+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 15:46:02 on 03-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01ESP301 in P2(1)2(1)2(1) CELL 0.71073 10.9877 11.9703 22.4663 90.000 90.000 90.000 ZERR 4.00 0.0007 0.0008 0.0018 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O S UNIT 112 128 8 44 4 V = 2954.90 F(000) = 1272.0 Mu = 0.17 mm-1 Cell Wt = 2418.46 Rho = 1.359 MERG 2 ISOR 0.01 $C $O SHEL 7 0.84 FMAP 2 PLAN 15 SIZE 0.07 0.07 0.60 L.S. 4 TEMP -153.00 WGHT 0.042100 FVAR 0.06495 C1 1 0.869165 0.516079 0.150404 11.00000 0.01223 0.03337 = 0.03330 -0.00203 0.00595 0.00835 C2 1 0.858936 0.500455 0.210520 11.00000 0.03773 0.03180 = 0.05044 -0.00427 0.00037 0.00387 AFIX 43 H2 2 0.829637 0.558599 0.235481 11.00000 -1.20000 AFIX 0 C3 1 0.892415 0.397400 0.234396 11.00000 0.03699 0.04760 = 0.05357 0.00081 0.00442 -0.01063 AFIX 43 H3 2 0.881460 0.384194 0.275746 11.00000 -1.20000 AFIX 0 C4 1 0.941148 0.314196 0.199159 11.00000 0.04248 0.04374 = 0.04718 0.00792 -0.00048 0.00431 AFIX 43 H4 2 0.969067 0.246165 0.216122 11.00000 -1.20000 AFIX 0 C5 1 0.948124 0.332350 0.139268 11.00000 0.05271 0.04834 = 0.06224 -0.01401 0.01119 0.01493 AFIX 43 H5 2 0.976642 0.274527 0.113884 11.00000 -1.20000 AFIX 0 C6 1 0.913405 0.436191 0.114588 11.00000 0.04089 0.03669 = 0.03606 -0.00205 -0.00134 0.00549 AFIX 43 H6 2 0.921330 0.449250 0.073060 11.00000 -1.20000 AFIX 0 C7 1 0.838269 0.628400 0.123610 11.00000 0.03836 0.02407 = 0.03489 -0.00466 0.00010 0.01369 C8 1 0.769982 0.629273 0.061924 11.00000 0.02983 0.03070 = 0.03568 0.00117 0.00095 0.00219 AFIX 13 H8 2 0.827943 0.608985 0.029353 11.00000 -1.20000 AFIX 0 C9 1 0.724332 0.751579 0.053012 11.00000 0.03146 0.03333 = 0.03745 0.01193 0.01610 -0.00276 AFIX 23 H9A 2 0.758936 0.783849 0.016137 11.00000 -1.20000 H9B 2 0.634444 0.753428 0.050150 11.00000 -1.20000 AFIX 0 C10 1 0.766765 0.816046 0.106531 11.00000 0.02242 0.02997 = 0.04309 0.00970 0.00363 -0.00458 C11 1 0.945354 0.706445 0.110881 11.00000 0.02471 0.02117 = 0.04540 0.00725 0.00165 -0.00527 C12 1 0.667263 0.550938 0.062281 11.00000 0.05290 0.03627 = 0.03472 -0.00194 -0.00111 0.00404 C13 1 0.970038 0.887264 0.065130 11.00000 0.04242 0.02153 = 0.06245 -0.00549 0.00545 0.00139 AFIX 33 H13A 2 0.931104 0.960897 0.064126 11.00000 -1.50000 H13B 2 0.970968 0.855406 0.024950 11.00000 -1.50000 H13C 2 1.053723 0.894902 0.079660 11.00000 -1.50000 AFIX 0 C14 1 0.717008 0.933856 0.118889 11.00000 0.01074 0.02126 = 0.02198 0.00153 0.00299 -0.00690 AFIX 13 H14 2 0.766678 0.989731 0.096420 11.00000 -1.20000 AFIX 0 C15 1 0.582180 0.947951 0.102061 11.00000 0.03350 0.02301 = 0.02871 0.00024 0.00417 -0.01064 AFIX 13 H15 2 0.570657 0.939106 0.058161 11.00000 -1.20000 AFIX 0 C16 1 0.429475 0.800511 0.103032 11.00000 0.02385 0.02593 = 0.04377 0.00194 -0.00291 -0.00326 C17 1 0.363315 0.724914 0.143755 11.00000 0.03159 0.04614 = 0.05146 -0.00084 0.00190 -0.00245 AFIX 33 H17A 2 0.390503 0.738009 0.184710 11.00000 -1.50000 H17B 2 0.379838 0.647183 0.132701 11.00000 -1.50000 H17C 2 0.275737 0.739423 0.140857 11.00000 -1.50000 AFIX 0 C18 1 0.822267 1.021022 0.199706 11.00000 0.04379 0.02862 = 0.04130 0.00234 0.00801 0.01112 C19 1 0.817218 1.033357 0.266425 11.00000 0.03059 0.03777 = 0.04243 0.00087 -0.00028 0.00208 AFIX 33 H19A 2 0.744471 0.995661 0.281707 11.00000 -1.50000 H19B 2 0.813929 1.112812 0.276816 11.00000 -1.50000 H19C 2 0.889970 0.999618 0.284134 11.00000 -1.50000 AFIX 0 C20 1 0.531997 1.060554 0.123149 11.00000 0.01867 0.03051 = 0.03765 -0.00351 0.00411 0.00807 AFIX 13 H20 2 0.532942 1.061895 0.167652 11.00000 -1.20000 AFIX 0 C21 1 0.323573 1.090739 0.145179 