+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 13:23:13 on 14-Oct-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P-1 CELL 0.71073 10.9353 11.1412 15.5260 81.631 82.691 86.120 ZERR 1.00 0.0003 0.0002 0.0004 0.001 0.001 0.001 LATT 1 SFAC C H N S CR UNIT 56 40 6 36 1 V = 1853.89 F(000) = 1018.0 Mu = 1.21 mm-1 Cell Wt = 2003.10 Rho = 1.794 MERG 2 ACTA OMIT 4 -4 4 OMIT 4 3 0 EADP S5A S5B EADP S6A S6B EADP C1A C2B EADP C2A C1B EADP C5A C6B EADP C6A C5B EADP C7A C7B EADP C8A C8B EADP C9A C9B EADP C10A C10B EADP S15A S15B EADP S16A S16B EADP C11A C12B EADP C12A C11B EADP C15A C16B EADP C16A C15B EADP C17A C17B EADP C18A C18B EADP C19A C19B EADP C20A C20B EADP S23A S23B EADP C21A C22B EADP C22A C21B EADP C24A C24B EADP C25A C25B EXYZ C1A C2B EXYZ C2A C1B EXYZ C5A C6B EXYZ C6A C5B EXYZ C11A C12B EXYZ C12A C11B EXYZ C15A C16B EXYZ C16A C15B EXYZ C21A C22B EXYZ C22A C21B FMAP 2 BOND $H PLAN 10 SIZE 0.05 0.15 0.35 WGHT 0.03470 0.28240 L.S. 20 TEMP -153.00 FVAR 0.16700 0.86162 0.96682 0.29996 0.95752 0.93972 MOLE 1 CR1 5 0.000000 0.500000 0.000000 10.50000 0.01731 0.01739 = 0.01659 -0.00455 -0.00168 0.00115 S31 4 0.220732 0.848471 0.026591 11.00000 0.04982 0.02565 = 0.02910 0.00304 -0.01327 -0.01527 S32 4 0.014979 0.525663 -0.310114 11.00000 0.02764 0.03540 = 0.01814 -0.00100 -0.00547 0.00350 S33 4 -0.386247 0.731303 -0.006932 11.00000 0.02428 0.02932 = 0.02572 -0.00292 -0.00652 0.00931 N31 3 0.092363 0.648122 0.005727 11.00000 0.02128 0.02328 = 0.02155 -0.00572 0.00000 -0.00010 N32 3 0.022974 0.527101 -0.131128 11.00000 0.02056 0.01888 = 0.02443 -0.00371 -0.00299 0.00330 N33 3 -0.156816 0.604966 -0.000655 11.00000 0.02054 0.02075 = 0.01870 -0.00482 -0.00048 -0.00081 C31 1 0.145161 0.731875 0.014382 11.00000 0.02430 0.02418 = 0.01352 0.00043 -0.00352 0.00383 C32 1 0.019594 0.526805 -0.205821 11.00000 0.01268 0.01860 = 0.02861 -0.00046 -0.00348 0.00487 C33 1 -0.251483 0.658990 -0.003380 11.00000 0.02361 0.01738 = 0.01543 -0.00306 -0.00099 -0.00215 MOLE 2 S1 4 0.289103 0.695815 0.582453 11.00000 0.03136 0.01488 = 0.01750 -0.00137 -0.00529 -0.00010 S2 4 0.360678 0.435952 0.626321 11.00000 0.02989 0.01563 = 0.01693 -0.00194 -0.00459 0.00160 S3 4 0.345701 0.398200 0.424719 11.00000 0.03031 0.01528 = 0.01739 -0.00222 -0.00587 0.00206 S4 4 0.278043 0.659549 0.382558 11.00000 0.03833 0.01480 = 0.01803 -0.00317 -0.00847 0.00237 C3 1 0.322491 0.554732 0.546420 11.00000 0.02236 0.01555 = 0.02039 -0.00153 -0.00337 -0.00125 C4 1 0.316231 0.539522 0.460919 11.00000 0.02368 0.01736 = 0.01896 -0.00176 -0.00348 -0.00129 PART 1 C2A 1 0.346460 0.524642 0.710297 21.00000 0.01815 0.01936 = 0.01778 -0.00214 -0.00041 -0.00245 C1A 1 0.312613 0.642616 0.689510 21.00000 0.01882 0.01902 = 0.01816 -0.00249 -0.00141 -0.00266 S5A 4 0.285379 0.728227 0.776299 21.00000 0.03285 0.01517 = 0.01845 -0.00406 -0.00514 0.00106 C8A 1 0.336678 0.597258 0.852678 21.00000 0.02228 0.01832 = 0.01490 -0.00062 0.00061 -0.00057 AFIX 23 H8A1 2 0.415796 0.613641 0.872359 21.00000 -1.20000 H8A2 2 0.274547 0.583507 0.904894 21.00000 -1.20000 AFIX 0 C7A 1 0.353173 0.484505 0.805674 21.00000 0.02614 0.01583 = 0.01946 -0.00097 -0.00181 -0.00216 AFIX 23 H7A1 2 0.434028 0.441986 0.814483 21.00000 -1.20000 H7A2 2 0.287391 0.427795 0.829644 21.00000 -1.20000 AFIX 0 SAME C2A > C7A C6A 1 0.299346 0.574055 0.296348 31.00000 0.02383 0.01832 = 0.01785 -0.00304 -0.00508 -0.00268 C5A 1 0.329683 0.455330 0.316329 31.00000 0.02108 0.02117 = 0.01638 -0.00399 -0.00416 -0.00051 S6A 4 0.341953 0.370604 0.229206 31.00000 0.02667 0.01780 = 0.01910 -0.00638 -0.00348 -0.00018 C10A 1 0.314818 0.510012 0.152570 31.00000 0.02665 0.02800 = 0.01784 -0.00517 -0.00721 0.00293 AFIX 23 H10A 2 0.391265 0.528646 0.112663 31.00000 -1.20000 H10B 2 0.249409 0.497575 0.116607 31.00000 -1.20000 AFIX 0 C9A 1 0.275395 0.616727 0.204274 31.00000 0.03056 0.01898 = 0.01519 -0.00048 -0.00401 -0.00590 AFIX 23 H9A1 2 0.323897 0.688258 0.179555 31.00000 -1.20000 H9A2 2 0.186709 0.639637 0.201843 31.00000 -1.20000 AFIX 0 PART 2 SAME C2A > C7A C2B 1 0.312613 0.642616 0.689510 -21.00000 0.01882 0.01902 = 0.01816 -0.00249 -0.00141 -0.00266 C1B 1 0.346460 0.524642 0.710297 -21.00000 0.01815 0.01936 = 0.01778 -0.00214 -0.00041 -0.00245 S5B 4 0.368588 0.457064 0.815200 -21.00000 0.03285 0.01517 = 0.01845 -0.00406 -0.00514 0.00106 C8B 1 0.347306 0.615225 0.844328 -21.00000 0.02228 0.01832 = 0.01490 -0.00062 0.00061 -0.00057 AFIX 23 H8B1 2 0.294078 0.614934 0.900919 -21.00000 -1.20000 H8B2 2 0.428353 0.645068 0.851008 -21.00000 -1.20000 AFIX 0 C7B 1 0.287372 0.700629 0.771955 -21.00000 0.02614 0.01583 = 0.01946 -0.00097 -0.00181 -0.00216 AFIX 23 H7B1 2 0.197320 0.711267 0.788847 -21.00000 -1.20000 H7B2 2 0.323334 0.781347 0.762880 -21.00000 -1.20000 AFIX 0 SAME C2A > C7A C6B 1 0.329683 0.455330 0.316329 -31.00000 0.02108 0.02117 = 0.01638 -0.00399 -0.00416 -0.00051 C5B 1 0.299346 0.574055 0.296348 -31.00000 0.02383 0.01832 = 0.01785 -0.00304 -0.00508 -0.00268 S6B 4 0.294836 0.637516 0.189003 -31.00000 0.02667 0.01780 = 0.01910 -0.00638 -0.00348 -0.00018 C10B 1 0.290463 0.480505 0.162048 -31.00000 0.02665 0.02800 = 0.01784 -0.00517 -0.00721 0.00293 AFIX 23 H10C 2 0.205517 0.464528 0.152669 -31.00000 -1.20000 H10D 2 0.345671 0.471497 0.107425 -31.00000 -1.20000 AFIX 0 C9B 1 0.332712 0.388779 0.238424 -31.00000 0.03056 0.01898 = 0.01519 -0.00048 -0.00401 -0.00590 AFIX 23 H9B1 2 0.276781 0.320556 0.252460 -31.00000 -1.20000 H9B2 2 0.417389 0.355550 0.222070 -31.00000 -1.20000 AFIX 0 MOLE 3 PART 0 S11 4 0.099838 0.231715 0.608393 11.00000 0.02421 0.02433 = 0.02080 -0.00579 -0.00560 0.00708 S12 4 0.190801 -0.024957 0.638816 11.00000 0.02282 0.01966 = 0.01785 -0.00256 -0.00322 -0.00102 S13 4 0.183627 -0.048741 0.435270 11.00000 0.02352 0.01846 = 0.01820 -0.00237 -0.00256 -0.00186 S14 4 0.091757 0.207924 0.403872 11.00000 0.02462 0.02380 = 0.01922 -0.00502 -0.00655 0.00644 C13 1 0.144172 0.097132 0.564682 11.00000 0.01366 0.02232 = 0.02121 -0.00164 -0.00296 0.00090 C14 1 0.140958 0.087177 0.477538 11.00000 0.01631 0.02151 = 0.01891 -0.00115 -0.00395 -0.00037 PART 3 SAME C2A > C7A C12A 1 0.167366 0.054941 0.727907 41.00000 0.01402 0.02673 = 0.01812 -0.00389 -0.00360 -0.00190 C11A 1 0.126933 0.171926 0.714442 41.00000 0.01495 0.02646 = 0.02295 -0.00798 -0.00418 0.00172 S15A 4 0.104289 0.257929 0.800838 41.00000 0.02050 0.02275 = 0.01515 -0.00417 -0.00308 0.00108 C18A 1 0.132980 0.116038 0.875740 41.00000 0.03045 0.02078 = 0.02081 -0.00716 -0.00354 0.00093 AFIX 23 H18A 2 0.193265 0.129596 0.915386 41.00000 -1.20000 H18B 2 0.055144 0.091746 0.912041 41.00000 -1.20000 AFIX 0 C17A 1 0.183703 0.014840 0.821323 41.00000 0.03231 0.03655 = 0.03879 -0.00174 -0.01192 -0.01714 AFIX 23 H17A 2 0.272367 -0.003203 0.827291 41.00000 -1.20000 H17B 2 0.139119 -0.060128 0.842995 41.00000 -1.20000 AFIX 0 SAME C2A > C7A C16A 1 0.116469 0.129237 0.314438 51.00000 0.01349 0.02444 = 0.02157 -0.00273 -0.00345 -0.00182 C15A 1 0.157840 0.012037 0.329158 51.00000 0.01547 0.02309 = 0.01932 -0.00320 -0.00326 -0.00365 S16A 4 0.173286 -0.068019 0.239388 51.00000 0.02909 0.02136 = 0.01964 -0.00471 -0.00216 -0.00540 C20A 1 0.138154 0.074233 0.166803 51.00000 0.02087 0.02704 = 0.01855 -0.00312 -0.00247 0.00053 AFIX 23 H20A 2 0.214299 0.101897 0.129781 51.00000 -1.20000 H20B 2 0.077436 0.059549 0.127803 51.00000 -1.20000 AFIX 0 C19A 1 0.085389 0.172124 0.223335 51.00000 0.01997 0.02272 = 0.02027 -0.00004 -0.00721 -0.00082 AFIX 23 H19A 2 0.122572 0.250720 0.200288 51.00000 -1.20000 H19B 2 -0.005189 0.183037 0.223179 51.00000 -1.20000 AFIX 0 PART 4 SAME C2A > C7A C12B 1 0.126933 0.171926 0.714442 -41.00000 0.01495 0.02646 = 0.02295 -0.00798 -0.00418 0.00172 C11B 1 0.167366 0.054941 0.727907 -41.00000 0.01402 0.02673 = 0.01812 -0.00389 -0.00360 -0.00190 S15B 4 0.186669 -0.011559 0.834742 -41.00000 0.02050 0.02275 = 0.01515 -0.00417 -0.00308 0.00108 C18B 1 0.141081 0.136269 0.872974 -41.00000 0.03045 0.02078 = 0.02081 -0.00716 -0.00354 0.00093 AFIX 23 H18C 2 0.075034 0.125186 0.922929 -41.00000 -1.20000 H18D 2 0.212755 0.168548 