+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 14:02:08 on 29-Jul-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02SRC154 in C2/c CELL 0.71073 26.8598 10.0338 22.9758 90.000 124.152 90.000 ZERR 8.00 0.0029 0.0009 0.0029 0.000 0.011 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O P BR UNIT 264 200 8 16 8 8 V = 5124.29 F(000) = 2368.0 Mu = 1.70 mm-1 Cell Wt = 4627.36 Rho = 1.500 MERG 2 OMIT -3.00 55.00 OMIT 0 0 2 TEMP -153 SIZE 0.1 0.06 0.01 FMAP 2 PLAN 10 BOND $H L.S. 4 WGHT 0.052400 19.984600 EXTI 0.000000 FVAR 0.09326 H1B 2 -0.055508 0.093184 -0.012251 11.00000 0.00602 H1A 2 -0.066958 0.011990 0.025150 11.00000 0.07706 MOLE 1 BR1 6 0.154358 0.160551 0.032123 11.00000 0.03578 0.02340 = 0.03595 0.00038 0.01582 0.00109 MOLE 2 C1 1 0.103144 0.250429 0.194890 11.00000 0.02726 0.02024 = 0.02612 0.00012 0.00905 0.00443 C2 1 0.073233 0.140910 0.199658 11.00000 0.02989 0.02149 = 0.02691 0.00000 0.01128 0.00161 AFIX 43 H2 2 0.088091 0.105063 0.244877 11.00000 -1.20000 AFIX 0 C3 1 0.023681 0.083020 0.142416 11.00000 0.03187 0.01771 = 0.02883 0.00136 0.01492 -0.00116 C4 1 -0.008193 -0.031658 0.150736 11.00000 0.03023 0.02730 = 0.03056 -0.00379 0.01067 -0.00382 AFIX 137 H4A 2 0.012964 -0.055091 0.200617 11.00000 -1.50000 H4B 2 -0.008629 -0.108759 0.124269 11.00000 -1.50000 H4C 2 -0.049612 -0.005597 0.132727 11.00000 -1.50000 AFIX 0 C5 1 0.002572 0.130004 0.073748 11.00000 0.02183 0.02210 = 0.02990 -0.00910 0.00670 0.00072 C6 1 0.033929 0.237412 0.066717 11.00000 0.02839 0.02014 = 0.02665 -0.00328 0.00983 0.00345 C7 1 0.016602 0.281797 -0.003156 11.00000 0.02859 0.02299 = 0.02924 -0.00225 0.01016 0.00443 C8 1 0.049018 0.397330 -0.008264 11.00000 0.02946 0.01502 = 0.03142 0.00337 0.01265 0.00935 C9 1 0.034869 0.436954 -0.073605 11.00000 0.03240 0.02799 = 0.03552 0.00405 0.01461 0.00551 AFIX 43 H9 2 0.005256 0.389986 -0.114677 11.00000 -1.20000 AFIX 0 C10 1 0.064292 0.546251 -0.078932 11.00000 0.04480 0.02911 = 0.03133 0.00562 0.01830 0.00773 AFIX 43 H10 2 0.056036 0.571156 -0.123434 11.00000 -1.20000 AFIX 0 C11 1 0.105327 0.618105 -0.019671 11.00000 0.04604 0.02199 = 0.05010 0.00281 0.02987 -0.00161 AFIX 43 H11 2 0.124117 0.694158 -0.023954 11.00000 -1.20000 AFIX 0 C12 1 0.119457 0.580659 0.046022 11.00000 0.03159 0.02238 = 0.03685 0.00358 0.01670 0.00379 AFIX 43 H12 2 0.147637 0.630773 0.086594 11.00000 -1.20000 AFIX 0 C13 1 0.091890 0.468728 0.051925 11.00000 0.02613 0.02018 = 0.02749 0.00177 0.01088 0.00319 C14 1 0.109477 0.423475 0.121488 11.00000 0.02329 0.01772 = 0.03111 -0.00342 0.00846 0.00137 C15 1 0.082104 0.298571 0.127437 11.00000 0.02586 0.01799 = 0.02975 0.00034 0.01197 0.00244 C16 1 