11.00000 0.01989 0.05110 = 0.06098 -0.00151 0.00485 0.00350 C22 1 0.197344 1.086037 0.118861 11.00000 0.06944 0.08952 = 0.09571 -0.00150 -0.00796 -0.00344 AFIX 33 H22A 2 0.202275 1.061241 0.077359 11.00000 -1.50000 H22B 2 0.160311 1.160454 0.120469 11.00000 -1.50000 H22C 2 0.147459 1.033361 0.141660 11.00000 -1.50000 AFIX 0 C23 1 0.593803 1.163854 0.100620 11.00000 0.01391 0.03023 = 0.02907 -0.00136 -0.00623 -0.00130 AFIX 13 H23 2 0.682802 1.161039 0.109806 11.00000 -1.20000 AFIX 0 C24 1 0.574008 1.192606 0.035003 11.00000 0.03203 0.04686 = 0.03781 -0.00872 0.01126 0.00096 AFIX 23 H24A 2 0.485683 1.198188 0.026820 11.00000 -1.20000 H24B 2 0.611428 1.265997 0.026182 11.00000 -1.20000 AFIX 0 C25 1 0.732265 1.129033 -0.027649 11.00000 0.06073 0.05277 = 0.09621 -0.01140 0.01664 0.00069 C26 1 0.773094 1.039416 -0.070448 11.00000 0.05589 0.05531 = 0.05191 -0.01076 0.00832 0.00706 AFIX 33 H26A 2 0.711039 0.980744 -0.072548 11.00000 -1.50000 H26B 2 0.850015 1.007198 -0.056561 11.00000 -1.50000 H26C 2 0.784748 1.072101 -0.110034 11.00000 -1.50000 AFIX 0 C27 1 0.579974 1.281754 0.185312 11.00000 0.04524 0.03321 = 0.04254 -0.01033 0.00525 0.00210 C28 1 0.516324 1.382851 0.211288 11.00000 0.05314 0.03571 = 0.04274 -0.00701 0.00746 -0.00484 AFIX 33 H28A 2 0.456162 1.410908 0.182765 11.00000 -1.50000 H28B 2 0.576366 1.441361 0.219571 11.00000 -1.50000 H28C 2 0.475262 1.361696 0.248334 11.00000 -1.50000 AFIX 0 N1 3 0.587161 0.490581 0.059304 11.00000 0.03952 0.04387 = 0.08536 0.00459 -0.02568 -0.01779 N2 3 0.901690 0.813333 0.105010 11.00000 0.03579 0.04330 = 0.04187 -0.00138 0.00888 -0.00482 O1 4 1.050500 0.677855 0.105293 11.00000 0.02197 0.04047 = 0.05831 -0.00359 0.00374 0.00663 O2 4 0.512080 0.864768 0.134349 11.00000 0.02219 0.01869 = 0.03470 0.00214 0.00446 -0.00248 O3 4 0.418826 0.809209 0.049165 11.00000 0.02831 0.04859 = 0.04190 -0.00194 -0.00498 -0.01163 O4 4 0.726008 0.956696 0.181062 11.00000 0.01491 0.04269 = 0.03646 -0.00229 -0.00174 -0.00851 O5 4 0.896892 1.058364 0.167042 11.00000 0.03714 0.04029 = 0.05268 -0.00840 -0.00214 -0.00768 O6 4 0.406530 1.059829 0.103156 11.00000 0.03295 0.03363 = 0.04318 -0.00289 -0.00297 -0.00204 O7 4 0.344594 1.118986 0.194127 11.00000 0.03442 0.06675 = 0.05785 -0.01268 0.01267 0.00587 O8 4 0.626932 1.108661 -0.002836 11.00000 0.05637 0.03813 = 0.05481 -0.00623 0.01156 -0.01292 O9 4 0.784665 1.210738 -0.015379 11.00000 0.09999 0.12817 = 0.19958 -0.05745 0.07461 -0.03335 O10 4 0.537778 1.261772 0.129257 11.00000 0.03564 0.03208 = 0.03342 -0.00476 -0.00389 0.00514 O11 4 0.655001 1.225617 0.210202 11.00000 0.02563 0.04766 = 0.04746 -0.01051 -0.00509 0.00112 S1 5 0.737000 0.719234 0.168986 11.00000 0.02811 0.03877 = 0.04413 0.00284 0.00342 0.00240 HKLF 4 Covalent radii and connectivity table for 01ESP301 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C1 - C6 C2 C7 C2 - C1 C3 C3 - C4 C2 C4 - C5 C3 C5 - C4 C6 C6 - C1 C5 C7 - C1 C11 C8 S1 C8 - C12 C9 C7 C9 - C10 C8 C10 - N2 C9 C14 S1 C11 - O1 N2 C7 C12 - N1 C8 C13 - N2 C14 - O4 C10 C15 C15 - O2 C20 C14 C16 - O3 O2 C17 C17 - C16 C18 - O5 O4 C19 C19 - C18 C20 - O6 C23 C15 C21 - O7 O6 C22 C22 - C21 C23 - O10 C20 C24 C24 - O8 C23 C25 - O9 O8 C26 C26 - C25 C27 - O11 O10 C28 C28 - C27 N1 - C12 N2 - C11 C13 C10 O1 - C11 O2 - C16 C15 O3 - C16 O4 - C18 C14 O5 - C18 O6 - C21 C20 O7 - C21 O8 - C25 C24 O9 - C25 O10 - C27 C23 O11 - C27 S1 - C10 C7 h k l Fo^2 Sigma Why rejected 0 5 0 1.90 0.40 observed but should be systematically absent 14067 Reflections read, of which 974 rejected -12 =< h =< 11, -14 =< k =< 11, -26 =< l =< 26, Max. 2-theta = 50.05 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 