527 0.8873 0.7 2.0000-X -0.5000+Y 1.0000-Z 5 F3 0.8468 1.1108 -0.0088 5.0 2.0000-X 0.5000+Y 0.0000-Z 6 F4 0.9790 0.9389 0.9681 2.7 2.0000-X 0.5000+Y 1.0000-Z 7 F5 0.0616 1.0243 -0.1449 3.8 1.0000-X 0.5000+Y 0.0000-Z 8 N2 1.1548 1.3652 0.7310 4.8 2.0000-X 0.5000+Y 1.0000-Z 9 H13 1.1501 0.3676 -0.0674 3.1 2.0000-X -0.5000+Y 0.0000-Z 10 H14 0.3076 1.4472 -0.0569 5.3 1.0000-X 0.5000+Y 0.0000-Z 11 H14 0.3076 0.4472 -0.0569 2.1 1.0000-X -0.5000+Y 0.0000-Z 12 F6 0.4169 0.6934 -0.1736 3.3 1.0000-X -0.5000+Y 0.0000-Z 13 F6 1.4169 0.6934 0.8264 2.8 2.0000-X -0.5000+Y 1.0000-Z 14 F7 0.6005 0.7284 -0.0379 3.4 1.0000-X -0.5000+Y 0.0000-Z 15 F8 1.2912 0.9963 0.9436 3.4 1.0000+X 0.0000+Y 1.0000+Z 16 F8 0.7088 0.4963 0.0564 2.7 1.0000-X -0.5000+Y 0.0000-Z 17 F9 0.6321 1.2276 0.0090 5.0 1.0000-X 0.5000+Y 0.0000-Z 18 F10 0.4472 1.1929 -0.1279 4.9 1.0000-X 0.5000+Y 0.0000-Z 19 N3 1.2334 0.3563 0.5949 1.9 2.0000-X -0.5000+Y 1.0000-Z 20 N3 1.2334 1.3563 0.5949 5.2 2.0000-X 0.5000+Y 1.0000-Z 21 H24 0.4659 0.4110 0.6954 0.8 1.0000-X -0.5000+Y 1.0000-Z 22 H25 0.4050 0.3248 0.5280 0.8 1.0000-X -0.5000+Y 1.0000-Z 23 F12 0.4016 0.9153 0.3722 3.0 1.0000-X 0.5000+Y 1.0000-Z 24 F13 1.3687 1.0455 0.2045 5.1 2.0000-X 0.5000+Y 1.0000-Z 25 F13 0.3687 1.0455 0.2045 3.7 1.0000-X 0.5000+Y 1.0000-Z 26 F15 1.1747 0.3919 0.2558 2.6 2.0000-X -0.5000+Y 1.0000-Z 27 N4 1.0432 1.3334 0.4284 5.1 2.0000-X 0.5000+Y 1.0000-Z 28 H35 1.0466 1.1252 0.2708 4.8 2.0000-X 0.5000+Y 1.0000-Z 29 H39A 0.7556 1.2534 0.3044 4.7 2.0000-X 0.5000+Y 1.0000-Z 30 H39B 0.2349 0.8981 -0.2535 3.9 -1.0000+X 0.0000+Y -1.0000+Z 31 H40A 0.9518 0.5616 0.4637 2.4 2.0000-X -0.5000+Y 1.0000-Z 32 H40B 0.8366 0.5908 0.4171 2.5 2.0000-X -0.5000+Y 1.0000-Z 33 H40C 0.8907 0.5824 0.3496 2.6 2.0000-X -0.5000+Y 1.0000-Z 34 H41 0.5230 0.6200 0.3334 2.3 1.0000-X 0.5000+Y 1.0000-Z 35 CL1 0.5747 1.0504 0.6007 3.2 0.0000+X 1.0000+Y 0.0000+Z 36 CL1 0.5747 0.0504 0.6007 0.0 0.0000+X 0.0000+Y 0.0000+Z 37 CL1 0.4253 0.5504 0.3993 1.8 1.0000-X 0.5000+Y 1.0000-Z 38 CL2 0.6222 1.1220 0.7961 3.1 0.0000+X 1.0000+Y 0.0000+Z 39 CL2 1.3778 0.6220 0.2039 3.8 2.0000-X 0.5000+Y 1.0000-Z 40 CL2 0.3778 0.6220 0.2039 2.3 1.0000-X 0.5000+Y 1.0000-Z 41 CL3 1.4956 0.8845 0.7055 3.8 1.0000+X 1.0000+Y 0.0000+Z 42 CL3 