0.147517 0.463896 0.304738 11.00000 0.03184 0.01716 = 0.02619 0.00325 0.01430 0.00139 C17 1 0.183490 0.508530 0.373662 11.00000 0.03061 0.02465 = 0.02761 0.00446 0.00822 0.00033 AFIX 43 H17 2 0.219736 0.463169 0.406809 11.00000 -1.20000 AFIX 0 C18 1 0.166033 0.620406 0.393878 11.00000 0.02788 0.01964 = 0.03604 -0.00558 0.01183 -0.00445 AFIX 43 H18 2 0.190450 0.651318 0.441038 11.00000 -1.20000 AFIX 0 C19 1 0.114195 0.685649 0.346435 11.00000 0.03716 0.02389 = 0.03660 -0.00066 0.01977 0.00321 AFIX 43 H19 2 0.102820 0.761876 0.360886 11.00000 -1.20000 AFIX 0 C20 1 0.078075 0.642933 0.277970 11.00000 0.03152 0.02611 = 0.04080 0.00715 0.01816 0.00436 AFIX 43 H20 2 0.042345 0.690303 0.245203 11.00000 -1.20000 AFIX 0 C21 1 0.093904 0.530441 0.256793 11.00000 0.03311 0.02268 = 0.03827 -0.00315 0.01839 -0.00312 AFIX 43 H21 2 0.068403 0.498780 0.209893 11.00000 -1.20000 AFIX 0 C22 1 0.233950 0.333436 0.276951 11.00000 0.02938 0.01312 = 0.02735 0.00187 0.01111 0.00030 C23 1 0.280357 0.412999 0.326589 11.00000 0.03050 0.02018 = 0.02801 -0.00013 0.01530 -0.00051 AFIX 43 H23 2 0.275669 0.464323 0.357961 11.00000 -1.20000 AFIX 0 C24 1 0.333734 0.418376 0.330886 11.00000 0.03933 0.01749 = 0.02924 0.00335 0.01015 0.00015 AFIX 43 H24 2 0.365335 0.474911 0.364486 11.00000 -1.20000 AFIX 0 C25 1 0.341271 0.341099 0.286065 11.00000 0.02883 0.02620 = 0.03981 0.00846 0.01464 0.00537 AFIX 43 H25 2 0.378404 0.342770 0.289975 11.00000 -1.20000 AFIX 0 C26 1 0.294439 0.261656 0.235685 11.00000 0.03913 0.02280 = 0.03952 0.00177 0.02171 0.00343 AFIX 43 H26 2 0.299394 0.209579 0.204740 11.00000 -1.20000 AFIX 0 C27 1 0.240805 0.258003 0.230362 11.00000 0.03667 0.02229 = 0.03225 0.00123 0.01357 -0.00113 AFIX 43 H27 2 0.208534 0.204667 0.195314 11.00000 -1.20000 AFIX 0 C28 1 0.185838 0.190113 0.342115 11.00000 0.02649 0.02033 = 0.02860 -0.00228 0.01204 -0.00193 C29 1 0.160682 0.193331 0.380427 11.00000 0.03084 0.01923 = 0.03539 -0.00015 0.01448 0.00161 AFIX 43 H29 2 0.135939 0.266121 0.375419 11.00000 -1.20000 AFIX 0 C30 1 0.171627 0.089560 0.426531 11.00000 0.03621 0.02557 = 0.03602 -0.00014 0.01902 -0.00145 AFIX 43 H30 2 0.154097 0.090943 0.452732 11.00000 -1.20000 AFIX 0 C31 1 0.208127 -0.015403 0.433938 11.00000 0.03645 0.02121 = 0.03101 0.00220 0.01107 0.00083 AFIX 43 H31 2 0.215573 -0.086147 0.465344 11.00000 -1.20000 AFIX 0 C32 1 0.233718 -0.018414 0.396361 11.00000 0.03253 0.02288 = 0.04110 0.00108 0.01273 0.00607 AFIX 43 H32 2 0.259059 -0.090546 0.402209 11.00000 -1.20000 AFIX 0 C33 1 0.222549 0.084198 0.349682 11.00000 0.03152 0.02095 = 0.03007 0.00145 0.01275 -0.00016 AFIX 43 H33 2 0.239829 0.081970 0.323218 11.00000 -1.20000 AFIX 