10 0 4.16 0.38 2 2.10 -2 5 1 13.15 0.29 4 4.69 0 5 1 2.78 0.17 4 2.65 4 0 8 0.46 0.10 4 0.61 4 Inconsistent equivalents 5105 Unique reflections, of which 0 suppressed R(int) = 0.2525 R(sigma) = 0.4831 Friedel opposites not merged Maximum memory for data reduction = 2928 / 50679 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 = 4003 / 484123 wR2 = 0.1930 before cycle 1 for 5105 data and 379 / 379 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.0426 0.0100 ISOR U11 O9 -0.0570 0.0100 ISOR U33 O9 0.0575 0.0100 ISOR U23 O9 -0.0746 0.0100 ISOR U13 O9 0.0334 0.0100 ISOR U12 O9 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. 0. 0. 0. 0. 0. 0. 234. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.011 0.000 GooF = S = 0.904; Restrained GooF = 0.907 for 234 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.06495 0.00018 -0.010 OSF Mean shift/esd = 0.000 Maximum = -0.010 for OSF Max. shift = 0.000 A for C25 Max. dU = 0.000 for O10 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4003 / 484123 wR2 = 0.1930 before cycle 2 for 5105 data and 379 / 379 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.0426 0.0100 ISOR U11 O9 -0.0570 0.0100 ISOR U33 O9 0.0574 0.0100 ISOR U23 O9 -0.0746 0.0100 ISOR U13 O9 0.0334 0.0100 ISOR U12 O9 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. 0. 0. 0. 0. 0. 0. 234. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.011 0.000 GooF = S = 0.904; Restrained GooF = 0.907 for 234 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.06495 0.00018 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U33 S1 Max. shift = 0.000 A for C25 Max. dU = 0.000 for O9 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4003 / 484123 wR2 = 0.1930 before cycle 3 for 5105 data and 379 / 379 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 0.0426 0.0100 ISOR U11 O9 -0.0570 0.0100 ISOR U33 O9 0.0574 0.0100 ISOR U23 O9 -0.0746 0.0100 ISOR U13 O9 0.0334 0.0100 ISOR U12 O9 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. 0. 0. 0. 0. 0. 0. 234. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.011 0.000 GooF = S = 0.904; Restrained GooF = 0.907 for 234 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.06495 0.00018 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for O9 Max. dU = 0.000 for C3 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4003 / 484123 wR2 = 0.1930 before cycle 4 for 5105 data and 379 / 379 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.0426 0.0100 ISOR U11 O9 -0.0570 0.0100 ISOR U33 O9 0.0574 0.0100 ISOR U23 O9 -0.0746 0.0100 ISOR U13 O9 0.0334 0.0100 ISOR U12 O9 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. 0. 0. 0. 0. 0. 0. 234. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.011 0.000 GooF = S = 0.904; Restrained GooF = 0.907 for 234 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.06495 0.00018 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y S1 Max. shift = 0.000 A for C23 Max. dU = 0.000 for C26 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.8296 0.5586 0.2355 43 0.950 0.000 C2 C1 C3 H3 0.8815 0.3842 0.2757 43 0.950 0.000 C3 C4 C2 H4 0.9691 0.2462 0.2161 43 0.950 0.000 C4 C5 C3 H5 0.9766 0.2745 0.1139 43 0.950 0.000 C5 C4 C6 H6 0.9213 0.4492 0.0731 43 0.950 0.000 C6 C1 C5 H8 0.8279 0.6090 0.0294 13 1.000 0.000 C8 C12 C9 C7 H9A 0.7589 0.7838 0.0161 23 0.990 0.000 C9 C10 C8 H9B 0.6344 0.7534 0.0502 23 0.990 0.000 C9 C10 C8 H13A 0.9311 0.9609 0.0641 33 0.980 0.000 C13 N2 H13A H13B 0.9710 0.8554 0.0249 33 0.980 0.000 C13 N2 H13A H13C 1.0537 0.8949 0.0797 33 0.980 0.000 C13 N2 H13A H14 0.7667 0.9897 0.0964 