0.893489 -41.00000 -1.20000 AFIX 0 C17B 1 0.094448 0.227714 0.798144 -41.00000 0.03231 0.03655 = 0.03879 -0.00174 -0.01192 -0.01714 AFIX 23 H17C 2 0.004014 0.243090 0.809582 -41.00000 -1.20000 H17D 2 0.134627 0.305802 0.793371 -41.00000 -1.20000 AFIX 0 SAME C2A > C7A C16B 1 0.157840 0.012037 0.329158 -51.00000 0.01547 0.02309 = 0.01932 -0.00320 -0.00326 -0.00365 C15B 1 0.116469 0.129237 0.314438 -51.00000 0.01349 0.02444 = 0.02157 -0.00273 -0.00345 -0.00182 S16B 4 0.077267 0.187874 0.212281 -51.00000 0.02909 0.02136 = 0.01964 -0.00471 -0.00216 -0.00540 C20B 1 0.141067 0.044754 0.171894 -51.00000 0.02087 0.02704 = 0.01855 -0.00312 -0.00247 0.00053 AFIX 23 H20C 2 0.082884 0.016137 0.136299 -51.00000 -1.20000 H20D 2 0.220327 0.059384 0.134377 -51.00000 -1.20000 AFIX 0 C19B 1 0.161606 -0.052554 0.250871 -51.00000 0.01997 0.02272 = 0.02027 -0.00004 -0.00721 -0.00082 AFIX 23 H19C 2 0.096101 -0.111848 0.260343 -51.00000 -1.20000 H19D 2 0.242527 -0.096741 0.240259 -51.00000 -1.20000 AFIX 0 MOLE 4 PART 0 S21 4 0.534541 -0.150063 0.421501 11.00000 0.02195 0.01332 = 0.01633 -0.00227 -0.00376 0.00137 S22 4 0.465437 0.112310 0.375665 11.00000 0.02234 0.01298 = 0.01553 -0.00207 -0.00437 0.00149 C23 1 0.499754 -0.007756 0.457381 11.00000 0.01624 0.01575 = 0.01713 -0.00180 -0.00308 0.00045 PART 5 SAME C2A > C7A C22A 1 0.486293 0.022493 0.290993 61.00000 0.01652 0.01546 = 0.01594 -0.00312 -0.00189 -0.00134 C21A 1 0.517299 -0.095090 0.312603 61.00000 0.01640 0.01810 = 0.01538 -0.00451 -0.00240 -0.00116 S23A 4 0.539841 -0.181706 0.225950 61.00000 0.02929 0.01554 = 0.01771 -0.00507 -0.00487 0.00054 C25A 1 0.495693 -0.048251 0.148329 61.00000 0.02331 0.02494 = 0.01578 -0.00414 -0.00492 0.00201 AFIX 23 H25A 2 0.562051 -0.034012 0.098852 61.00000 -1.20000 H25B 2 0.419336 -0.063428 0.124402 61.00000 -1.20000 AFIX 0 C24A 1 0.474320 0.064177 0.196413 61.00000 0.02076 0.01749 = 0.01892 -0.00054 -0.00509 -0.00367 AFIX 23 H24A 2 0.536227 0.124703 0.171782 61.00000 -1.20000 H24B 2 0.391011 0.102298 0.189698 61.00000 -1.20000 AFIX 0 PART 6 SAME C2A > C7A C22B 1 0.517299 -0.095090 0.312603 -61.00000 0.01640 0.01810 = 0.01538 -0.00451 -0.00240 -0.00116 C21B 1 0.486293 0.022493 0.290993 -61.00000 0.01652 0.01546 = 0.01594 -0.00312 -0.00189 -0.00134 S23B 4 0.468868 0.083923 0.185430 -61.00000 0.02929 0.01554 = 0.01771 -0.00507 -0.00487 0.00054 C25B 1 0.514367 -0.068668 0.152916 -61.00000 0.02331 0.02494 = 0.01578 -0.00414 -0.00492 0.00201 AFIX 23 H25C 2 0.447511 -0.096747 0.124506 -61.00000 -1.20000 H25D 2 0.589570 -0.063215 0.109965 -61.00000 -1.20000 AFIX 0 C24B 1 0.539523 -0.161148 0.233821 -61.00000 0.02076 0.01749 = 0.01892 -0.00054 -0.00509 -0.00367 AFIX 23 H24C 2 0.483609 -0.229076 0.240859 -61.00000 -1.20000 H24D 2 0.625813 -0.194706 0.226723 -61.00000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for s92 in P-1 C 0.770 H 0.320 N 0.700 S 1.030 CR 1.240 Cr1 - N32 N32_$1 N33_$1 N33 N31_$1 N31 S31 - C31 S32 - C32 S33 - C33 N31 - C31 Cr1 N32 - C32 Cr1 N33 - C33 Cr1 C31 - N31 S31 C32 - N32 S32 C33 - N33 S33 S1 - C2B_b C1A_a C3 S2 - C1B_b C2A_a C3 S3 - C6B_b C5A_a C4 S4 - C5B_b C6A_a C4 C3 - C4 S1 S2 C4 - C3 S4 S3 C2A_a - C1A_a C7A_a S2 C1A_a - C2A_a S1 S5A_a S5A_a - C1A_a C8A_a C8A_a - C7A_a S5A_a C7A_a - C2A_a C8A_a C6A_a - C5A_a C9A_a S4 C5A_a - C6A_a S3 S6A_a S6A_a - C5A_a C10A_a C10A_a - C9A_a S6A_a C9A_a - C6A_a C10A_a C2B_b - C1B_b C7B_b S1 C1B_b - C2B_b S5B_b S2 S5B_b - C1B_b C8B_b C8B_b - C7B_b S5B_b C7B_b - C2B_b C8B_b C6B_b - C5B_b C9B_b S3 C5B_b - C6B_b S6B_b S4 S6B_b - C5B_b C10B_b C10B_b - C9B_b S6B_b C9B_b - C6B_b C10B_b S11 - C12B_d C11A_c C13 S12 - C11B_d C12A_c C13 S13 - C16B_d C15A_c C14 S14 - C15B_d C16A_c C14 C13 - C14 S12 S11 C14 - C13 S14 S13 C12A_c - C11A_c C17A_c S12 C11A_c - C12A_c S11 S15A_c S15A_c - C11A_c C18A_c C18A_c - C17A_c S15A_c C17A_c - C12A_c C18A_c C16A_c - C15A_c C19A_c S14 C15A_c - C16A_c S13 S16A_c S16A_c - C15A_c C20A_c C20A_c - C19A_c S16A_c C19A_c - C16A_c C20A_c C12B_d - C11B_d C17B_d S11 C11B_d - C12B_d S12 S15B_d S15B_d - C11B_d C18B_d C18B_d - C17B_d S15B_d C17B_d - C12B_d C18B_d C16B_d - C15B_d C19B_d S13 C15B_d - C16B_d S16B_d S14 S16B_d - C15B_d C20B_d C20B_d - C19B_d S16B_d C19B_d - C16B_d C20B_d S21 - C22B_f C21A_e C23 S22 - C21B_f C22A_e C23 C23 - C23_$2 S21 S22 C22A_e - C21A_e C24A_e S22 C21A_e - C22A_e S21 S23A_e S23A_e - C21A_e C25A_e C25A_e - C24A_e S23A_e C24A_e - C22A_e C25A_e C22B_f - C21B_f C24B_f S21 C21B_f - C22B_f S23B_f S22 S23B_f - C21B_f C25B_f C25B_f - C24B_f S23B_f C24B_f - C22B_f C25B_f Operators for generating equivalent atoms: $1 -x, -y+1, -z $2 -x+1, -y, -z+1 35809 Reflections read, of which 12 rejected -14 =< h =< 14, -14 =< k =< 13, -20 =< l =< 20, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) -1 3 0 44.53 0.95 4 9.22 -4 6 0 637.90 1.21 7 167.23 1 -1 1 70.78 1.40 6 13.29 -1 1 1 91.25 1.59 6 14.68 -1 -11 3 34.31 1.18 3 19.86 -1 5 4 643.90 7.11 7 65.64 -4 13 7 7.22 2.20 2 11.04 -5 9 8 56.68 1.03 6 7.11 8 Inconsistent equivalents 8416 Unique reflections, of which 0 suppressed R(int) = 0.0590 R(sigma) = 0.0584 Friedel opposites merged Maximum memory for data reduction = 5750 / 84061 Special position constraints for Cr1 x = 0.0000 y = 0.5000 z = 0.0000 sof = 0.50000 Input constraints retained (at least in part) for sof Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 7382 / 658220 wR2 = 0.0863 before cycle 1 for 8416 data and 498 / 498 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.1230 0.0400 SAME/SADI C21A_e C25A_e C1B_b C8B_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. 450. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.004; Restrained GooF = 0.995 for 450 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.16714 0.00017 0.824 OSF 2 0.86249 0.00274 0.317 FVAR 2 3 0.96840 0.00286 0.552 FVAR 3 4 0.29937 0.00236 -0.251 FVAR 4 5 0.95848 0.00293 0.326 FVAR 5 6 0.94096 0.00285 0.435 FVAR 6 Mean shift/su = 0.109 Maximum = 0.824 for OSF Max. shift = 0.030 A for C24B_f Max. dU = 0.001 for C18A_c Least-squares cycle 2 Maximum vector length = 511 Memory required = 7382 / 658220 wR2 = 0.0862 before cycle 2 for 8416 data and 498 / 498 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.1238 0.0400 SAME/SADI C21A_e C25A_e C1B_b C8B_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. 450. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.003; Restrained GooF = 0.994 for 450 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.16716 0.00017 0.100 OSF 2 0.86285 0.00274 0.130 FVAR 2 3 0.96891 0.00286 0.180 FVAR 3 4 0.29915 0.00236 -0.091 FVAR 4 5 0.95886 0.00293 0.130 FVAR 5 6 0.94146 0.00285 0.176 FVAR 6 Mean shift/su = 0.043 Maximum = -0.226 for x S23A_e Max. shift = 0.028 A for C25B_f Max. dU = 0.000 for C25A_e Least-squares cycle 3 Maximum vector length = 511 Memory required = 7382 / 658220 wR2 = 0.0862 before cycle 3 for 8416 data and 498 / 498 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 0.1238 0.0400 SAME/SADI C21A_e C25A_e C1B_b C8B_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. 450. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.003; Restrained GooF = 0.994 for 450 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.16716 0.00017 -0.004 OSF 2 0.86287 0.00274 0.007 FVAR 2 3 0.96901 0.00286 0.035 FVAR 3 4 0.29915 0.00237 -0.001 FVAR 4 5 0.95890 0.00293 0.016 FVAR 5 6 0.94145 0.00285 -0.005 FVAR 6 Mean shift/su = 0.014 Maximum = -0.165 for x C24B_f Max. shift = 0.021 A for C24B_f Max. dU = 0.000 for C24A_e Least-squares cycle 4 Maximum vector length = 511 Memory required = 7382 / 658220 wR2 = 0.0862 before cycle 4 for 8416 data and 498 / 498 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.1239 0.0400 SAME/SADI C21A_e C25A_e C1B_b C8B_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. 450. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.003; Restrained GooF = 0.994 for 450 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.16716 0.00017 -0.010 OSF 2 0.86289 0.00274 0.007 FVAR 2 3 0.96903 0.00286 0.006 FVAR 3 4 0.29915 0.00237 -0.003 FVAR 4 5 0.95890 0.00293 -0.002 FVAR 5 6 0.94146 0.00286 0.004 FVAR 6 Mean shift/su = 0.008 Maximum = 0.124 for z C25B_f Max. shift = 0.019 A for C25B_f Max. dU = 0.000 for C24A_e Least-squares cycle 5 Maximum vector length = 511 Memory required = 7382 / 658220 wR2 = 0.0862 before cycle 5 for 8416 data and 498 / 498 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 0.1240 0.0400 SAME/SADI C21A_e C25A_e C1B_b C8B_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. 450. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.003; Restrained GooF = 0.994 for 450 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.16716 0.00017 -0.001 OSF 2 0.86288 0.00274 -0.001 FVAR 2 3 0.96905 0.00286 0.008 FVAR 3 4 0.29914 0.00237 0.000 FVAR 4 5 0.95891 0.00293 0.006 FVAR 5 6 0.94145 0.00286 -0.003 FVAR 6 Mean shift/su = 0.007 Maximum = -0.104 for x C25B_f Max. shift = 0.018 A for C25B_f Max. dU = 0.000 for C25A_e Least-squares cycle 6 Maximum vector length = 511 Memory required = 7382 / 658220 wR2 = 0.0862 before cycle 6 for 8416 data and 498 / 498 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint 0.1241 0.0400 SAME/SADI C21A_e C25A_e C1B_b C8B_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. 450. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.003; Restrained GooF = 0.994 for 450 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.16716 0.00017 0.002 OSF 2 0.86289 0.00274 0.001 FVAR 2 3 0.96905 0.00286 -0.001 FVAR 3 4 0.29914 0.00237 -0.001 FVAR 4 5 0.95890 0.00293 -0.004 FVAR 5 6 0.94143 0.00286 -0.007 FVAR 6 Mean shift/su = 0.005 Maximum = -0.112 for x C25B_f Max. shift = 0.019 A for C25B_f Max. dU = 0.000 for C24A_e Least-squares cycle 7 Maximum vector length = 511 Memory required = 7382 / 658220 wR2 = 0.0862 before cycle 7 for 8416 data and 498 / 498 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint 0.1241 0.0400 SAME/SADI C21A_e C25A_e C1B_b C8B_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. 450. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.003; Restrained GooF = 0.994 for 450 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.16716 0.00017 0.001 OSF 2 0.86288 0.00274 -0.001 FVAR 2 3 0.96905 0.00286 0.000 FVAR 3 4 0.29914 0.00237 0.000 FVAR 4 5 0.95891 0.00293 0.001 FVAR 5 6 0.94141 0.00286 -0.009 FVAR 6 Mean shift/su = 0.005 Maximum = -0.111 for x C25B_f Max. shift = 0.019 A for C25B_f Max. dU = 0.000 for C24A_e Least-squares cycle 8 Maximum vector length = 511 Memory required = 7382 / 658220 wR2 = 0.0862 before cycle 8 for 8416 data and 498 / 498 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint 0.1242 0.0400 SAME/SADI C21A_e C25A_e C1B_b C8B_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. 450. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.003; Restrained GooF = 0.994 for 450 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.16716 0.00017 0.002 OSF 2 0.86288 0.00274 0.000 FVAR 2 3 0.96905 0.00286 -0.001 FVAR 3 4 0.29914 0.00237 0.000 FVAR 4 5 0.95890 0.00293 -0.004 FVAR 5 6 0.94139 0.00286 -0.005 FVAR 6 Mean shift/su = 0.004 Maximum = -0.109 for x C25B_f Max. shift = 0.019 A for C25B_f Max. dU = 0.000 for C25A_e Least-squares cycle 9 Maximum vector length = 511 Memory required = 7382 / 658220 wR2 = 0.0862 before cycle 9 for 8416 data and 498 / 498 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint 0.1242 0.0400 SAME/SADI C21A_e C25A_e C1B_b C8B_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. 450. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.003; Restrained GooF = 0.994 for 450 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.16716 0.00017 0.001 OSF 2 0.86288 0.00274 -0.001 FVAR 2 3 0.96905 0.00286 0.000 FVAR 3 4 0.29914 0.00237 0.000 FVAR 4 5 0.95890 0.00293 0.001 FVAR 5 6 0.94138 0.00286 -0.007 FVAR 6 Mean shift/su = 0.004 Maximum = -0.085 for x C25B_f Max. shift = 0.014 A for H25D_f Max. dU = 0.000 for C25A_e Least-squares cycle 10 Maximum vector length = 511 Memory required = 7382 / 658220 wR2 = 0.0862 before cycle 10 for 8416 data and 498 / 498 parameters Disagreeable restraints before cycle 10 Observed Target Error Sigma Restraint 0.1242 0.0400 SAME/SADI C21A_e C25A_e C1B_b C8B_b Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 450. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.003; Restrained GooF = 0.994 for 450 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.16716 0.00017 0.002 OSF 2 0.86288 0.00274 0.000 FVAR 2 3 0.96904 0.00286 -0.002 FVAR 3 4 0.29914 0.00237 -0.001 FVAR 4 5 0.95889 0.00293 -0.002 FVAR 5 6 0.94137 0.00286 -0.003 FVAR 6 Mean shift/su = 0.003 Maximum = -0.066 for x C25B_f Max. shift = 0.011 A for C25B_f Max. dU = 0.000 for C25A_e Least-squares cycle 11 Maximum vector length = 511 Memory required = 7382 / 658220 wR2 = 0.0862 before cycle 11 for 8416 data and 498 / 498 parameters Disagreeable restraints before cycle 11 Observed Target Error Sigma Restraint 0.1242 0.0400 SAME/SADI C21A_e C25A_e C1B_b C8B_b Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 450. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.003; Restrained GooF = 0.994 for 450 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.16716 0.00017 0.001 OSF 2 0.86288 0.00274 -0.001 FVAR 2 3 0.96904 0.00286 0.000 FVAR 3 4 0.29914 0.00237 0.000 FVAR 4 5 0.95889 0.00293 0.000 FVAR 5 6 0.94135 0.00286 -0.004 FVAR 6 Mean shift/su = 0.002 Maximum = -0.038 for x C25B_f Max. shift = 0.006 A for H25D_f Max. dU = 0.000 for C25A_e Least-squares cycle 12 Maximum vector length = 511 Memory required = 7382 / 658220 wR2 = 0.0862 before cycle 12 for 8416 data and 498 / 498 parameters Disagreeable restraints before cycle 12 Observed Target Error Sigma Restraint 0.1242 0.0400 SAME/SADI C21A_e C25A_e C1B_b C8B_b Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 450. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.003; Restrained GooF = 0.993 for 450 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.16716 0.00017 0.001 OSF 2 0.86288 0.00274 0.000 FVAR 2 3 0.96904 0.00286 -0.001 FVAR 3 4 0.29914 0.00237 0.000 FVAR 4 5 0.95889 0.00293 -0.001 FVAR 5 6 0.94135 0.00286 -0.001 FVAR 6 Mean shift/su = 0.001 Maximum = 0.027 for z C25B_f Max. shift = 0.004 A for C25B_f Max. dU = 0.000 for C25A_e Least-squares cycle 13 Maximum vector length = 511 Memory required = 7382 / 658220 wR2 = 0.0862 before cycle 13 for 8416 data and 498 / 498 parameters Disagreeable restraints before cycle 13 Observed Target Error Sigma Restraint 0.1242 0.0400 SAME/SADI C21A_e C25A_e C1B_b C8B_b Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 450. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.003; Restrained GooF = 0.993 for 450 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.16716 0.00017 0.000 OSF 2 0.86288 0.00274 0.000 FVAR 2 3 0.96904 0.00286 0.000 FVAR 3 4 0.29914 0.00237 0.000 FVAR 4 5 0.95889 0.00293 0.000 FVAR 5 6 0.94135 0.00286 -0.001 FVAR 6 Mean shift/su = 0.001 Maximum = -0.013 for x C24B_f Max. shift = 0.002 A for C25B_f Max. dU = 0.000 for C25A_e Least-squares cycle 14 Maximum vector length = 511 Memory required = 7382 / 658220 wR2 = 0.0862 before cycle 14 for 8416 data and 498 / 498 parameters Disagreeable restraints before cycle 14 Observed Target Error Sigma Restraint 0.1242 0.0400 SAME/SADI C21A_e C25A_e C1B_b C8B_b Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 450. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.003; Restrained GooF = 0.994 for 450 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.16716 0.00017 0.001 OSF 2 0.86288 0.00274 0.000 FVAR 2 3 0.96904 0.00286 0.000 FVAR 3 4 0.29914 0.00237 0.000 FVAR 4 5 0.95888 0.00293 -0.001 FVAR 5 6 0.94135 0.00286 0.000 FVAR 6 Mean shift/su = 0.001 Maximum = -0.009 for y C25B_f Max. shift = 0.001 A for C25B_f Max. dU = 0.000 for C25A_e Least-squares cycle 15 Maximum vector length = 511 Memory required = 7382 / 658220 wR2 = 0.0862 before cycle 15 for 8416 data and 498 / 498 parameters Disagreeable restraints before cycle 15 Observed Target Error Sigma Restraint 0.1242 0.0400 SAME/SADI C21A_e C25A_e C1B_b C8B_b Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 450. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.003; Restrained GooF = 0.993 for 450 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.16716 0.00017 0.001 OSF 2 0.86288 0.00274 0.000 FVAR 2 3 0.96904 0.00286 0.000 FVAR 3 4 0.29914 0.00237 0.000 FVAR 4 5 0.95888 0.00293 0.000 FVAR 5 6 0.94135 0.00286 0.000 FVAR 6 Mean shift/su = 0.000 Maximum = -0.005 for x C24B_f Max. shift = 0.001 A for C25B_f Max. dU = 0.000 for C25A_e Least-squares cycle 16 Maximum vector length = 511 Memory required = 7382 / 658220 wR2 = 0.0862 before cycle 16 for 8416 data and 498 / 498 parameters Disagreeable restraints before cycle 16 Observed Target Error Sigma Restraint 0.1242 0.0400 SAME/SADI C21A_e C25A_e C1B_b C8B_b Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 450. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.003; Restrained GooF = 0.993 for 450 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.16716 0.00017 -0.001 OSF 2 0.86288 0.00274 0.000 FVAR 2 3 0.96903 0.00286 0.000 FVAR 3 4 0.29914 0.00237 0.000 FVAR 4 5 0.95888 0.00293 0.000 FVAR 5 6 0.94135 0.00286 0.000 FVAR 6 Mean shift/su = 0.000 Maximum = -0.003 for y C25B_f Max. shift = 0.000 A for H25D_f Max. dU = 0.000 for C25A_e Least-squares cycle 17 Maximum vector length = 511 Memory required = 7382 / 658220 wR2 = 0.0861 before cycle 17 for 8416 data and 498 / 498 parameters Disagreeable restraints before cycle 17 Observed Target Error Sigma Restraint 0.1242 0.0400 SAME/SADI C21A_e C25A_e C1B_b C8B_b Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 450. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.003; Restrained GooF = 0.993 for 450 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.16716 0.00017 0.000 OSF 2 0.86288 0.00274 0.000 FVAR 2 3 0.96904 0.00286 0.000 FVAR 3 4 0.29914 0.00237 0.000 FVAR 4 5 0.95889 0.00293 0.000 FVAR 5 6 0.94135 0.00286 0.000 FVAR 6 Mean shift/su = 0.000 Maximum = -0.002 for x C20B_d Max. shift = 0.000 A for C20B_d Max. dU = 0.000 for C20A_c Least-squares cycle 18 Maximum vector length = 511 Memory required = 7382 / 658220 wR2 = 0.0861 before cycle 18 for 8416 data and 498 / 498 parameters Disagreeable restraints before cycle 18 Observed Target Error Sigma Restraint 0.1242 0.0400 SAME/SADI C21A_e C25A_e C1B_b C8B_b Summary of restraints applied in cycle 18 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 450. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.003; Restrained GooF = 0.993 for 450 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.16716 0.00017 -0.001 OSF 2 0.86288 0.00274 0.000 FVAR 2 3 0.96904 0.00286 0.000 FVAR 3 4 0.29914 0.00237 0.000 FVAR 4 5 0.95888 0.00293 0.000 FVAR 5 6 0.94135 0.00286 0.000 FVAR 6 Mean shift/su = 0.000 Maximum = 0.001 for x C20B_d Max. shift = 0.000 A for C20B_d Max. dU = 0.000 for C17A_c Least-squares cycle 19 Maximum vector length = 511 Memory required = 7382 / 658220 wR2 = 0.0861 before cycle 19 for 8416 data and 498 / 498 parameters Disagreeable restraints before cycle 19 Observed Target Error Sigma Restraint 0.1242 0.0400 SAME/SADI C21A_e C25A_e C1B_b C8B_b Summary of restraints applied in cycle 19 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 450. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.003; Restrained GooF = 0.993 for 450 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.16716 0.00017 0.000 OSF 2 0.86288 0.00274 0.000 FVAR 2 3 0.96904 0.00286 0.000 FVAR 3 4 0.29914 0.00237 0.000 FVAR 4 5 0.95888 0.00293 0.000 FVAR 5 6 0.94135 0.00286 0.000 FVAR 6 Mean shift/su = 0.000 Maximum = 0.001 for z C19B_d Max. shift = 0.000 A for C19B_d Max. dU = 0.000 for C17A_c Least-squares cycle 20 Maximum vector length = 511 Memory required = 7382 / 658220 wR2 = 0.0862 before cycle 20 for 8416 data and 498 / 498 parameters Disagreeable restraints before cycle 20 Observed Target Error Sigma Restraint 0.1242 0.0400 SAME/SADI C21A_e C25A_e C1B_b C8B_b Summary of restraints applied in cycle 20 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 450. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.003; Restrained GooF = 0.993 for 450 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.16716 0.00017 -0.001 OSF 2 0.86288 0.00274 0.000 FVAR 2 3 0.96904 0.00286 0.000 FVAR 3 4 0.29914 0.00237 0.000 FVAR 4 5 0.95888 0.00293 0.000 FVAR 5 6 0.94135 0.00286 0.000 FVAR 6 Mean shift/su = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for C20B_d Max. dU = 0.000 for C17A_c Largest correlation matrix elements -0.976 x C18B_d / x C18A_c -0.901 z C19B_d / y C19B_d -0.852 z C25B_f / x C25B_f -0.943 x C25B_f / x C25A_e -0.889 z C9B_b / y C9B_b -0.844 x C9B_b / x S6A_a -0.943 x C8B_b / x C8A_a 0.875 x C25B_f / U12 C25A_e 0.843 y C10B_b / y S6B_b -0.936 x S23B_f / x C24A_e -0.874 z C9B_b / x C9B_b -0.843 x C7B_b / x S5A_a -0.926 x S16B_d / x C19A_c -0.864 x C20B_d / x C20A_c -0.841 z C10B_b / x C10B_b 0.920 U12 C18A_c / x C18A_c -0.864 x C19B_d / x S16A_c -0.835 x S23B_f / U12 C24A_e -0.909 x C18B_d / U12 C18A_c -0.856 y C18B_d / y C18A_c -0.831 z C18B_d / z C18A_c -0.906 x C24B_f / x S23A_e -0.853 z C24B_f / y C24B_f -0.831 U12 C25A_e / x C25A_e Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H8A1 0.4158 0.6137 0.8724 23 0.990 0.000 C8A_a C7A_a S5A_a H8A2 0.2746 0.5836 0.9049 23 0.990 0.000 C8A_a C7A_a S5A_a H7A1 0.4342 0.4419 0.8145 23 0.990 0.000 C7A_a C2A_a C8A_a H7A2 0.2875 0.4276 0.8297 23 0.990 0.000 C7A_a C2A_a C8A_a H10A 0.3911 0.5285 0.1126 23 0.990 0.000 C10A_a C9A_a S6A_a H10B 0.2492 0.4975 0.1167 23 0.990 0.000 C10A_a C9A_a S6A_a H9A1 0.3242 0.6883 0.1795 23 0.990 0.000 C9A_a C6A_a C10A_a H9A2 0.1868 0.6400 0.2017 23 0.990 0.000 C9A_a C6A_a C10A_a H8B1 0.2948 0.6153 0.9009 23 0.990 0.000 C8B_b C7B_b S5B_b H8B2 0.4290 0.6449 0.8507 23 0.990 0.000 C8B_b C7B_b S5B_b H7B1 0.1978 0.7119 0.7888 23 0.990 0.000 C7B_b C2B_b C8B_b H7B2 0.3241 0.7816 0.7626 23 0.990 0.000 C7B_b C2B_b C8B_b H10C 0.2038 0.4637 0.1539 23 0.990 0.000 C10B_b C9B_b S6B_b H10D 0.3435 0.4697 0.1076 23 0.990 0.000 C10B_b C9B_b S6B_b H9B1 0.2762 0.3197 0.2534 23 0.990 0.000 C9B_b C6B_b C10B_b H9B2 0.4167 0.3548 0.2223 23 0.990 0.000 C9B_b C6B_b C10B_b H18A 0.1951 0.1298 0.9146 23 0.990 0.000 C18A_c C17A_c S15A_c H18B 0.0565 0.0922 0.9127 23 0.990 0.000 C18A_c C17A_c S15A_c H17A 0.2717 -0.0050 0.8274 23 0.990 0.000 C17A_c C12A_c C18A_c H17B 0.1375 -0.0600 0.8430 23 0.990 0.000 C17A_c C12A_c C18A_c H20A 0.2142 0.1017 0.1297 23 0.990 0.000 C20A_c C19A_c S16A_c H20B 0.0772 0.0595 0.1279 23 0.990 0.000 C20A_c C19A_c S16A_c H19A 0.1229 0.2508 0.2003 23 0.990 0.000 C19A_c C16A_c C20A_c H19B -0.0051 0.1835 0.2230 23 0.990 0.000 C19A_c C16A_c C20A_c H18C 0.0744 0.1250 0.9228 23 0.990 0.000 C18B_d C17B_d S15B_d H18D 0.2121 0.1685 0.8939 23 0.990 0.000 C18B_d C17B_d S15B_d H17C 0.0041 0.2436 0.8094 23 0.990 0.000 C17B_d C12B_d C18B_d H17D 0.1349 0.3059 0.7934 23 0.990 0.000 C17B_d C12B_d C18B_d H20C 0.0826 0.0143 0.1367 23 0.990 0.000 C20B_d C19B_d S16B_d H20D 0.2197 0.0585 0.1345 23 0.990 0.000 C20B_d C19B_d S16B_d H19C 0.0966 -0.1131 0.2610 23 0.990 0.000 C19B_d C16B_d C20B_d H19D 0.2430 -0.0972 0.2407 23 0.990 0.000 C19B_d C16B_d C20B_d H25A 0.5634 -0.0337 0.0991 23 0.990 0.000 C25A_e C24A_e S23A_e H25B 0.4205 -0.0632 0.1238 23 0.990 0.000 C25A_e C24A_e S23A_e H24A 0.5360 0.1253 0.1719 23 0.990 0.000 C24A_e C22A_e C25A_e H24B 0.3909 0.1022 0.1897 23 0.990 0.000 C24A_e C22A_e C25A_e H25C 0.4209 -0.1001 0.1374 23 0.990 0.000 C25B_f C24B_f S23B_f H25D 0.5628 -0.0731 0.1054 23 0.990 0.000 C25B_f C24B_f S23B_f H24C 0.4850 -0.2344 0.2451 23 0.990 0.000 C24B_f C22B_f C25B_f H24D 0.6238 -0.1901 0.2228 23 0.990 0.000 C24B_f C22B_f C25B_f s92 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Cr1 0.00000 0.50000 0.00000 0.50000 0.01732 0.01743 0.01660 -0.00453 -0.00168 0.00111 0.01702 0.00000 0.00000 0.00000 0.00000 0.00000 0.00030 0.00030 0.00030 0.00022 0.00023 0.00022 0.00014 S31 0.22074 0.84848 0.02660 1.00000 0.04977 0.02567 0.02914 0.00305 -0.01324 -0.01529 0.03418 0.00107 0.00007 0.00006 0.00005 0.00000 0.00048 