0 N1 3 -0.045853 0.073660 0.018165 11.00000 0.03967 0.03055 = 0.03046 0.00239 0.01388 -0.00175 O1 4 -0.023925 0.229826 -0.057559 11.00000 0.03437 0.02975 = 0.02684 -0.00289 0.00919 -0.00224 O2 4 0.145022 0.485493 0.174895 11.00000 0.03399 0.02247 = 0.03168 0.00011 0.01137 -0.00285 P1 5 0.166978 0.316542 0.275999 11.00000 0.02840 0.01938 = 0.02648 0.00001 0.01108 -0.00029 HKLF 4 1.0 1.00 -2.00 0.00 1.00 0.00 0.00 -1.00 1.00 1.00 Covalent radii and connectivity table for 02SRC154 in C2/c C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 BR 1.140 Br1 - no bonds found C1 - C2 C15 P1 C2 - C3 C1 C3 - C2 C5 C4 C4 - C3 C5 - N1 C3 C6 C6 - C15 C5 C7 C7 - O1 C6 C8 C8 - C9 C13 C7 C9 - C8 C10 C10 - C11 C9 C11 - C10 C12 C12 - C11 C13 C13 - C12 C8 C14 C14 - O2 C13 C15 C15 - C6 C1 C14 C16 - C17 C21 P1 C17 - C16 C18 C18 - C19 C17 C19 - C18 C20 C20 - C19 C21 C21 - C20 C16 C22 - C23 C27 P1 C23 - C22 C24 C24 - C23 C25 C25 - C26 C24 C26 - C27 C25 C27 - C26 C22 C28 - C29 C33 P1 C29 - C28 C30 C30 - C31 C29 C31 - C32 C30 C32 - C31 C33 C33 - C32 C28 N1 - C5 O1 - C7 O2 - C14 P1 - C22 C1 C16 C28 h k l Fo^2 Sigma Why rejected -4 0 1 4.77 0.96 observed but should be systematically absent -2 0 3 5.02 1.01 observed but should be systematically absent 9658 Reflections read, of which 364 rejected -28 =< h =< 28, -10 =< k =< 10, -22 =< l =< 24, Max. 2-theta = 43.92 2 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 8 2 0 13.50 0.82 3 6.84 1 1 1 405.02 18.81 2 150.65 8 2 1 21.73 0.84 4 4.99 -3 1 2 57.57 0.97 3 45.31 -1 1 2 34.35 0.91 2 26.02 1 1 2 9.81 0.73 3 4.44 8 2 2 35.11 1.74 3 13.02 -1 1 3 44.11 1.82 2 11.74 4 2 3 435.99 23.04 3 181.82 3 3 4 32.11 1.23 2 7.08 5 3 8 82.84 3.70 3 38.60 2 4 10 19.11 1.25 3 6.68 3 5 10 8.25 0.90 3 5.50 6 4 13 52.51 2.84 3 22.80 14 Inconsistent equivalents 3107 Unique reflections, of which 0 suppressed R(int) = 0.0739 R(sigma) = 0.0721 Friedel opposites merged Maximum memory for data reduction = 3148 / 38599 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 = 4104 / 448992 wR2 = 0.1219 before cycle 1 for 3107 data and 353 / 353 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0524 * P )^2 + 19.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09331 0.00028 0.181 OSF 2 0.00000 0.00012 -2.969 EXTI Mean shift/esd = 0.010 Maximum = -2.969 for EXTI Max. shift = 0.001 A for H1B Max. dU = 0.000 for H1B Least-squares cycle 2 Maximum vector length = 511 Memory required = 4104 / 448992 wR2 = 0.1219 before cycle 2 for 3107 data and 353 / 353 parameters GooF = S = 1.012; Restrained GooF = 1.012 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0524 * P )^2 + 19.