13 1.000 0.000 C14 O4 C10 C15 H15 0.5707 0.9391 0.0582 13 1.000 0.000 C15 O2 C20 C14 H17A 0.3905 0.7380 0.1847 33 0.980 0.000 C17 C16 H17A H17B 0.3798 0.6472 0.1327 33 0.980 0.000 C17 C16 H17A H17C 0.2757 0.7394 0.1409 33 0.980 0.000 C17 C16 H17A H19A 0.7445 0.9957 0.2817 33 0.980 0.000 C19 C18 H19A H19B 0.8139 1.1128 0.2768 33 0.980 0.000 C19 C18 H19A H19C 0.8900 0.9996 0.2841 33 0.980 0.000 C19 C18 H19A H20 0.5329 1.0619 0.1677 13 1.000 0.000 C20 O6 C23 C15 H22A 0.2023 1.0612 0.0774 33 0.980 0.000 C22 C21 H22A H22B 0.1603 1.1605 0.1205 33 0.980 0.000 C22 C21 H22A H22C 0.1475 1.0334 0.1417 33 0.980 0.000 C22 C21 H22A H23 0.6828 1.1610 0.1098 13 1.000 0.000 C23 O10 C20 C24 H24A 0.4857 1.1982 0.0268 23 0.990 0.000 C24 O8 C23 H24B 0.6114 1.2660 0.0262 23 0.990 0.000 C24 O8 C23 H26A 0.7110 0.9807 -0.0725 33 0.980 0.000 C26 C25 H26A H26B 0.8500 1.0072 -0.0566 33 0.980 0.000 C26 C25 H26A H26C 0.7847 1.0721 -0.1100 33 0.980 0.000 C26 C25 H26A H28A 0.4562 1.4109 0.1828 33 0.980 0.000 C28 C27 H28A H28B 0.5764 1.4414 0.2196 33 0.980 0.000 C28 C27 H28A H28C 0.4753 1.3617 0.2483 33 0.980 0.000 C28 C27 H28A 01ESP301 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.86917 0.51608 0.15040 1.00000 0.01222 0.03338 0.03330 -0.00203 0.00595 0.00835 0.02630 0.01689 0.00093 0.00078 0.00046 0.00000 0.00608 0.00541 0.00595 0.00504 0.00504 0.00465 0.00274 C2 0.85894 0.50046 0.21052 1.00000 0.03773 0.03180 0.05044 -0.00427 0.00037 0.00387 0.03999 0.01718 0.00095 0.00079 0.00048 0.00000 0.00704 0.00553 0.00665 0.00523 0.00582 0.00517 0.00316 H2 0.82964 0.55860 0.23548 1.00000 0.04799 0.00000 0.00000 C3 0.89241 0.39740 0.23440 1.00000 0.03698 0.04760 0.05357 0.00081 0.00442 -0.01063 0.04605 0.01784 0.00100 0.00084 0.00049 0.00000 0.00721 0.00609 0.00680 0.00564 0.00604 0.00544 0.00344 H3 0.88146 0.38419 0.27575 1.00000 0.05526 0.00000 0.00000 C4 0.94115 0.31420 0.19916 1.00000 0.04248 0.04374 0.04718 0.00792 -0.00048 0.00431 0.04447 0.01799 0.00099 0.00081 0.00051 0.00000 0.00716 0.00597 0.00663 0.00557 0.00600 0.00549 0.00333 H4 0.96907 0.24617 0.21612 1.00000 0.05336 0.00000 0.00000 C5 0.94812 0.33235 0.13927 1.00000 0.05271 0.04834 0.06224 -0.01401 0.01119 0.01493 0.05443 0.01941 0.00105 0.00089 0.00054 0.00000 0.00754 0.00617 0.00726 0.00580 0.00620 0.00587 0.00358 H5 0.97664 0.27453 0.11388 1.00000 0.06532 0.00000 0.00000 C6 0.91341 0.43619 0.11459 1.00000 0.04089 0.03669 0.03606 -0.00205 -0.00134 0.00549 0.03788 0.01645 0.00091 0.00078 0.00046 0.00000 0.00700 0.00551 0.00594 0.00542 0.00580 0.00539 0.00304 H6 0.92133 0.44925 0.07306 1.00000 0.04546 0.00000 0.00000 C7 0.83827 0.62840 0.12361 1.00000 0.03836 0.02407 0.03489 -0.00466 0.00010 0.01369 0.03244 0.01715 0.00100 0.00075 0.00042 0.00000 0.00676 0.00514 0.00607 0.00479 0.00550 0.00504 0.00290 C8 0.76998 0.62927 0.06192 1.00000 0.02983 0.03070 0.03568 0.00117 0.00095 0.00219 0.03207 0.01666 0.00098 0.00070 0.00042 0.00000 0.00657 0.00526 0.00590 0.00477 0.00555 0.00510 0.00282 H8 0.82794 0.60899 0.02935 1.00000 0.03849 0.00000 0.00000 C9 0.72433 0.75158 0.05301 1.00000 0.03146 0.03333 0.03745 0.01193 0.01610 -0.00276 0.03408 0.01645 0.00096 0.00065 0.00039 0.00000 0.00658 0.00554 0.00580 0.00472 0.00528 0.00476 0.00294 H9A 0.75894 0.78385 0.01614 1.00000 0.04090 0.00000 0.00000 H9B 0.63444 0.75343 0.05015 1.00000 0.04090 0.00000 0.00000 C10 0.76676 0.81605 0.10653 1.00000 0.02242 0.02997 0.04309 0.00970 0.00363 -0.00458 0.03183 0.01813 0.00103 0.00073 0.00046 0.00000 0.00631 0.00544 0.00611 0.00473 0.00576 0.00506 0.00285 C11 0.94535 0.70645 0.11088 1.00000 0.02471 0.02117 0.04540 0.00725 0.00165 -0.00527 