0.5044 1.3845 0.2945 4.8 1.0000-X 1.5000+Y 1.0000-Z 43 CL3 0.5044 0.3845 0.2945 1.6 1.0000-X 0.5000+Y 1.0000-Z 44 H42 0.5387 0.5718 0.3508 2.1 1.0000-X 0.5000+Y 1.0000-Z 45 CL4 0.5837 1.0586 0.6048 3.2 0.0000+X 1.0000+Y 0.0000+Z 46 CL4 0.5837 0.0586 0.6048 0.0 0.0000+X 0.0000+Y 0.0000+Z 47 CL4 0.4163 0.5586 0.3952 1.8 1.0000-X 0.5000+Y 1.0000-Z 48 CL5 0.5939 1.0330 0.7908 2.8 0.0000+X 1.0000+Y 0.0000+Z 49 CL5 0.4061 0.5330 0.2092 2.1 1.0000-X 0.5000+Y 1.0000-Z 50 CL6 0.4837 0.8284 0.6458 2.3 0.0000+X 1.0000+Y 0.0000+Z 51 CL6 0.5163 1.3284 0.3542 4.5 1.0000-X 1.5000+Y 1.0000-Z 52 CL6 0.5163 0.3284 0.3542 1.3 1.0000-X 0.5000+Y 1.0000-Z Molecule 2 scale 0.839 inches = 2.131 cm per Angstrom F9 F3 F2 F10 CL2 CL5 F14 F6 F12 C41 F13 CL3 C42 CL6 CL4 CL1 F11 F12 Atom Peak x y z Sof Height Distances and Angles C41 0.13 0.5348 0.0541 0.6894 0.567 3.1 0 H41 1.000 0 CL1 1.737 107.4 0 CL2 1.716 107.4 111.9 0 CL3 1.744 107.4 111.1 111.4 0 C42 0.504 102.5 72.7 146.1 42.7 0 H42 1.025 29.9 101.4 134.2 83.1 72.9 0 CL4 1.779 108.7 4.5 107.4 114.3 76.8 104.7 0 CL5 1.433 119.7 126.4 32.5 78.9 116.6 132.2 123.1 0 CL6 2.237 109.5 86.5 130.8 25.7 17.7 80.1 90.2 99.6 H41 0.09 0.4770 0.1200 0.6666 0.567 2.4 0 C41 1.000 0 C42 1.213 23.9 0 H42 0.523 77.7 54.0 7 F11 2.951 110.7 87.7 40.5 CL1 0.00 0.5747 0.0504 0.6007 0.567 4.0 0 C41 1.737 0 C42 1.659 16.8 0 CL4 0.145 104.3 119.4 6 H25 3.005 135.8 119.8 107.3 8 F12 3.418 86.5 101.7 52.6 137.5 7 F11 3.487 73.8 64.3 152.7 90.6 100.3 9 F12 3.570 115.2 101.3 138.9 49.2 117.5 44.7 CL2 0.04 0.6222 0.1220 0.7961 0.567 3.7 0 C41 1.716 0 C42 2.152 7.5 0 CL5 0.921 56.6 50.4 1 F2 3.111 144.4 148.7 155.6 4 F9 3.383 136.3 136.9 99.3 71.4 2 F3 3.414 152.1 145.4 107.3 48.2 63.6 5 F10 3.437 90.6 92.9 78.2 107.6 46.5 109.3 11 F14 3.623 90.9 83.6 53.7 105.2 103.0 62.6 119.4 CL3 0.00 0.4956 -0.1155 0.7055 0.567 2.6 0 C41 1.744 0 C42 1.416 14.0 0 CL5 2.033 43.8 56.4 0 CL6 1.006 105.7 91.9 136.7 12 H39C 3.089 109.4 110.0 119.4 97.7 3 F6 3.185 146.4 158.6 111.1 107.0 58.5 7 F11 3.537 72.3 62.5 114.3 62.2 62.4 117.3 C42 0.00 0.5206 0.0097 0.6695 0.433 3.0 0 C41 0.504 0 H41 1.213 53.6 0 CL1 1.659 90.4 102.0 0 CL2 2.152 26.4 77.5 96.4 0 CL3 1.416 123.4 118.0 137.8 104.6 0 H42 1.000 78.4 25.0 108.0 100.9 103.4 0 