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09326 0.00028 -0.187 OSF 2 0.00000 0.00012 -3.958 EXTI Mean shift/esd = 0.013 Maximum = -3.958 for EXTI Max. shift = 0.001 A for H1B Max. dU = 0.000 for H1B Least-squares cycle 3 Maximum vector length = 511 Memory required = 4104 / 448992 wR2 = 0.1219 before cycle 3 for 3107 data and 353 / 353 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0524 * P )^2 + 19.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09326 0.00028 0.000 OSF 2 0.00000 0.00012 -3.959 EXTI Mean shift/esd = 0.012 Maximum = -3.959 for EXTI Max. shift = 0.001 A for H1B Max. dU = 0.000 for H1B Least-squares cycle 4 Maximum vector length = 511 Memory required = 4104 / 448992 wR2 = 0.1219 before cycle 4 for 3107 data and 353 / 353 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0524 * P )^2 + 19.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09326 0.00028 0.000 OSF 2 0.00000 0.00012 -3.959 EXTI Mean shift/esd = 0.012 Maximum = -3.959 for EXTI Max. shift = 0.000 A for H1B Max. dU = 0.000 for H1B Largest correlation matrix elements -0.711 z N1 / U11 H1B 0.658 U13 C21 / U11 C21 0.639 U13 O1 / U33 O1 0.683 U13 Br1 / U33 Br1 0.655 U13 C3 / U33 C3 0.636 U13 C30 / U11 C30 0.680 U13 Br1 / U11 Br1 0.651 U13 C21 / U33 C21 0.635 U13 C3 / U11 C3 0.675 U13 C20 / U33 C20 0.647 U13 C11 / U11 C11 0.633 U13 C16 / U11 C16 0.670 U13 C19 / U33 C19 0.647 U13 O2 / U33 O2 0.631 U13 C7 / U33 C7 0.668 U13 C26 / U33 C26 0.646 U13 C19 / U11 C19 0.630 U12 C11 / U23 C11 0.661 U13 C11 / U33 C11 0.645 U13 C10 / U33 C10 0.630 U13 C2 / U33 C2 0.659 U13 C16 / U33 C16 0.639 U13 C23 / U33 C23 0.629 U13 P1 / U33 P1 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.0881 0.1051 0.2449 43 0.950 0.000 C2 C3 C1 H4A 0.0130 -0.0551 0.2006 137 0.980 0.000 C4 C3 H4A H4B -0.0086 -0.1088 0.1243 137 0.980 0.000 C4 C3 H4A H4C -0.0496 -0.0056 0.1327 137 0.980 0.000 C4 C3 H4A H9 0.0053 0.3900 -0.1147 43 0.950 0.000 C9 C8 C10 H10 0.0560 0.5712 -0.1234 43 0.950 0.000 C10 C11 C9 H11 0.1241 0.6942 -0.0240 43 0.950 0.000 C11 C10 C12 H12 0.1476 0.6308 0.0866 43 0.950 0.000 C12 C11 C13 H17 0.2197 0.4632 0.4068 43 0.950 0.000 C17 C16 C18 H18 0.1904 0.6513 0.4410 43 0.950 0.000 C18 C19 C17 H19 0.1028 0.7619 0.3609 43 0.950 0.000 C19 C18 C20 H20 0.0423 0.6903 0.2452 43 0.950 0.000 C20 C19 C21 H21 0.0684 0.4988 0.2099 43 0.950 0.000 C21 C20 C16 H23 0.2757 0.4643 0.3580 43 0.950 0.000 C23 C22 C24 H24 0.3653 0.4749 0.3645 43 0.950 0.000 C24 C23 C25 H25 0.3784 0.3428 0.2900 43 0.950 0.000 C25 C26 C24 H26 0.2994 0.2096 0.2047 43 0.950 0.000 C26 C27 C25 H27 0.2085 0.2047 0.1953 43 0.950 0.000 C27 C26 C22 H29 0.1359 0.2661 0.3754 43 0.950 0.000 C29 C28 C30 H30 0.1541 