0.03043 0.01760 0.00106 0.00077 0.00046 0.00000 0.00649 0.00546 0.00622 0.00512 0.00575 0.00545 0.00285 C12 0.66726 0.55094 0.06228 1.00000 0.05290 0.03627 0.03472 -0.00194 -0.00111 0.00404 0.04130 0.02088 0.00120 0.00088 0.00046 0.00000 0.00777 0.00604 0.00610 0.00551 0.00601 0.00595 0.00327 C13 0.97004 0.88726 0.06513 1.00000 0.04242 0.02153 0.06245 -0.00549 0.00545 0.00139 0.04213 0.01715 0.00099 0.00068 0.00044 0.00000 0.00707 0.00484 0.00670 0.00508 0.00602 0.00517 0.00319 H13A 0.93110 0.96090 0.06413 1.00000 0.06320 0.00000 0.00000 H13B 0.97097 0.85541 0.02495 1.00000 0.06320 0.00000 0.00000 H13C 1.05372 0.89490 0.07966 1.00000 0.06320 0.00000 0.00000 C14 0.71701 0.93386 0.11889 1.00000 0.01074 0.02126 0.02198 0.00153 0.00299 -0.00690 0.01800 0.01501 0.00087 0.00066 0.00038 0.00000 0.00592 0.00493 0.00541 0.00449 0.00482 0.00443 0.00247 H14 0.76668 0.98973 0.09642 1.00000 0.02159 0.00000 0.00000 C15 0.58218 0.94795 0.10206 1.00000 0.03350 0.02301 0.02871 0.00024 0.00417 -0.01064 0.02841 0.01620 0.00093 0.00072 0.00042 0.00000 0.00666 0.00496 0.00563 0.00461 0.00533 0.00509 0.00278 H15 0.57066 0.93911 0.05816 1.00000 0.03409 0.00000 0.00000 C16 0.42948 0.80051 0.10303 1.00000 0.02385 0.02593 0.04377 0.00194 -0.00291 -0.00326 0.03118 0.01884 0.00094 0.00078 0.00052 0.00000 0.00653 0.00546 0.00641 0.00546 0.00591 0.00494 0.00297 C17 0.36332 0.72491 0.14376 1.00000 0.03159 0.04614 0.05146 -0.00084 0.00190 -0.00245 0.04306 0.01675 0.00093 0.00076 0.00042 0.00000 0.00671 0.00562 0.00638 0.00528 0.00547 0.00544 0.00313 H17A 0.39050 0.73801 0.18471 1.00000 0.06459 0.00000 0.00000 H17B 0.37984 0.64718 0.13270 1.00000 0.06459 0.00000 0.00000 H17C 0.27574 0.73942 0.14086 1.00000 0.06459 0.00000 0.00000 C18 0.82227 1.02102 0.19971 1.00000 0.04379 0.02862 0.04130 0.00234 0.00801 0.01112 0.03790 0.02136 0.00119 0.00083 0.00050 0.00000 0.00758 0.00574 0.00689 0.00539 0.00598 0.00554 0.00333 C19 0.81722 1.03336 0.26643 1.00000 0.03059 0.03777 0.04243 0.00087 -0.00028 0.00208 0.03693 0.01530 0.00090 0.00069 0.00039 0.00000 0.00680 0.00536 0.00631 0.00510 0.00523 0.00497 0.00305 H19A 0.74447 0.99566 0.28171 1.00000 0.05539 0.00000 0.00000 H19B 0.81393 1.11281 0.27682 1.00000 0.05539 0.00000 0.00000 H19C 0.88997 0.99962 0.28413 1.00000 0.05539 0.00000 0.00000 C20 0.53200 1.06055 0.12315 1.00000 0.01867 0.03051 0.03765 -0.00351 0.00411 0.00807 0.02894 0.01782 0.00097 0.00072 0.00044 0.00000 0.00633 0.00515 0.00593 0.00490 0.00518 0.00509 0.00273 H20 0.53294 1.06190 0.16765 1.00000 0.03473 0.00000 0.00000 C21 0.32357 1.09074 0.14518 1.00000 0.01989 0.05110 0.06098 -0.00151 0.00485 0.00350 0.04399 0.02217 0.00118 0.00090 0.00060 0.00000 0.00711 0.00680 0.00738 0.00604 0.00648 0.00563 0.00366 C22 0.19734 1.08604 0.11886 1.00000 0.06944 0.08952 0.09571 -0.00150 -0.00796 -0.00344 0.08489 0.02007 0.00120 0.00089 0.00053 0.00000 0.00859 0.00777 0.00810 0.00658 0.00722 0.00684 0.00471 H22A 0.20227 1.06124 0.07736 1.00000 0.12733 0.00000 0.00000 H22B 0.16031 1.16045 0.12047 1.00000 0.12733 0.00000 0.00000 H22C 0.14746 1.03336 0.14166 1.00000 0.12733 0.00000 0.00000 C23 0.59380 1.16385 0.10062 1.00000 0.01391 0.03023 0.02907 -0.00136 -0.00623 -0.00130 0.02440 0.01544 0.00087 0.00072 0.00041 0.00000 0.00600 0.00527 0.00568 0.00469 0.00497 0.00486 0.00267 H23 0.68280 1.16104 0.10981 1.00000 0.02928 0.00000 0.00000 C24 0.57401 1.19261 0.03500 1.00000 0.03203 0.04686 0.03781 -0.00872 0.01126 0.00096 0.03890 0.01738 0.00095 0.00074 0.00042 0.00000 0.00677 0.00590 0.00617 0.00512 0.00528 0.00534 0.00314 H24A 0.48568 1.19819 0.02682 1.00000 0.04668 0.00000 0.00000 H24B 0.61143 