0.00038 0.00041 0.00029 0.00035 0.00033 0.00019 S32 0.01496 0.52565 -0.31012 1.00000 0.02764 0.03541 0.01820 -0.00099 -0.00549 0.00344 0.02734 0.00105 0.00006 0.00006 0.00004 0.00000 0.00038 0.00040 0.00036 0.00028 0.00028 0.00030 0.00017 S33 -0.38627 0.73129 -0.00692 1.00000 0.02433 0.02931 0.02566 -0.00288 -0.00649 0.00925 0.02671 0.00106 0.00006 0.00006 0.00004 0.00000 0.00037 0.00038 0.00038 0.00028 0.00029 0.00028 0.00016 N31 0.09243 0.64815 0.00571 1.00000 0.02133 0.02322 0.02176 -0.00560 0.00000 -0.00027 0.02211 0.00322 0.00019 0.00019 0.00013 0.00000 0.00117 0.00121 0.00119 0.00089 0.00091 0.00093 0.00047 N32 0.02292 0.52706 -0.13113 1.00000 0.02050 0.01896 0.02444 -0.00367 -0.00286 0.00314 0.02141 0.00323 0.00018 0.00018 0.00014 0.00000 0.00116 0.00114 0.00132 0.00091 0.00094 0.00087 0.00047 N33 -0.15675 0.60502 -0.00067 1.00000 0.02090 0.02073 0.01874 -0.00487 -0.00058 -0.00085 0.02007 0.00305 0.00019 0.00018 0.00013 0.00000 0.00117 0.00113 0.00115 0.00085 0.00089 0.00091 0.00045 C31 0.14507 0.73181 0.01441 1.00000 0.02429 0.02415 0.01366 0.00041 -0.00346 0.00372 0.02113 0.00396 0.00023 0.00023 0.00015 0.00000 0.00143 0.00144 0.00132 0.00101 0.00105 0.00113 0.00056 C32 0.01952 0.52674 -0.20583 1.00000 0.01258 0.01865 0.02883 -0.00052 -0.00358 0.00472 0.02045 0.00397 0.00021 0.00022 0.00018 0.00000 0.00126 0.00134 0.00165 0.00107 0.00108 0.00098 0.00056 C33 -0.25153 0.65901 -0.00339 1.00000 0.02382 0.01746 0.01553 -0.00313 -0.00118 -0.00178 0.01892 0.00364 0.00023 0.00021 0.00015 0.00000 0.00143 0.00128 0.00131 0.00096 0.00105 0.00108 0.00053 S1 0.28912 0.69583 0.58245 1.00000 0.03142 0.01494 0.01746 -0.00141 -0.00527 -0.00009 0.02120 0.00095 0.00006 0.00005 0.00004 0.00000 0.00037 0.00032 0.00034 0.00024 0.00027 0.00026 0.00015 S2 0.36065 0.43593 0.62633 1.00000 0.02992 0.01567 0.01696 -0.00196 -0.00461 0.00163 0.02085 0.00096 0.00006 0.00005 0.00004 0.00000 0.00037 0.00032 0.00033 0.00024 0.00027 0.00026 0.00015 S3 0.34570 0.39820 0.42472 1.00000 0.03028 0.01530 0.01742 -0.00222 -0.00589 0.00199 0.02088 0.00095 0.00006 0.00005 0.00004 0.00000 0.00037 0.00032 0.00034 0.00024 0.00027 0.00026 0.00015 S4 0.27806 0.65956 0.38255 1.00000 0.03843 0.01482 0.01800 -0.00317 -0.00850 0.00246 0.02339 0.00097 0.00006 0.00005 0.00004 0.00000 0.00040 0.00033 0.00034 0.00024 0.00029 0.00027 0.00015 C3 0.32249 0.55474 0.54639 1.00000 0.02290 0.01561 0.02028 -0.00157 -0.00355 -0.00095 0.01960 0.00372 0.00023 0.00021 0.00016 0.00000 0.00136 0.00127 0.00137 0.00098 0.00105 0.00100 0.00053 C4 0.31618 0.53946 0.46092 1.00000 0.02407 0.01718 0.01879 -0.00183 -0.00359 -0.00099 0.01999 0.00375 0.00023 0.00022 0.00016 0.00000 0.00140 0.00130 0.00139 0.00099 0.00107 0.00103 0.00054 C2A_a 0.34646 0.52465 0.71029 0.86288 0.01849 0.01951 0.01769 -0.00225 -0.00056 -0.00219 0.01868 0.00362 0.00022 0.00021 0.00015 0.00274 0.00131 0.00136 0.00133 0.00100 0.00102 0.00101 0.00053 C1A_a 0.31268 0.64266 0.68949 0.86288 0.01917 0.01882 0.01815 -0.00253 -0.00155 -0.00250 0.01871 0.00362 0.00022 0.00021 0.00015 0.00274 0.00132 0.00133 0.00134 0.00100 0.00103 0.00100 0.00053 S5A_a 0.28538 0.72823 0.77631 0.86288 0.03294 0.01534 0.01858 -0.00408 -0.00512 0.00105 0.02204 0.00159 0.00013 0.00007 0.00006 0.00274 0.00050 0.00054 0.00044 0.00032 0.00034 0.00048 0.00027 C8A_a 0.33671 0.59731 0.85268 0.86288 0.02239 0.01841 0.01467 -0.00057 0.00068 -0.00044 0.01894 0.00847 0.00081 0.00032 0.00026 0.00274 0.00231 0.00170 0.00161 0.00128 0.00161 0.00193 0.00109 H8A1_a 0.41582 0.61374 0.87236 0.86288 0.02273 0.00274 0.00000 H8A2_a 0.27458 0.58358 0.90490 0.86288 0.02273 0.00274 0.00000 C7A_a 0.35327 0.48438 0.80571 0.86288 0.02640 0.01563 0.01906 -0.00092 -0.00164 -0.00247 0.02054 0.00849 0.00050 0.00042 0.00031 0.00274 0.00234 0.00276 0.00209 0.00168 0.00153 0.00190 0.00107 H7A1_a 0.43416 0.44192 0.81449 0.86288 0.02465 0.00274 0.00000 H7A2_a 0.28752 0.42763 0.82969 0.86288 0.02465 0.00274 0.00000 C6A_a 0.29930 0.57404 0.29635 0.96904 0.02425 0.01849 0.01780 -0.00317 -0.00531 -0.00239 0.01981 0.00362 0.00023 0.00021 0.00016 0.00286 0.00138 0.00134 0.00135 0.00100 0.00106 0.00104 0.00054 C5A_a 0.32959 0.45527 0.31636 0.96904 0.02122 0.02113 0.01646 -0.00394 -0.00419 -0.00063 0.01932 0.00362 0.00022 0.00022 0.00016 0.00286 0.00135 0.00137 0.00130 0.00099 0.00103 0.00103 0.00053 S6A_a 0.34195 0.37061 0.22921 0.96904 0.02675 0.01797 0.01929 -0.00638 -0.00348 -0.00026 0.02093 0.00151 0.00011 0.00007 0.00005 0.00286 0.00047 0.00039 0.00040 0.00026 0.00033 0.00034 0.00023 C10A_a 0.31470 0.50993 0.15258 0.96904 0.02701 0.02811 0.01785 -0.00519 -0.00725 0.00301 0.02393 0.00417 0.00029 0.00026 0.00017 0.00286 0.00194 0.00159 0.00144 0.00112 0.00122 0.00129 0.00074 H10A_a 0.39107 0.52848 0.11257 0.96904 0.02871 0.00286 0.00000 H10B_a 0.24917 0.49746 0.11673 0.96904 0.02871 0.00286 0.00000 C9A_a 0.27545 0.61692 0.20422 0.96904 0.03058 0.01934 0.01464 -0.00096 -0.00405 -0.00505 0.02136 0.00571 0.00043 0.00034 0.00022 0.00286 0.00236 0.00174 0.00155 0.00117 0.00153 0.00145 0.00090 H9A1_a 0.32417 0.68831 0.17951 0.96904 0.02564 0.00286 0.00000 H9A2_a 0.18682 0.64005 0.20174 0.96904 0.02564 0.00286 0.00000 C2B_b 0.31268 0.64266 0.68949 0.13712 0.01917 0.01882 0.01815 -0.00253 -0.00155 -0.00250 0.01871 0.00362 0.00022 0.00021 0.00015 0.00274 0.00132 0.00133 0.00134 0.00100 0.00103 0.00100 0.00053 C1B_b 0.34646 0.52465 0.71029 0.13712 0.01849 0.01951 0.01769 -0.00225 -0.00056 -0.00219 0.01868 0.00362 0.00022 0.00021 0.00015 0.00274 0.00131 0.00136 0.00133 0.00100 0.00102 0.00101 0.00053 S5B_b 0.36840 0.45695 0.81528 0.13712 0.03294 0.01534 0.01858 -0.00408 -0.00512 0.00105 0.02204 0.01736 0.00102 0.00087 0.00061 0.00274 0.00050 0.00054 0.00044 0.00032 0.00034 0.00048 0.00027 C8B_b 0.34780 0.61531 0.84419 0.13712 0.02239 0.01841 0.01467 -0.00057 0.00068 -0.00044 0.01894 0.05880 0.00601 0.00193 0.00179 0.00274 0.00231 0.00170 0.00161 0.00128 0.00161 0.00193 0.00109 H8B1_b 0.29480 0.61527 0.90085 0.13712 0.02273 0.00274 0.00000 H8B2_b 0.42904 0.64490 0.85068 0.13712 0.02273 0.00274 0.00000 C7B_b 0.28781 0.70099 0.77185 0.13712 0.02640 0.01563 0.01906 -0.00092 -0.00164 -0.00247 0.02054 0.04948 0.00385 0.00206 0.00127 0.00274 0.00234 0.00276 0.00209 0.00168 0.00153 0.00190 0.00107 H7B1_b 0.19781 0.71190 0.78884 0.13712 0.02465 0.00274 0.00000 H7B2_b 0.32405 0.78158 0.76265 0.13712 0.02465 0.00274 0.00000 C6B_b 0.32959 0.45527 0.31636 0.03096 0.02122 0.02113 0.01646 -0.00394 -0.00419 -0.00063 0.01932 0.00362 0.00022 0.00022 0.00016 0.00286 0.00135 0.00137 0.00130 0.00099 0.00103 0.00103 0.00053 C5B_b 0.29930 0.57404 0.29635 0.03096 0.02425 0.01849 0.01780 -0.00317 -0.00531 -0.00239 0.01981 0.00362 0.00023 0.00021 0.00016 0.00286 0.00138 0.00134 0.00135 0.00100 0.00106 0.00104 0.00054 S6B_b 0.29498 0.63667 0.18860 0.03096 0.02675 0.01797 0.01929 -0.00638 -0.00348 -0.00026 0.02093 0.05439 0.00428 0.00248 0.00120 0.00286 0.00047 0.00039 0.00040 0.00026 0.00033 0.00034 0.00023 C10B_b 0.28913 0.47936 0.16251 0.03096 0.02701 0.02811 0.01785 -0.00519 -0.00725 0.00301 0.02393 0.09918 0.01172 0.00322 0.00288 0.00286 0.00194 0.00159 0.00144 0.00112 0.00122 0.00129 0.00074 H10C_b 0.20379 0.46366 0.15388 0.03096 0.02871 0.00286 0.00000 H10D_b 0.34350 0.46970 0.10763 0.03096 0.02871 0.00286 0.00000 C9B_b 0.33209 0.38797 0.23889 0.03096 0.03058 0.01934 0.01464 -0.00096 -0.00405 -0.00505 0.02136 0.17125 0.01714 0.00376 0.00352 0.00286 0.00236 0.00174 0.00155 0.00117 0.00153 0.00145 0.00090 H9B1_b 0.27624 0.31971 0.25341 0.03096 0.02564 0.00286 0.00000 H9B2_b 0.41670 0.35475 0.22232 0.03096 0.02564 0.00286 0.00000 S11 0.09985 0.23172 0.60839 1.00000 0.02438 0.02431 0.02080 -0.00581 -0.00566 0.00713 0.02302 0.00100 0.00006 0.00006 0.00004 0.00000 0.00036 0.00035 0.00035 0.00026 0.00027 0.00027 0.00015 S12 0.19079 -0.02497 0.63882 1.00000 0.02286 0.01971 0.01786 -0.00257 -0.00321 -0.00102 0.02008 0.00094 0.00006 0.00006 0.00004 0.00000 0.00034 0.00033 0.00034 0.00025 0.00026 0.00025 0.00014 S13 0.18362 -0.04875 0.43527 1.00000 0.02355 0.01851 0.01818 -0.00235 -0.00258 -0.00192 0.02005 0.00093 0.00006 0.00005 0.00004 0.00000 0.00034 0.00033 0.00034 0.00025 0.00026 0.00025 0.00014 S14 0.09176 0.20792 0.40387 1.00000 0.02474 0.02383 0.01921 -0.00504 -0.00658 0.00650 0.02240 0.00097 0.00006 0.00006 0.00004 0.00000 0.00036 0.00035 0.00034 0.00026 0.00027 0.00027 0.00015 C13 0.14412 0.09709 0.56469 1.00000 0.01399 0.02243 0.02108 -0.00158 -0.00294 0.00106 0.01933 0.00376 0.00021 0.00022 0.00016 0.00000 0.00126 0.00136 0.00136 0.00104 0.00102 0.00101 0.00054 C14 0.14086 0.08711 0.47756 1.00000 0.01648 0.02155 0.01921 -0.00125 -0.00404 -0.00024 0.01910 0.00369 0.00021 0.00022 0.00016 0.00000 0.00130 0.00134 0.00137 0.00101 0.00103 0.00101 0.00053 C12A_c 0.16732 0.05491 0.72790 0.29914 0.01412 0.02697 0.01822 -0.00406 -0.00361 -0.00175 0.01949 0.00362 0.00021 0.00022 0.00016 0.00237 0.00127 0.00146 0.00136 0.00104 0.00101 0.00103 0.00054 C11A_c 0.12695 0.17197 0.71444 0.29914 0.01550 0.02650 0.02285 -0.00797 -0.00437 0.00203 0.02112 0.00369 0.00022 0.00022 0.00016 0.00237 0.00129 0.00146 0.00143 0.00107 0.00105 0.00104 0.00055 S15A_c 0.10433 0.25799 0.80085 0.29914 0.02054 0.02308 0.01528 -0.00424 -0.00317 0.00114 0.01949 0.00566 0.00038 0.00040 0.00027 0.00237 0.00058 0.00069 0.00056 0.00039 0.00044 0.00049 0.00031 C18A_c 0.13393 0.11615 0.87564 0.29914 0.03157 0.02109 0.02099 -0.00737 -0.00388 0.00212 0.02419 0.05447 0.00423 0.00166 0.00095 0.00237 0.00234 0.00284 0.00157 0.00155 0.00137 0.00323 0.00143 H18A_c 0.19514 0.12975 0.91459 0.29914 0.02903 0.00237 0.00000 H18B_c 0.05654 0.09222 0.91269 0.29914 0.02903 0.00237 0.00000 C17A_c 0.18322 0.01432 0.82136 0.29914 0.03230 0.03666 0.03779 -0.00190 -0.01198 -0.01639 0.03455 0.03043 0.00191 0.00147 0.00080 0.00237 0.00299 0.00422 0.00307 0.00257 0.00213 0.00263 0.00188 H17A_c 0.27169 -0.00496 0.82742 0.29914 0.04146 0.00237 0.00000 H17B_c 0.13752 -0.05998 0.84300 0.29914 0.04146 0.00237 0.00000 C16A_c 0.11640 0.12918 0.31445 0.95888 0.01381 0.02445 0.02154 -0.00289 -0.00350 -0.00157 0.01981 0.00366 0.00021 0.00022 0.00016 0.00293 0.00126 0.00142 0.00139 0.00104 0.00103 0.00102 0.00054 C15A_c 0.15776 0.01198 0.32919 0.95888 0.01565 0.02300 0.01928 -0.00309 -0.00334 -0.00369 0.01906 0.00358 0.00021 0.00021 0.00016 0.00293 0.00127 0.00140 0.00134 0.00102 0.00102 0.00103 0.00054 S16A_c 0.17328 -0.06802 0.23938 0.95888 0.02917 0.02150 0.01974 -0.00471 -0.00214 -0.00545 0.02316 0.00171 0.00013 0.00007 0.00005 0.00293 0.00053 0.00041 0.00042 0.00027 0.00037 0.00035 0.00024 C20A_c 0.13807 0.07417 0.16682 0.95888 0.02107 0.02691 0.01858 -0.00306 -0.00252 0.00058 0.02226 0.00637 0.00048 0.00026 0.00018 0.00293 0.00142 0.00182 0.00141 0.00116 0.00113 0.00182 0.00067 H20A_c 0.21417 0.10173 0.12970 0.95888 0.02671 0.00293 0.00000 H20B_c 0.07724 0.05945 0.12792 0.95888 0.02671 0.00293 0.00000 C19A_c 0.08546 0.17235 0.22327 0.95888 0.01972 0.02346 0.01990 -0.00068 -0.00764 -0.00042 0.02083 0.00971 0.00067 0.00049 0.00029 0.00293 0.00208 0.00213 0.00187 0.00146 0.00150 0.00149 0.00081 H19A_c 0.12294 0.25081 0.20026 0.95888 0.02499 0.00293 0.00000 H19B_c -0.00509 0.18354 0.22304 0.95888 0.02499 0.00293 0.00000 C12B_d 0.12695 0.17197 0.71444 0.70086 0.01550 0.02650 0.02285 -0.00797 -0.00437 0.00203 0.02112 0.00369 0.00022 0.00022 0.00016 0.00237 0.00129 0.00146 0.00143 0.00107 0.00105 0.00104 0.00055 C11B_d 0.16732 0.05491 0.72790 0.70086 0.01412 0.02697 0.01822 -0.00406 -0.00361 -0.00175 0.01949 0.00362 0.00021 0.00022 0.00016 0.00237 0.00127 0.00146 0.00136 0.00104 0.00101 0.00103 0.00054 S15B_d 0.18669 -0.01155 0.83475 0.70086 0.02054 0.02308 0.01528 -0.00424 -0.00317 0.00114 0.01949 0.00268 0.00015 0.00013 0.00007 0.00237 0.00058 0.00069 0.00056 0.00039 0.00044 0.00049 0.00031 C18B_d 0.14069 0.13624 0.87304 0.70086 0.03157 0.02109 0.02099 -0.00737 -0.00388 0.00212 0.02419 0.02022 0.00167 0.00064 0.00043 0.00237 0.00234 0.00284 0.00157 0.00155 0.00137 0.00323 0.00143 H18C_d 0.07436 0.12503 0.92280 0.70086 0.02903 0.00237 0.00000 H18D_d 0.21214 0.16846 0.89386 0.70086 0.02903 0.00237 0.00000 C17B_d 0.09446 0.22794 0.79812 0.70086 0.03230 0.03666 0.03779 -0.00190 -0.01198 -0.01639 0.03455 0.00929 0.00066 0.00060 0.00045 0.00237 0.00299 0.00422 0.00307 0.00257 0.00213 0.00263 0.00188 H17C_d 0.00405 0.24363 0.80944 0.70086 0.04146 0.00237 0.00000 H17D_d 0.13492 0.30587 0.79338 0.70086 0.04146 0.00237 0.00000 C16B_d 0.15776 0.01198 0.32919 0.04112 0.01565 0.02300 0.01928 -0.00309 -0.00334 -0.00369 0.01906 0.00358 0.00021 0.00021 0.00016 0.00293 0.00127 0.00140 0.00134 0.00102 0.00102 0.00103 0.00054 C15B_d 0.11640 0.12918 0.31445 0.04112 0.01381 0.02445 0.02154 -0.00289 -0.00350 -0.00157 0.01981 0.00366 0.00021 0.00022 0.00016 0.00293 0.00126 0.00142 0.00139 0.00104 0.00103 0.00102 0.00054 S16B_d 0.07587 0.18652 0.21228 0.04112 0.02917 0.02150 0.01974 -0.00471 -0.00214 -0.00545 0.02316 0.06272 0.00469 0.00291 0.00153 0.00293 0.00053 0.00041 0.00042 0.00027 0.00037 0.00035 0.00024 C20B_d 0.14059 0.04351 0.17214 0.04112 0.02107 0.02691 0.01858 -0.00306 -0.00252 0.00058 0.02226 0.16642 0.01302 0.00528 0.00210 0.00293 0.00142 0.00182 0.00141 0.00116 0.00113 0.00182 0.00067 H20C_d 0.08260 0.01431 0.13667 0.04112 0.02671 0.00293 0.00000 H20D_d 0.21971 0.05852 0.13454 0.04112 0.02671 0.00293 0.00000 C19B_d 0.16181 -0.05343 0.25127 0.04112 0.01972 0.02346 0.01990 -0.00068 -0.00764 -0.00042 0.02083 0.14268 0.01337 0.00395 0.00295 0.00293 0.00208 0.00213 0.00187 0.00146 0.00150 0.00149 0.00081 H19C_d 0.09664 -0.11310 0.26104 0.04112 0.02499 0.00293 0.00000 H19D_d 0.24295 -0.09722 0.24069 0.04112 0.02499 0.00293 0.00000 S21 0.53453 -0.15008 0.42150 1.00000 0.02202 0.01333 0.01635 -0.00226 -0.00379 0.00131 0.01719 0.00090 0.00006 0.00005 0.00004 0.00000 0.00033 0.00031 0.00033 0.00023 0.00025 0.00024 0.00014 S22 0.46545 0.11232 0.37566 1.00000 0.02240 0.01301 0.01555 -0.00208 -0.00439 0.00151 0.01690 0.00090 0.00006 0.00005 0.00004 0.00000 0.00033 0.00030 0.00032 0.00023 0.00025 0.00024 0.00014 C23 0.49974 -0.00777 0.45739 1.00000 0.01656 0.01591 0.01709 -0.00193 -0.00312 0.00080 0.01653 0.00361 0.00021 0.00021 0.00015 0.00000 0.00125 0.00123 0.00123 0.00095 0.00099 0.00095 0.00050 C22A_e 0.48630 0.02249 0.29100 0.94135 0.01672 0.01558 0.01576 -0.00310 -0.00193 -0.00107 0.01592 0.00349 0.00021 0.00020 0.00015 0.00286 0.00126 0.00126 0.00128 0.00093 0.00099 0.00096 0.00050 C21A_e 0.51721 -0.09514 0.31264 0.94135 0.01647 0.01808 0.01547 -0.00455 -0.00234 -0.00108 0.01640 0.00349 0.00021 0.00020 0.00015 0.00286 0.00126 0.00131 0.00126 0.00095 0.00098 0.00098 0.00051 S23A_e 0.53987 -0.18169 0.22595 0.94135 0.02934 0.01577 0.01780 -0.00508 -0.00479 0.00059 0.02060 0.00181 0.00015 0.00007 0.00005 0.00286 0.00045 0.00043 0.00041 0.00026 0.00035 0.00043 0.00023 C25A_e 0.49650 -0.04804 0.14821 0.94135 0.02534 0.02386 0.01547 -0.00353 -0.00437 0.00033 0.02138 0.00821 0.00076 0.00027 0.00020 0.00286 0.00145 0.00172 0.00143 0.00124 0.00135 0.00231 0.00069 H25A_e 0.56336 -0.03370 0.09909 0.94135 0.02566 0.00286 0.00000 H25B_e 0.42055 -0.06317 0.12376 0.94135 0.02566 0.00286 0.00000 C24A_e 0.47435 0.06446 0.19641 0.94135 0.02078 0.01813 0.01823 -0.00088 -0.00504 -0.00364 0.01885 0.01010 0.00072 0.00046 0.00029 0.00286 0.00181 0.00241 0.00192 0.00136 0.00169 0.00200 0.00090 H24A_e 0.53598 0.12531 0.17192 0.94135 0.02262 0.00286 0.00000 H24B_e 0.39089 0.10219 0.18967 0.94135 0.02262 0.00286 0.00000 C22B_f 0.51721 -0.09514 0.31264 0.05865 0.01647 0.01808 0.01547 -0.00455 -0.00234 -0.00108 0.01640 0.00349 0.00021 0.00020 0.00015 0.00286 0.00126 0.00131 0.00126 0.00095 0.00098 0.00098 0.00051 C21B_f 0.48630 0.02249 0.29100 0.05865 0.01672 0.01558 0.01576 -0.00310 -0.00193 -0.00107 0.01592 0.00349 0.00021 0.00020 0.00015 0.00286 0.00126 0.00126 0.00128 0.00093 0.00099 0.00096 0.00050 S23B_f 0.46898 0.08326 0.18513 0.05865 0.02934 0.01577 0.01780 -0.00508 -0.00479 0.00059 0.02060 0.04835 0.00355 0.00216 0.00112 0.00286 0.00045 0.00043 0.00041 0.00026 0.00035 0.00043 0.00023 C25B_f 0.49703 -0.07321 0.15550 0.05865 0.02534 0.02386 0.01547 -0.00353 -0.00437 0.00033 0.02138 0.14658 0.01413 0.00367 0.00274 0.00286 0.00145 0.00172 0.00143 0.00124 0.00135 0.00231 0.00069 H25C_f 0.42089 -0.10010 0.13739 0.05865 0.02566 0.00286 0.00000 H25D_f 0.56282 -0.07315 0.10541 0.05865 0.02566 0.00286 0.00000 C24B_f 0.53605 -0.16244 0.23443 0.05865 0.02078 0.01813 0.01823 -0.00088 -0.00504 -0.00364 0.01885 0.12665 0.01082 0.00350 0.00211 0.00286 0.00181 0.00241 0.00192 0.00136 0.00169 0.00200 0.00090 H24C_f 0.48502 -0.23441 0.24510 0.05865 0.02262 0.00286 0.00000 H24D_f 0.62378 -0.19009 0.22278 0.05865 0.02262 0.00286 0.00000 Final Structure Factor Calculation for s92 in P-1 Total number of l.s. parameters = 498 Maximum vector length = 511 Memory required = 6884 / 24017 wR2 = 0.0862 before cycle 21 for 8416 data and 0 / 498 parameters Disagreeable restraints before cycle 21 Observed Target Error Sigma Restraint 0.1242 0.0400 SAME/SADI C21A_e C25A_e C1B_b C8B_b Summary of restraints applied in cycle 21 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 450. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.003; Restrained GooF = 0.993 for 450 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0379 for 5705 Fo > 4sig(Fo) and 0.0749 for all 8416 data wR2 = 0.0862, GooF = S = 1.003, Restrained GooF = 0.993 for all data Occupancy sum of asymmetric unit = 49.50 for non-hydrogen and 20.00 for hydrogen atoms Principal mean square atomic displacements U 0.0198 0.0174 0.0139 Cr1 0.0586 0.0250 0.0189 S31 0.0388 0.0266 0.0167 S32 0.0383 0.0264 0.0154 S33 0.0252 0.0232 0.0180 N31 0.0245 0.0240 0.0157 N32 0.0225 0.0210 0.0167 N33 0.0302 0.0207 0.0125 C31 0.0303 0.0218 0.0093 C32 0.0242 0.0175 0.0151 C33 0.0317 0.0173 0.0146 S1 0.0306 0.0169 0.0150 S2 0.0313 0.0167 0.0147 S3 0.0397 0.0161 0.0144 S4 0.0231 0.0201 0.0155 C3 0.0242 0.0188 0.0170 C4 0.0205 0.0192 0.0164 C2A_a 0.0206 0.0183 0.0173 C1A_a 0.0334 0.0184 0.0143 S5A_a 0.0243 0.0188 0.0137 C8A_a 0.0267 0.0199 0.0150 C7A_a 0.0252 0.0188 0.0154 C6A_a 0.0222 0.0208 0.0150 C5A_a 0.0269 0.0218 0.0141 S6A_a 0.0328 0.0238 0.0152 C10A_a 0.0317 0.0182 0.0143 C9A_a 0.0206 0.0183 0.0173 C2B_b 0.0205 0.0192 0.0164 C1B_b 0.0334 0.0184 0.0143 S5B_b 0.0243 0.0188 0.0137 C8B_b 0.0267 0.0199 0.0150 C7B_b 0.0222 0.0208 0.0150 C6B_b 0.0252 0.0188 0.0154 C5B_b 0.0269 0.0218 0.0141 S6B_b 0.0328 0.0238 0.0152 C10B_b 0.0317 0.0182 0.0143 C9B_b 0.0335 0.0192 0.0164 S11 0.0229 0.0197 0.0176 S12 0.0237 0.0184 0.0181 S13 0.0328 0.0183 0.0160 S14 0.0240 0.0206 0.0134 C13 0.0226 0.0196 0.0151 C14 0.0270 0.0185 0.0130 C12A_c 0.0298 0.0190 0.0146 C11A_c 0.0246 0.0193 0.0145 S15A_c 0.0328 0.0239 0.0158 C18A_c 0.0525 0.0350 0.0161 C17A_c 0.0245 0.0216 0.0132 C16A_c 0.0238 0.0195 0.0139 C15A_c 0.0310 0.0210 0.0174 S16A_c 0.0276 0.0207 0.0185 C20A_c 0.0257 0.0231 0.0137 C19A_c 0.0298 0.0190 0.0146 C12B_d 0.0270 0.0185 0.0130 C11B_d 0.0246 0.0193 0.0145 S15B_d 0.0328 0.0239 0.0158 C18B_d 0.0525 0.0350 0.0161 C17B_d 0.0238 0.0195 0.0139 C16B_d 0.0245 0.0216 0.0132 C15B_d 0.0310 0.0210 0.0174 S16B_d 0.0276 0.0207 0.0185 C20B_d 0.0257 0.0231 0.0137 C19B_d 0.0228 0.0159 0.0129 S21 0.0233 0.0149 0.0125 S22 0.0182 0.0171 0.0143 C23 0.0168 0.0164 0.0145 C22A_e 0.0191 0.0166 0.0136 C21A_e 0.0298 0.0186 0.0133 S23A_e 0.0265 0.0230 0.0147 C25A_e 0.0240 0.0167 0.0158 C24A_e 0.0191 0.0166 0.0136 C22B_f 0.0168 0.0164 0.0145 C21B_f 0.0298 0.0186 0.0133 S23B_f 0.0265 0.0230 0.0147 C25B_f 0.0240 0.0167 0.0158 C24B_f Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.017 0.026 0.036 0.046 0.059 0.076 0.100 0.147 1.000 Number in group 932. 830. 835. 848. 779. 861. 833. 821. 831. 846. GooF 0.854 0.914 0.948 1.046 1.079 1.013 1.101 1.075 1.015 0.981 K 2.275 1.081 0.971 0.972 0.981 1.001 1.008 0.990 0.999 1.010 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.63 inf Number in group 851. 831. 846. 838. 856. 829. 839. 847. 833. 846. GooF 0.890 0.881 0.920 0.910 0.957 0.969 1.028 1.051 1.000 1.341 K 1.009 1.032 1.026 0.997 1.012 1.009 1.021 1.011 0.997 1.000 R1 0.196 0.145 0.123 0.096 0.080 0.061 0.055 0.040 0.031 0.032 Recommended weighting scheme: WGHT 0.0339 0.3128 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/su Fc/Fc(max) Resolution(A) -6 0 3 366.98 168.97 5.66 0.040 1.64 -1 2 5 718.34 547.71 5.57 0.071 2.66 1 2 7 423.61 576.86 5.11 0.073 2.14 3 3 8 166.75 18.49 5.10 0.013 1.70 0 0 4 261.25 134.41 4.85 0.035 3.81 -1 -2 8 198.06 35.52 4.55 0.018 1.68 3 -8 7 209.95 119.94 4.54 0.033 1.06 3 1 1 571.34 385.87 4.47 0.060 3.52 -10 3 0 57.92 159.54 4.43 0.038 1.03 -4 4 2 550.61 699.72 4.41 0.081 1.83 4 0 0 513.56 397.84 4.38 0.061 2.71 4 7 10 74.55 4.27 4.33 0.006 1.14 1 4 8 130.27 36.61 4.32 0.018 1.70 5 9 7 113.19 20.93 4.27 0.014 1.05 -2 -4 2 187.86 25.04 4.25 0.015 2.26 -4 -2 8 232.78 140.20 4.23 0.036 1.40 5 0 0 4826.57 4095.72 4.21 0.195 2.17 -12 6 3 -130.63 405.64 4.20 0.061 0.78 3 3 0 1603.07 1342.91 4.16 0.112 2.64 -2 1 7 466.67 582.66 4.14 0.074 1.95 -1 -5 3 417.90 529.71 4.12 0.070 1.90 3 0 0 1053.08 894.84 4.08 0.091 3.61 4 -4 5 1718.41 1404.86 4.07 0.114 1.59 1 -4 10 212.23 297.40 3.82 0.053 1.26 -8 4 1 6.21 68.60 3.79 0.025 1.18 -1 -4 2 247.05 9.43 3.74 0.009 2.42 3 -3 13 1006.55 806.13 3.66 0.087 1.06 3 -8 13 -27.34 175.15 3.56 0.040 0.83 6 -2 10 1014.05 1222.51 3.56 0.107 1.17 -6 0 1 1837.99 1576.11 3.51 0.121 1.77 -9 0 8 79.85 204.47 3.50 0.044 0.97 2 -1 6 564.16 677.67 3.45 0.079 2.29 6 -3 11 161.41 80.06 3.45 0.027 1.07 1 2 13 130.27 217.25 3.45 0.045 1.19 2 -4 1 739.77 864.83 3.41 0.090 2.35 3 -8 2 792.96 617.45 3.32 0.076 1.23 5 -4 1 115.93 56.15 3.32 0.023 1.65 0 7 9 1256.53 1460.37 3.31 0.116 1.24 1 -3 1 1422.90 1638.53 3.31 0.123 3.28 -8 1 12 487.82 689.28 3.31 0.080 0.88 4 2 3 322.72 395.22 3.31 0.061 2.40 4 3 2 205.18 142.95 3.22 0.036 2.26 9 -1 12 227.03 370.47 3.21 0.059 0.92 6 11 12 869.30 584.78 3.21 0.074 0.80 -1 -2 3 1655.25 1391.63 3.20 0.114 3.28 -6 12 6 -108.80 229.40 3.19 0.046 0.78 6 2 3 1866.26 1411.89 3.18 0.114 1.73 -3 6 1 371.03 459.51 3.18 0.065 1.61 -10 5 3 24.93 101.19 3.16 0.031 0.93 -1 7 9 1025.12 1209.54 3.15 0.106 1.22 Bond lengths and angles Cr1 - Distance Angles N32 2.0001 (0.0022) N32_$1 2.0001 (0.0022) 180.00 (0.12) N33_$1 2.0092 (0.0020) 90.36 (0.08) 89.64 (0.08) N33 2.0092 (0.0020) 89.64 (0.08) 90.36 (0.08) 180.00 N31_$1 2.0112 (0.0021) 88.22 (0.08) 91.78 (0.08) 88.89 (0.08) 91.11 (0.08) N31 2.0112 (0.0021) 91.78 (0.08) 88.22 (0.08) 91.11 (0.08) 88.89 (0.08) 180.00 Cr1 - N32 N32_$1 N33_$1 N33 N31_$1 S31 - Distance Angles C31 1.6331 (0.0027) S31 - S32 - Distance Angles C32 1.6281 (0.0028) S32 - S33 - Distance Angles C33 1.6339 (0.0025) S33 - N31 - Distance Angles C31 1.1608 (0.0031) Cr1 2.0112 (0.0021) 175.90 (0.20) N31 - C31 N32 - Distance Angles C32 1.1655 (0.0031) Cr1 2.0001 (0.0022) 167.13 (0.20) N32 - C32 N33 - Distance Angles C33 1.1650 (0.0030) Cr1 2.0092 (0.0020) 174.92 (0.19) N33 - C33 C31 - Distance Angles N31 1.1608 (0.0031) S31 1.6331 (0.0027) 179.28 (0.23) C31 - N31 C32 - Distance Angles N32 1.1655 (0.0031) S32 1.6281 (0.0028) 179.75 (0.25) C32 - N32 C33 - Distance Angles N33 1.1650 (0.0030) S33 1.6339 (0.0025) 178.47 (0.22) C33 - N33 S1 - Distance Angles C1A_a 1.7265 (0.0024) C3 1.7447 (0.0024) 94.20 (0.11) S1 - C1A_a S2 - Distance Angles C2A_a 1.7329 (0.0024) C3 1.7451 (0.0025) 94.91 (0.11) S2 - C2A_a S3 - Distance Angles C5A_a 1.7362 (0.0025) C4 1.7435 (0.0024) 93.74 (0.11) S3 - C5A_a S4 - Distance Angles C6A_a 1.7364 (0.0024) C4 1.7391 (0.0025) 94.70 (0.11) S4 - C6A_a C3 - Distance Angles C4 1.3730 (0.0035) S1 1.7447 (0.0024) 121.43 (0.19) S2 1.7451 (0.0025) 123.01 (0.19) 115.54 (0.14) C3 - C4 S1 C4 - Distance Angles C3 1.3730 (0.0035) S4 1.7391 (0.0025) 122.05 (0.19) S3 1.7435 (0.0024) 121.86 (0.19) 116.10 (0.14) C4 - C3 S4 C2A_a - Distance Angles C1A_a 1.3455 (0.0033) C7A_a 1.4939 (0.0051) 114.89 (0.27) S2 1.7329 (0.0024) 116.64 (0.18) 128.09 (0.24) C2A_a - C1A_a C7A_a C1A_a - Distance Angles C2A_a 1.3455 (0.0033) S1 1.7265 (0.0024) 118.70 (0.18) S5A_a 1.7459 (0.0024) 116.28 (0.19) 124.85 (0.14) C1A_a - C2A_a S1 S5A_a - Distance Angles C1A_a 