0.0909 0.4527 43 0.950 0.000 C30 C31 C29 H31 0.2156 -0.0861 0.4653 43 0.950 0.000 C31 C32 C30 H32 0.2591 -0.0905 0.4022 43 0.950 0.000 C32 C31 C33 H33 0.2398 0.0820 0.3232 43 0.950 0.000 C33 C32 C28 02SRC154 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq H1B -0.05552 0.09312 -0.01211 1.00000 0.00472 0.12804 0.00247 0.00563 0.00273 0.00000 0.01974 H1A -0.06703 0.01175 0.02514 1.00000 0.07777 0.17388 0.00320 0.00767 0.00372 0.00000 0.02674 Br1 0.15436 0.16055 0.03212 1.00000 0.03578 0.02340 0.03595 0.00038 0.01582 0.00109 0.03407 0.00126 0.00002 0.00005 0.00003 0.00000 0.00037 0.00035 0.00038 0.00026 0.00029 0.00026 0.00025 C1 0.10314 0.25043 0.19489 1.00000 0.02725 0.02024 0.02611 0.00012 0.00905 0.00443 0.02778 0.01198 0.00023 0.00049 0.00027 0.00000 0.00294 0.00299 0.00314 0.00250 0.00263 0.00256 0.00130 C2 0.07323 0.14091 0.19966 1.00000 0.02989 0.02148 0.02692 0.00000 0.01128 0.00161 0.02865 0.01216 0.00023 0.00049 0.00028 0.00000 0.00306 0.00301 0.00302 0.00251 0.00269 0.00263 0.00131 H2 0.08809 0.10506 0.24488 1.00000 0.03437 0.00000 0.00000 C3 0.02368 0.08302 0.14242 1.00000 0.03187 0.01771 0.02883 0.00136 0.01492 -0.00116 0.02729 0.01214 0.00023 0.00049 0.00027 0.00000 0.00316 0.00279 0.00328 0.00253 0.00285 0.00260 0.00129 C4 -0.00819 -0.03166 0.15074 1.00000 0.03023 0.02730 0.03056 -0.00380 0.01067 -0.00382 0.03286 0.01213 0.00024 0.00050 0.00028 0.00000 0.00308 0.00308 0.00320 0.00260 0.00271 0.00268 0.00136 H4A 0.01296 -0.05509 0.20062 1.00000 0.04929 0.00000 0.00000 H4B -0.00863 -0.10876 0.12427 1.00000 0.04929 0.00000 0.00000 H4C -0.04961 -0.00560 0.13273 1.00000 0.04929 0.00000 0.00000 C5 0.00257 0.13001 0.07375 1.00000 0.02181 0.02212 0.02987 -0.00912 0.00667 0.00071 0.02888 0.01192 0.00023 0.00051 0.00028 0.00000 0.00296 0.00298 0.00338 0.00264 0.00280 0.00262 0.00135 C6 0.03393 0.23741 0.06672 1.00000 0.02839 0.02013 0.02666 -0.00327 0.00983 0.00345 0.02813 0.01193 0.00023 0.00050 0.00027 0.00000 0.00307 0.00291 0.00322 0.00254 0.00275 0.00263 0.00132 C7 0.01660 0.28180 -0.00316 1.00000 0.02859 0.02299 0.02924 -0.00224 0.01016 0.00443 0.03026 0.01312 0.00024 0.00053 0.00029 0.00000 0.00316 0.00301 0.00350 0.00267 0.00298 0.00266 0.00136 C8 0.04902 0.39733 -0.00827 1.00000 0.02946 0.01502 0.03141 0.00336 0.01266 0.00934 0.02771 0.01222 0.00023 0.00049 0.00027 0.00000 0.00310 0.00270 0.00343 0.00254 0.00283 0.00260 0.00132 C9 0.03487 0.43695 -0.07360 1.00000 0.03240 0.02799 0.03552 0.00405 0.01460 0.00551 0.03441 0.01349 0.00025 0.00053 0.00030 0.00000 0.00322 0.00321 0.00357 0.00273 0.00290 0.00277 0.00141 H9 0.00526 0.38999 -0.11468 1.00000 0.04129 0.00000 0.00000 C10 0.06429 0.54625 -0.07893 1.00000 0.04479 0.02911 0.03132 0.00563 0.01829 0.00773 0.03676 0.01364 0.00026 0.00054 0.00030 0.00000 0.00363 0.00328 0.00337 0.00282 0.00309 0.00300 0.00147 H10 0.05604 0.57115 -0.12343 1.00000 0.04411 0.00000 0.00000 C11 0.10533 0.61810 -0.01967 1.00000 0.04604 0.02199 0.05010 0.00281 0.02987 -0.00161 0.03780 0.01417 0.00026 0.00054 0.00032 0.00000 0.00369 0.00301 0.00412 0.00296 0.00340 0.00287 0.00150 H11 0.12412 0.69416 -0.02395 1.00000 0.04536 0.00000 0.00000 C12 0.11946 0.58066 0.04602 1.00000 0.03158 0.02238 0.03685 0.00358 0.01670 0.00379 0.03165 0.01327 0.00024 0.00051 0.00030 0.00000 0.00320 0.00304 0.00350 0.00267 0.00285 0.00271 0.00136 H12 0.14764 0.63077 0.08659 1.00000 0.03797 0.00000 0.00000 C13 0.09189 0.46873 0.05193 1.00000 0.02612 0.02018 0.02749 0.00177 0.01088 0.00319 0.02688 0.01203 0.00023 0.00049 0.00027 0.00000 0.00290 0.00294 0.00318 0.00254 0.00264 0.00255 0.00129 C14 0.10948 0.42347 0.12149 1.00000 0.02329 0.01772 0.03110 -0.00342 0.00846 0.00138 0.02776 0.01274 0.00023 0.00050 0.00029 0.00000 0.00298 0.00286 0.00335 0.00272 0.00278 0.00256 0.00131 C15 0.08210 0.29857 0.12744 1.00000 0.02585 0.01799 0.02974 0.00034 0.01196 0.00244 0.02652 0.01178 0.00023 0.00048 0.00027 0.00000 0.00297 0.00279 0.00325 0.00250 0.00270 0.00248 0.00129 C16 0.14752 0.46390 0.30474 1.00000 0.03184 0.01716 0.02619 0.00325 0.01430 0.00139 0.02615 0.01202 0.00023 0.00048 0.00027 0.00000 0.00313 0.00269 0.00314 0.00244 0.00276 0.00253 0.00127 C17 0.18349 0.50853 0.37366 1.00000 0.03061 0.02465 0.02761 0.00446 0.00822 0.00033 0.03206 0.01235 0.00024 0.00052 0.00028 0.00000 0.00301 0.00311 0.00326 0.00263 0.00271 0.00272 0.00135 H17 0.21974 0.46317 0.40681 1.00000 0.03847 0.00000 0.00000 C18 0.16603 0.62041 0.39388 1.00000 0.02789 0.01964 0.03605 -0.00559 0.01183 -0.00446 0.03120 0.01249 0.00023 0.00050 0.00030 0.00000 0.00319 0.00294 0.00335 0.00258 0.00286 0.00260 0.00137 H18 0.19045 0.65132 0.44104 1.00000 0.03744 0.00000 0.00000 C19 0.11419 0.68565 0.34643 1.00000 0.03716 0.02389 0.03659 -0.00066 0.01976 0.00321 0.03306 0.01295 0.00025 0.00053 0.00029 0.00000 0.00338 0.00305 0.00359 0.00272 0.00313 0.00279 0.00140 H19 0.10282 0.76188 0.36089 1.00000 0.03968 0.00000 0.00000 C20 0.07808 0.64293 0.27797 1.00000 0.03152 0.02611 0.04080 0.00715 0.01816 0.00436 0.03398 0.01310 0.00025 0.00051 0.00030 0.00000 0.00317 0.00318 0.00374 0.00279 0.00303 0.00274 0.00141 H20 0.04235 0.69030 0.24520 1.00000 0.04077 0.00000 0.00000 C21 0.09390 0.53044 0.25679 1.00000 0.03311 0.02268 0.03827 -0.00316 0.01839 -0.00312 0.03225 0.01296 0.00024 0.00051 0.00030 0.00000 0.00332 0.00313 0.00341 0.00269 0.00298 0.00272 