1.26600 0.02618 1.00000 0.04668 0.00000 0.00000 C25 0.73227 1.12903 -0.02765 1.00000 0.06073 0.05277 0.09621 -0.01140 0.01664 0.00069 0.06990 0.02440 0.00145 0.00097 0.00062 0.00000 0.00840 0.00665 0.00822 0.00662 0.00723 0.00686 0.00422 C26 0.77309 1.03942 -0.07045 1.00000 0.05589 0.05531 0.05191 -0.01076 0.00832 0.00706 0.05437 0.01735 0.00106 0.00077 0.00041 0.00000 0.00751 0.00630 0.00624 0.00551 0.00606 0.00595 0.00346 H26A 0.71104 0.98074 -0.07255 1.00000 0.08155 0.00000 0.00000 H26B 0.85001 1.00720 -0.05656 1.00000 0.08155 0.00000 0.00000 H26C 0.78475 1.07210 -0.11003 1.00000 0.08155 0.00000 0.00000 C27 0.57997 1.28175 0.18531 1.00000 0.04524 0.03321 0.04254 -0.01033 0.00525 0.00210 0.04033 0.02040 0.00111 0.00086 0.00053 0.00000 0.00723 0.00569 0.00679 0.00535 0.00578 0.00554 0.00318 C28 0.51632 1.38285 0.21129 1.00000 0.05314 0.03571 0.04274 -0.00701 0.00746 -0.00484 0.04386 0.01672 0.00103 0.00066 0.00042 0.00000 0.00726 0.00517 0.00616 0.00505 0.00588 0.00549 0.00315 H28A 0.45616 1.41091 0.18277 1.00000 0.06580 0.00000 0.00000 H28B 0.57637 1.44136 0.21957 1.00000 0.06580 0.00000 0.00000 H28C 0.47526 1.36170 0.24833 1.00000 0.06580 0.00000 0.00000 N1 0.58716 0.49058 0.05930 1.00000 0.03952 0.04387 0.08536 0.00459 -0.02568 -0.01779 0.05625 0.01582 0.00094 0.00071 0.00043 0.00000 0.00836 0.00607 0.00797 0.00559 0.00651 0.00532 0.00319 N2 0.90169 0.81333 0.10501 1.00000 0.03579 0.04330 0.04187 -0.00138 0.00888 -0.00482 0.04032 0.01424 0.00083 0.00068 0.00037 0.00000 0.00730 0.00599 0.00624 0.00475 0.00557 0.00519 0.00258 O1 1.05050 0.67786 0.10529 1.00000 0.02197 0.04047 0.05831 -0.00359 0.00374 0.00663 0.04025 0.01180 0.00067 0.00050 0.00031 0.00000 0.00471 0.00407 0.00480 0.00341 0.00421 0.00375 0.00206 O2 0.51208 0.86477 0.13435 1.00000 0.02219 0.01869 0.03470 0.00214 0.00446 -0.00248 0.02519 0.01096 0.00060 0.00044 0.00025 0.00000 0.00455 0.00340 0.00426 0.00307 0.00353 0.00323 0.00181 O3 0.41883 0.80921 0.04916 1.00000 0.02831 0.04859 0.04190 -0.00194 -0.00498 -0.01163 0.03960 0.01096 0.00059 0.00050 0.00031 0.00000 0.00488 0.00429 0.00474 0.00364 0.00395 0.00358 0.00211 O4 0.72601 0.95670 0.18106 1.00000 0.01491 0.04269 0.03646 -0.00229 -0.00174 -0.00851 0.03135 0.01136 0.00060 0.00048 0.00027 0.00000 0.00451 0.00388 0.00441 0.00344 0.00358 0.00362 0.00185 O5 0.89689 1.05836 0.16704 1.00000 0.03714 0.04029 0.05268 -0.00840 -0.00214 -0.00768 0.04337 0.01109 0.00068 0.00052 0.00033 0.00000 0.00522 0.00408 0.00484 0.00383 0.00441 0.00382 0.00215 O6 0.40653 1.05983 0.10316 1.00000 0.03295 0.03363 0.04318 -0.00289 -0.00297 -0.00204 0.03659 0.01133 0.00070 0.00051 0.00029 0.00000 0.00514 0.00385 0.00441 0.00341 0.00416 0.00371 0.00198 O7 0.34459 1.11899 0.19413 1.00000 0.03442 0.06675 0.05785 -0.01268 0.01267 0.00587 0.05301 0.01346 0.00074 0.00057 0.00035 0.00000 0.00527 0.00467 0.00516 0.00430 0.00462 0.00407 0.00241 O8 0.62693 1.10866 -0.00284 1.00000 0.05637 0.03813 0.05481 -0.00623 0.01156 -0.01292 0.04977 0.01154 0.00076 0.00049 0.00031 0.00000 0.00579 0.00405 0.00502 0.00373 0.00463 0.00394 0.00228 O9 0.78466 1.21074 -0.01538 1.00000 0.10000 0.12817 0.19958 -0.05745 0.07461 -0.03335 0.14258 0.01887 0.00097 0.00084 0.00053 0.00000 0.00775 0.00683 0.00825 0.00657 0.00647 0.00625 0.00433 O10 0.53778 1.26177 0.12926 1.00000 0.03564 0.03208 0.03342 -0.00476 -0.00389 0.00514 0.03371 0.01122 0.00062 0.00046 0.00028 0.00000 0.00502 0.00382 0.00455 0.00339 0.00362 0.00352 0.00200 O11 0.65500 1.22562 0.21020 1.00000 0.02563 0.04766 0.04746 -0.01051 -0.00509 0.00112 0.04025 0.01094 0.00065 0.00053 0.00029 0.00000 0.00485 0.00413 0.00454 0.00372 