CL4 1.735 86.7 101.3 4.2 92.3 139.6 109.1 0 CL5 1.719 48.2 90.7 114.0 24.4 80.3 109.1 110.0 0 CL6 1.764 157.3 133.0 106.8 133.4 34.8 109.1 109.8 109.9 H42 0.00 0.4613 0.0718 0.6492 0.433 2.3 0 C41 1.025 0 H41 0.523 72.4 0 C42 1.000 28.8 101.0 7 F11 2.576 141.0 131.9 116.0 CL4 0.00 0.5837 0.0587 0.6048 0.433 4.1 0 C41 1.779 0 CL1 0.145 71.1 0 C42 1.735 16.4 56.4 6 H25 3.052 130.6 70.1 114.6 8 F12 3.332 88.6 125.4 103.1 139.5 7 F11 3.616 69.8 26.3 60.4 87.5 99.3 CL5 0.11 0.5939 0.0330 0.7908 0.433 3.4 0 C41 1.433 0 CL2 0.921 90.9 0 CL3 2.033 57.3 148.2 0 C42 1.719 15.2 105.2 43.3 11 F14 3.166 117.5 112.7 85.9 106.1 5 F10 3.371 98.7 86.3 97.0 104.4 137.7 CL6 0.02 0.4837 -0.1716 0.6458 0.433 2.7 0 C41 2.237 0 CL3 1.006 48.7 0 C42 1.764 5.0 53.3 7 F11 3.194 76.2 101.6 72.4 10 F13 3.566 117.5 89.0 121.3 166.3 3 F6 3.610 105.8 57.5 110.2 115.0 63.5 Code Atom x y z Height Symmetry Transformation 1 F2 0.7857 0.3527 0.8873 5.3 2.0000-X -0.5000+Y 1.0000-Z 2 F3 0.8468 0.1108 0.9912 5.7 2.0000-X -0.5000+Y 1.0000-Z 3 F6 0.4169 -0.3066 0.8264 1.1 1.0000-X -1.5000+Y 1.0000-Z 4 F9 0.6321 0.2276 1.0090 2.9 1.0000-X -0.5000+Y 1.0000-Z 5 F10 0.4472 0.1929 0.8721 1.1 1.0000-X -0.5000+Y 1.0000-Z 6 H25 0.5950 -0.1752 0.4720 4.9 0.0000+X -1.0000+Y 0.0000+Z 7 F11 0.3207 0.0196 0.4812 1.3 1.0000-X -0.5000+Y 1.0000-Z 8 F12 0.5984 0.4153 0.6278 4.0 0.0000+X 0.0000+Y 0.0000+Z 9 F12 0.4016 -0.0847 0.3722 2.9 1.0000-X -0.5000+Y 1.0000-Z 10 F13 0.6313 -0.4545 0.7955 4.0 0.0000+X -1.0000+Y 0.0000+Z 11 F14 0.7484 -0.2205 0.8546 5.2 0.0000+X -1.0000+Y 0.0000+Z 12 H39C 0.2810 -0.0971 0.6721 0.0 -1.0000+X -1.0000+Y 0.0000+Z Molecule 3 Atom Peak x y z Sof Height Distances and Angles 2 0.52 0.0511 0.0832 0.0704 1.000 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. 0.11: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.53: Structure factors and derivatives 4.20: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.86: Solve l.s. equations 0.00: Generate HTAB table 0.09: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.08: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.03: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + udel1 finished at 14:08:10 Total CPU time: 6.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++