0.00137 H21 0.06840 0.49878 0.20989 1.00000 0.03870 0.00000 0.00000 C22 0.23395 0.33344 0.27695 1.00000 0.02938 0.01312 0.02735 0.00187 0.01111 0.00030 0.02592 0.01178 0.00023 0.00047 0.00026 0.00000 0.00301 0.00260 0.00298 0.00251 0.00264 0.00252 0.00125 C23 0.28036 0.41300 0.32659 1.00000 0.03050 0.02019 0.02801 -0.00013 0.01530 -0.00050 0.02684 0.01209 0.00023 0.00049 0.00027 0.00000 0.00325 0.00290 0.00307 0.00252 0.00276 0.00263 0.00128 H23 0.27567 0.46432 0.35796 1.00000 0.03221 0.00000 0.00000 C24 0.33373 0.41838 0.33089 1.00000 0.03933 0.01749 0.02924 0.00334 0.01014 0.00015 0.03366 0.01307 0.00025 0.00051 0.00029 0.00000 0.00368 0.00297 0.00323 0.00260 0.00291 0.00266 0.00145 H24 0.36533 0.47491 0.36449 1.00000 0.04039 0.00000 0.00000 C25 0.34127 0.34110 0.28606 1.00000 0.02883 0.02620 0.03980 0.00846 0.01463 0.00537 0.03414 0.01315 0.00025 0.00052 0.00029 0.00000 0.00311 0.00311 0.00349 0.00298 0.00291 0.00279 0.00141 H25 0.37840 0.34277 0.28997 1.00000 0.04097 0.00000 0.00000 C26 0.29444 0.26166 0.23568 1.00000 0.03913 0.02280 0.03952 0.00178 0.02171 0.00343 0.03402 0.01345 0.00026 0.00053 0.00030 0.00000 0.00364 0.00310 0.00352 0.00277 0.00317 0.00282 0.00141 H26 0.29939 0.20958 0.20474 1.00000 0.04082 0.00000 0.00000 C27 0.24081 0.25800 0.23036 1.00000 0.03667 0.02228 0.03225 0.00122 0.01357 -0.00114 0.03356 0.01319 0.00026 0.00052 0.00029 0.00000 0.00357 0.00304 0.00340 0.00269 0.00295 0.00269 0.00142 H27 0.20853 0.20467 0.19531 1.00000 0.04027 0.00000 0.00000 C28 0.18584 0.19011 0.34211 1.00000 0.02650 0.02033 0.02860 -0.00228 0.01205 -0.00192 0.02701 0.01162 0.00023 0.00048 0.00027 0.00000 0.00296 0.00297 0.00309 0.00243 0.00269 0.00250 0.00132 C29 0.16068 0.19333 0.38043 1.00000 0.03084 0.01923 0.03539 -0.00015 0.01448 0.00161 0.03073 0.01222 0.00024 0.00050 0.00028 0.00000 0.00310 0.00299 0.00327 0.00259 0.00280 0.00253 0.00137 H29 0.13594 0.26612 0.37542 1.00000 0.03688 0.00000 0.00000 C30 0.17163 0.08956 0.42653 1.00000 0.03621 0.02557 0.03602 -0.00014 0.01901 -0.00145 0.03329 0.01245 0.00024 0.00052 0.00029 0.00000 0.00338 0.00320 0.00337 0.00279 0.00293 0.00288 0.00139 H30 0.15410 0.09094 0.45273 1.00000 0.03995 0.00000 0.00000 C31 0.20813 -0.01540 0.43394 1.00000 0.03644 0.02120 0.03101 0.00221 0.01106 0.00083 0.03385 0.01231 0.00025 0.00053 0.00029 0.00000 0.00324 0.00303 0.00324 0.00257 0.00289 0.00283 0.00141 H31 0.21557 -0.08615 0.46534 1.00000 0.04062 0.00000 0.00000 C32 0.23372 -0.01841 0.39636 1.00000 0.03253 0.02288 0.04111 0.00109 0.01273 0.00607 0.03651 0.01266 0.00025 0.00054 0.00030 0.00000 0.00328 0.00315 0.00358 0.00287 0.00304 0.00267 0.00147 H32 0.25906 -0.09055 