0.00383 0.00393 0.00205 S1 0.73700 0.71923 0.16899 1.00000 0.02811 0.03877 0.04413 0.00284 0.00342 0.00240 0.03700 0.00487 0.00027 0.00021 0.00012 0.00000 0.00205 0.00157 0.00182 0.00146 0.00165 0.00156 0.00082 Final Structure Factor Calculation for 01ESP301 in P2(1)2(1)2(1) Total number of l.s. parameters = 379 Maximum vector length = 511 Memory required = 3626 / 26068 wR2 = 0.1930 before cycle 5 for 5105 data and 2 / 379 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 0.0426 0.0100 ISOR U11 O9 -0.0570 0.0100 ISOR U33 O9 0.0574 0.0100 ISOR U23 O9 -0.0746 0.0100 ISOR U13 O9 0.0334 0.0100 ISOR U12 O9 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. 0. 0. 0. 0. 0. 0. 234. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.011 0.000 GooF = S = 0.904; Restrained GooF = 0.907 for 234 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0848 for 1634 Fo > 4sig(Fo) and 0.3088 for all 5105 data wR2 = 0.1930, GooF = S = 0.904, Restrained GooF = 0.907 for all data Flack x parameter = -0.1437 with esd 0.2442 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 = 42.00 for non-hydrogen and 32.00 for hydrogen atoms Principal mean square atomic displacements U 0.0363 0.0348 0.0078 C1 0.0514 0.0395 0.0291 C2 0.0559 0.0526 0.0297 C3 0.0541 0.0439 0.0354 C4 0.0713 0.0655 0.0265 C5 0.0452 0.0358 0.0326 C6 0.0471 0.0352 0.0149 C7 0.0363 0.0319 0.0280 C8 0.0539 0.0353 0.0130 C9 0.0483 0.0295 0.0177 C10 0.0474 0.0281 0.0158 C11 0.0539 0.0367 0.0333 C12 0.0644 0.0414 0.0206 C13 0.0247 0.0227 0.0066 C14 0.0411 0.0282 0.0159 C15 0.0445 0.0276 0.0214 C16 0.0518 0.0463 0.0310 C17 0.0547 0.0365 0.0226 C18 0.0426 0.0382 0.0300 C19 0.0391 0.0343 0.0134 C20 0.0617 0.0514 0.0189 C21 0.0980 0.0901 0.0666 C22 0.0318 0.0299 0.0115 C23 0.0537 0.0413 0.0217 C24 0.1049 0.0575 0.0474 C25 0.0645 0.0620 0.0366 C26 0.0513 0.0443 0.0254 C27 0.0595 0.0407 0.0314 C28 0.0994 0.0503 0.0191 N1 0.0505 0.0417 0.0287 N2 0.0592 0.0423 0.0193 O1 0.0362 0.0229 0.0165 O2 0.0539 0.0433 0.0216 O3 0.0454 0.0363 0.0123 O4 0.0571 0.0443 0.0287 O5 0.0445 0.0354 0.0299 O6 0.0759 0.0571 0.0260 O7 0.0727 0.0452 0.0314 O8 0.2705 0.0973 0.0600 O9 may be split into 0.7928 1.2034 -0.0080 and 0.7765 1.2181 -0.0228 0.0430 0.0306 0.0275 O10 0.0587 0.0377 0.0244 O11 0.0463 0.0376 0.0271 S1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.018 0.027 0.035 0.043 0.052 0.063 0.078 0.099 0.139 1.000 Number in group 549. 519. 492. 512. 526. 490. 509. 487. 511. 510. GooF 0.746 0.794 0.820 0.860 0.869 0.920 0.893 0.977 0.976 1.136 K -0.047 1.212 0.991 0.862 1.015 0.987 0.992 1.014 0.996 1.030 Resolution(A) 0.84 0.88 0.91 0.95 1.00 1.07 1.15 1.26 1.45 1.81 inf Number in group 527. 509. 497. 523. 499. 512. 514. 508. 506. 510. GooF 0.785 0.824 0.831 0.797 0.809 0.930 0.964 0.913 0.983 1.141 K 0.685 0.834 1.196 1.076 1.045 1.020 1.060 0.954 1.026 1.020 R1 0.560 0.523 0.458 0.402 0.321 0.271 0.221 0.149 0.097 0.048 Recommended weighting scheme: WGHT 0.0419 0.0000 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 3 5 0 3293.21 1980.78 6.05 0.181 2.00 8 5 1 4924.37 1378.60 5.76 0.151 1.19 0 8 0 94.83 437.22 4.11 0.085 1.50 -9 3 4 1036.31 167.42 3.50 0.053 1.14 2 10 0 406.02 18.42 3.48 0.017 1.17 -7 1 1 1904.04 1107.26 3.45 0.136 1.55 2 2 0 2215.84 2702.80 3.40 0.212 4.05 2 3 12 608.34 352.76 3.37 0.077 1.62 3 5 2 7717.31 6390.59 3.36 0.326 1.97 2 5 1 4556.52 3500.28 3.32 0.241 2.18 0 0 6 183.19 69.09 3.30 0.034 3.74 3 0 2 4631.44 3598.75 3.30 0.244 3.48 -5 7 11 -118.79 219.49 3.27 0.060 1.13 5 1 0 5577.95 4007.10 3.26 0.258 2.16 0 5 5 5897.76 5079.26 3.20 0.290 2.11 1 2 2 1312.05 1559.02 3.19 0.161 4.76 0 8 