1.7459 (0.0024) C8A_a 1.8449 (0.0038) 90.63 (0.14) S5A_a - C1A_a C8A_a - Distance Angles C7A_a 1.5331 (0.0055) S5A_a 1.8449 (0.0038) 108.97 (0.26) H8A1_a 0.9900 109.89 109.89 H8A2_a 0.9900 109.89 109.89 108.30 C8A_a - C7A_a S5A_a H8A1_a C7A_a - Distance Angles C2A_a 1.4939 (0.0051) C8A_a 1.5331 (0.0055) 108.08 (0.32) H7A1_a 0.9900 110.09 110.09 H7A2_a 0.9900 110.09 110.09 108.42 C7A_a - C2A_a C8A_a H7A1_a C6A_a - Distance Angles C5A_a 1.3432 (0.0033) C9A_a 1.4906 (0.0041) 116.79 (0.25) S4 1.7364 (0.0024) 116.68 (0.19) 126.25 (0.21) C6A_a - C5A_a C9A_a C5A_a - Distance Angles C6A_a 1.3432 (0.0033) S3 1.7362 (0.0025) 118.63 (0.19) S6A_a 1.7454 (0.0024) 115.40 (0.19) 125.90 (0.14) C5A_a - C6A_a S3 S6A_a - Distance Angles C5A_a 1.7454 (0.0024) C10A_a 1.8449 (0.0029) 90.48 (0.12) S6A_a - C5A_a C10A_a - Distance Angles C9A_a 1.5391 (0.0046) S6A_a 1.8449 (0.0029) 109.85 (0.20) H10A_a 0.9900 109.69 109.69 H10B_a 0.9900 109.69 109.69 108.19 C10A_a - C9A_a S6A_a H10A_a C9A_a - Distance Angles C6A_a 1.4906 (0.0041) C10A_a 1.5391 (0.0046) 106.23 (0.28) H9A1_a 0.9900 110.48 110.48 H9A2_a 0.9900 110.48 110.48 108.67 C9A_a - C6A_a C10A_a H9A1_a S5B_b - Distance Angles C8B_b 1.8751 (0.0148) S5B_b - C8B_b - Distance Angles C7B_b 1.5471 (0.0152) S5B_b 1.8751 (0.0148) 110.24 (1.24) H8B1_b 0.9900 109.61 109.61 H8B2_b 0.9900 109.61 109.61 108.13 C8B_b - C7B_b S5B_b H8B1_b C7B_b - Distance Angles C8B_b 1.5471 (0.0152) H7B1_b 0.9900 110.32 H7B2_b 0.9900 110.32 108.56 C7B_b - C8B_b H7B1_b S6B_b - Distance Angles C10B_b 1.8623 (0.0155) S6B_b - C10B_b - Distance Angles C9B_b 1.5459 (0.0157) S6B_b 1.8623 (0.0154) 109.19 (1.73) H10C_b 0.9900 109.84 109.84 H10D_b 0.9900 109.84 109.84 108.27 C10B_b - C9B_b S6B_b H10C_b C9B_b - Distance Angles C10B_b 1.5459 (0.0157) H9B1_b 0.9900 110.23 H9B2_b 0.9900 110.24 108.51 C9B_b - C10B_b H9B1_b S11 - Distance Angles C11A_c 1.7380 (0.0025) C13 1.7490 (0.0025) 94.62 (0.12) S11 - C11A_c S12 - Distance Angles C12A_c 1.7343 (0.0024) C13 1.7419 (0.0025) 94.41 (0.11) S12 - C12A_c S13 - Distance Angles C15A_c 1.7374 (0.0025) C14 1.7481 (0.0025) 93.76 (0.11) S13 - C15A_c S14 - Distance Angles C16A_c 1.7312 (0.0025) C14 1.7376 (0.0024) 94.75 (0.11) S14 - C16A_c C13 - Distance Angles C14 1.3785 (0.0034) S12 1.7419 (0.0025) 121.88 (0.19) S11 1.7490 (0.0025) 122.44 (0.19) 115.67 (0.14) C13 - C14 S12 C14 - Distance Angles C13 1.3785 (0.0034) S14 1.7376 (0.0024) 121.99 (0.19) S13 1.7481 (0.0025) 121.84 (0.19) 116.16 (0.14) C14 - C13 S14 C12A_c - Distance Angles C11A_c 1.3437 (0.0034) C17A_c 1.4841 (0.0113) 111.72 (0.64) S12 1.7343 (0.0024) 118.17 (0.19) 130.11 (0.64) C12A_c - C11A_c C17A_c C11A_c - Distance Angles C12A_c 1.3437 (0.0034) S11 1.7380 (0.0025) 117.13 (0.19) S15A_c 1.7429 (0.0043) 120.39 (0.25) 122.48 (0.21) C11A_c - C12A_c S11 S15A_c - Distance Angles C11A_c 1.7429 (0.0043) C18A_c 1.8554 (0.0138) 87.92 (0.51) S15A_c - C11A_c C18A_c - Distance Angles C17A_c 1.5389 (0.0142) S15A_c 1.8554 (0.0138) 109.50 (0.93) H18A_c 0.9900 109.77 109.77 H18B_c 0.9900 109.77 109.77 108.23 C18A_c - C17A_c S15A_c H18A_c C17A_c - Distance Angles C12A_c 1.4841 (0.0113) C18A_c 1.5389 (0.0142) 109.15 (0.97) H17A_c 0.9900 109.85 109.85 H17B_c 0.9900 109.85 109.85 108.28 C17A_c - C12A_c C18A_c H17A_c C16A_c - Distance Angles C15A_c 1.3495 (0.0033) C19A_c 1.5005 (0.0043) 115.34 (0.28) S14 1.7312 (0.0025) 117.03 (0.19) 127.35 (0.25) C16A_c - C15A_c C19A_c C15A_c - Distance Angles C16A_c 1.3495 (0.0033) S13 1.7374 (0.0025) 118.25 (0.19) S16A_c 1.7460 (0.0024) 116.17 (0.19) 125.49 (0.14) C15A_c - C16A_c S13 S16A_c - Distance Angles C15A_c 1.7460 (0.0024) C20A_c 1.8534 (0.0027) 90.06 (0.12) S16A_c - C15A_c C20A_c - Distance Angles C19A_c 1.5366 (0.0052) S16A_c 1.8534 (0.0027) 109.25 (0.22) H20A_c 0.9900 109.83 109.83 H20B_c 0.9900 109.83 109.83 108.26 C20A_c - C19A_c S16A_c H20A_c C19A_c - Distance Angles C16A_c 1.5005 (0.0043) C20A_c 1.5366 (0.0052) 106.68 (0.29) H19A_c 0.9900 110.39 110.39 H19B_c 0.9900 110.39 110.39 108.61 C19A_c - C16A_c C20A_c H19A_c S15B_d - Distance Angles C18B_d 1.8478 (0.0065) S15B_d - C18B_d - Distance Angles C17B_d 1.5447 (0.0086) S15B_d 1.8478 (0.0065) 110.51 (0.44) H18C_d 0.9900 109.55 109.55 H18D_d 0.9900 109.55 109.55 108.10 C18B_d - C17B_d S15B_d H18C_d C17B_d - Distance Angles C18B_d 1.5447 (0.0086) H17C_d 0.9900 110.32 H17D_d 0.9900 110.32 108.56 C17B_d - C18B_d H17C_d S16B_d - Distance Angles C20B_d 1.8579 (0.0155) S16B_d - C20B_d - Distance Angles C19B_d 1.5435 (0.0155) S16B_d 1.8579 (0.0155) 109.30 (1.63) H20C_d 0.9900 109.82 109.81 H20D_d 0.9900 109.82 109.82 108.26 C20B_d - C19B_d S16B_d H20C_d C19B_d - Distance Angles C20B_d 1.5435 (0.0155) H19C_d 0.9900 110.33 H19D_d 0.9900 110.33 108.57 C19B_d - C20B_d H19C_d S21 - Distance Angles C21A_e 1.7413 (0.0024) C23 1.7580 (0.0024) 93.88 (0.11) S21 - C21A_e S22 - Distance Angles C22A_e 1.7485 (0.0023) C23 1.7607 (0.0024) 94.55 (0.11) S22 - C22A_e C23 - Distance Angles C23_$2 1.3599 (0.0047) S21 1.7580 (0.0024) 121.85 (0.24) S22 1.7607 (0.0024) 122.65 (0.25) 115.50 (0.13) C23 - C23_$2 S21 C22A_e - Distance Angles C21A_e 1.3362 (0.0032) C24A_e 1.4943 (0.0045) 116.59 (0.29) S22 1.7485 (0.0023) 116.95 (0.18) 126.45 (0.26) C22A_e - C21A_e C24A_e C21A_e - Distance Angles C22A_e 1.3362 (0.0032) S21 1.7413 (0.0024) 119.10 (0.18) S23A_e 1.7503 (0.0023) 115.68 (0.18) 125.20 (0.14) C21A_e - C22A_e S21 S23A_e - Distance Angles C21A_e 1.7503 (0.0023) C25A_e 1.8509 (0.0029) 90.85 (0.12) S23A_e - C21A_e C25A_e - Distance Angles C24A_e 1.5413 (0.0055) S23A_e 1.8509 (0.0029) 109.39 (0.21) H25A_e 0.9900 109.80 109.80 H25B_e 0.9900 109.80 109.80 108.25 C25A_e - C24A_e S23A_e H25A_e C24A_e - Distance Angles C22A_e 1.4943 (0.0045) C25A_e 1.5413 (0.0055) 107.29 (0.30) H24A_e 0.9900 110.26 110.26 H24B_e 0.9900 110.26 110.26 108.52 C24A_e - C22A_e C25A_e H24A_e S23B_f - Distance Angles C25B_f 1.8627 (0.0151) S23B_f - C25B_f - Distance Angles C24B_f 1.5469 (0.0153) S23B_f 1.8627 (0.0151) 110.47 (1.38) H25C_f 0.9900 109.56 109.56 H25D_f 0.9900 109.56 109.56 108.10 C25B_f - C24B_f S23B_f H25C_f C24B_f - Distance Angles C25B_f 1.5469 (0.0153) H24C_f 0.9900 110.31 H24D_f 0.9900 110.31 108.56 C24B_f - C25B_f H24C_f FMAP and GRID set by program FMAP 2 3 36 GRID -1.515 -2 -2 1.515 2 2 R1 = 0.0736 for 8416 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.41 at 0.0891 0.1797 0.2771 [ 0.82 A from C15B ] Deepest hole -0.41 at 0.0567 0.4974 0.0266 [ 0.78 A from CR1 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 6199 / 32028 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0891 0.1797 0.2771 1.00000 0.05 0.41 0.82 C16A 0.82 C15B 0.86 C19A 1.03 S16B Q2 1 0.0120 0.5009 -0.4331 1.00000 0.05 0.38 1.97 S32 3.09 S11 3.44 S14 3.45 C3 Q3 1 0.0183 0.5804 -0.1703 1.00000 0.05 0.37 0.79 N32 0.87 C32 2.34 S32 2.38 H19A Q4 1 0.4860 0.0526 0.4169 1.00000 0.05 0.36 0.87 C23 0.89 S22 1.97 C23 2.03 C22A Q5 1 0.1297 0.0042 0.3353 1.00000 0.05 0.35 0.32 C15A 0.32 C16B 1.38 C16A 1.38 C15B Q6 1 0.1618 -0.0354 0.2856 1.00000 0.05 0.35 0.60 C19B 0.84 S16A 0.91 C15A 0.91 C16B Q7 1 0.2854 0.5903 0.2486 1.00000 0.05 0.35 0.73 C9A 0.77 C6A 0.77 C5B 0.99 S6B Q8 1 0.1701 0.0432 0.7895 1.00000 0.05 0.34 0.58 C17A 0.89 S15B 0.95 C12A 0.95 C11B Q9 1 -0.0198 0.5449 -0.3727 1.00000 0.05 0.34 1.08 S32 2.66 C32 2.80 S14 3.39 C5A Q10 1 0.2940 0.4223 0.3741 1.00000 0.05 0.34 0.96 C5A 0.96 C6B 1.02 S3 1.93 C6A Shortest distances between peaks (including symmetry equivalents) 5 6 0.96 2 9 1.13 1 5 2.08 2 2 2.13 1 6 2.46 7 10 2.50 4 4 2.72 9 10 3.00 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.02: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.02: Analyse other restraints etc. 1.28: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.08: Set up l.s. refinement 0.02: Generate idealized H-atoms 11.28: Structure factors and derivatives 49.33: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.13: Apply other restraints 3.42: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 13:24:23 Total CPU time: 65.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++