5 2147.30 1481.28 3.18 0.157 1.42 -1 8 11 144.87 434.93 3.13 0.085 1.20 2 5 0 4566.70 3810.59 3.08 0.252 2.19 -1 9 11 -32.33 146.33 3.08 0.049 1.11 5 0 3 1929.52 1416.95 3.07 0.153 2.11 -7 5 8 -151.10 274.98 3.07 0.068 1.19 5 8 3 863.41 1387.22 3.06 0.152 1.22 -8 2 20 1260.19 94.43 3.03 0.040 0.86 -5 1 2 402.02 159.74 3.01 0.051 2.12 -1 8 12 477.95 795.58 3.00 0.115 1.16 -3 5 2 7786.39 6431.70 2.98 0.327 1.97 9 9 7 1422.39 13.78 2.97 0.015 0.87 8 6 4 248.92 852.84 2.94 0.119 1.11 6 0 2 5385.28 4254.72 2.92 0.266 1.81 6 9 1 2634.40 1634.25 2.90 0.165 1.07 -5 1 5 742.22 467.04 2.87 0.088 1.95 1 7 10 40.64 186.12 2.85 0.056 1.35 -9 4 16 1053.99 59.39 2.83 0.031 0.88 6 1 1 1377.30 853.24 2.83 0.119 1.80 0 5 9 1574.00 1924.22 2.80 0.179 1.73 -4 5 9 173.19 396.35 2.79 0.081 1.46 5 0 2 13760.15 10617.74 2.78 0.420 2.16 5 2 7 858.76 576.67 2.78 0.098 1.74 1 1 11 573.28 377.28 2.78 0.079 1.98 3 8 1 403.22 611.85 2.78 0.101 1.38 2 7 6 1085.86 725.47 2.78 0.110 1.50 5 1 2 390.28 156.21 2.77 0.051 2.12 1 2 3 14126.03 16056.49 2.75 0.516 4.30 2 4 18 1005.67 1763.13 2.74 0.171 1.13 -6 3 3 331.89 654.78 2.73 0.104 1.62 6 2 0 3215.56 2384.79 2.73 0.199 1.75 2 6 5 1116.83 837.08 2.72 0.118 1.73 4 1 8 648.07 800.11 2.72 0.115 1.94 10 1 5 1024.71 238.03 2.70 0.063 1.06 FMAP and GRID set by program FMAP 2 3 25 GRID -1.136 -2 -2 1.136 2 2 R1 = 0.2582 for 2926 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.44 at 0.2351 0.2760 0.0614 [ 1.18 A from O9 ] Deepest hole -0.37 at 0.7569 0.4785 0.0684 [ 1.32 A from C12 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 3325 / 23299 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7351 1.2240 -0.0614 1.00000 0.05 0.44 1.18 O9 1.37 C25 2.09 H22B 2.19 H26C Q2 1 0.7434 0.7365 0.1104 1.00000 0.05 0.42 0.99 C10 1.32 C9 1.33 S1 1.69 C7 Q3 1 0.7444 0.9553 0.0317 1.00000 0.05 0.32 1.53 H14 2.00 C14 2.01 H15 2.09 H9A Q4 1 0.7371 0.7349 0.2269 1.00000 0.05 0.32 1.31 S1 2.35 H2 2.42 O7 2.84 H28C Q5 1 0.7647 0.8161 0.0647 1.00000 0.05 0.31 0.93 C9 0.94 C10 1.16 H9A 1.65 H9B Q6 1 0.9345 0.6917 0.0660 1.00000 0.05 0.30 1.03 C11 1.56 O1 1.74 N2 1.74 H8 Q7 1 0.7185 0.9367 0.2280 1.00000 0.05 0.30 1.08 O4 1.43 H19A 1.65 C18 1.81 C19 Q8 1 0.8581 0.4941 0.2599 1.00000 0.05 0.28 1.00 H2 1.11 C2 1.35 C3 1.39 H3 Q9 1 0.2343 1.1533 0.0712 1.00000 0.05 0.27 1.17 H22A 1.38 H22B 1.40 C22 2.07 C21 Q10 1 0.1443 0.9828 0.1765 1.00000 0.05 0.27 0.99 H22C 1.62 H3 1.88 C22 2.20 H2 Q11 1 0.5258 1.0404 0.0721 1.00000 0.05 0.27 1.18 C20 1.35 H15 1.44 C15 1.50 O6 Q12 1 0.9331 0.8937 0.0100 1.00000 0.05 0.26 0.70 H13B 1.31 C13 1.46 H13A 2.05 H13C Q13 1 0.2554 0.7263 0.0837 1.00000 0.05 0.26 1.31 H17C 1.80 C17 1.99 H17B 2.15 C16 Q14 1 0.9652 0.9760 0.0841 1.00000 0.05 0.26 0.61 H13A 1.15 C13 1.38 H13C 1.96 H13B Q15 1 0.9585 1.0785 0.0369 1.00000 0.05 0.26 1.56 H13A 2.38 C13 2.56 H26B 2.62 H13C Shortest distances between peaks (including symmetry equivalents) 2 5 1.42 8 10 1.44 1 9 1.48 14 15 1.62 3 5 1.84 12 14 1.97 3 12 2.25 12 15 2.31 2 6 2.39 5 6 2.39 5 12 2.41 4 7 2.42 2 4 2.62 3 14 2.71 6 12 2.73 3 11 2.76 3 15 2.78 10 14 2.86 5 14 2.95 Time profile in seconds ----------------------- 0.17: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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 0.02: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 2.13: 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 4.91: Structure factors and derivatives 5.42: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.86: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 15:46:17 Total CPU time: 13.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++