0.40221 1.00000 0.04381 0.00000 0.00000 C33 0.22255 0.08420 0.34968 1.00000 0.03152 0.02095 0.03007 0.00145 0.01276 -0.00017 0.02999 0.01201 0.00024 0.00050 0.00028 0.00000 0.00310 0.00302 0.00309 0.00262 0.00269 0.00267 0.00133 H33 0.23983 0.08197 0.32322 1.00000 0.03599 0.00000 0.00000 N1 -0.04585 0.07364 0.01819 1.00000 0.03976 0.03064 0.03037 0.00248 0.01382 -0.00167 0.03680 0.01373 0.00026 0.00059 0.00038 0.00000 0.00388 0.00339 0.00392 0.00312 0.00351 0.00277 0.00154 O1 -0.02392 0.22983 -0.05756 1.00000 0.03437 0.02975 0.02684 -0.00289 0.00919 -0.00223 0.03468 0.00870 0.00017 0.00035 0.00019 0.00000 0.00216 0.00210 0.00223 0.00184 0.00199 0.00192 0.00094 O2 0.14502 0.48549 0.17489 1.00000 0.03399 0.02247 0.03167 0.00012 0.01137 -0.00285 0.03324 0.00863 0.00016 0.00034 0.00019 0.00000 0.00213 0.00199 0.00227 0.00187 0.00196 0.00189 0.00092 P1 0.16698 0.31654 0.27600 1.00000 0.02840 0.01938 0.02648 0.00001 0.01108 -0.00029 0.02712 0.00313 0.00006 0.00013 0.00007 0.00000 0.00078 0.00075 0.00080 0.00064 0.00067 0.00064 0.00039 Final Structure Factor Calculation for 02SRC154 in C2/c Total number of l.s. parameters = 353 Maximum vector length = 511 Memory required = 3751 / 25039 wR2 = 0.1219 before cycle 5 for 3107 data and 0 / 353 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0524 * P )^2 + 19.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0493 for 2378 Fo > 4sig(Fo) and 0.0726 for all 3107 data wR2 = 0.1219, GooF = S = 1.011, Restrained GooF = 1.011 for all data Occupancy sum of asymmetric unit = 38.00 for non-hydrogen and 25.00 for hydrogen atoms Principal mean square atomic displacements U 0.0457 0.0332 0.0233 Br1 0.0413 0.0240 0.0181 C1 0.0395 0.0253 0.0212 C2 0.0360 0.0285 0.0173 C3 0.0450 0.0311 0.0225 C4 0.0494 0.0213 0.0160 C5 0.0427 0.0239 0.0178 C6 0.0451 0.0254 0.0203 C7 0.0421 0.0307 0.0104 C8 0.0444 0.0351 0.0236 C9 0.0515 0.0349 0.0239 C10 0.0507 0.0418 0.0209 C11 0.0412 0.0329 0.0208 C12 0.0365 0.0256 0.0186 C13 0.0448 0.0218 0.0167 C14 0.0368 0.0255 0.0173 C15 0.0352 0.0272 0.0161 C16 0.0485 0.0268 0.0208 C17 0.0474 0.0294 0.0167 C18 0.0402 0.0363 0.0227 C19 0.0462 0.0332 0.0226 C20 0.0411 0.0340 0.0217 C21 0.0395 0.0253 0.0129 C22 0.0324 0.0279 0.0202 C23 0.0566 0.0278 0.0166 C24 0.0493 0.0327 0.0205 C25 0.0403 0.0396 0.0221 C26 0.0483 0.0304 0.0220 C27 0.0355 0.0261 0.0194 C28 0.0432 0.0300 0.0190 C29 0.0391 0.0354 0.0254 C30 0.0522 0.0287 0.0207 C31 0.0566 0.0330 0.0199 C32 0.0413 0.0279 0.0207 C33 0.0510 0.0314 0.0280 N1 0.0497 0.0311 0.0233 O1 0.0494 0.0285 0.0218 O2 0.0374 0.0246 0.0194 P1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.029 0.043 0.057 0.075 0.094 0.118 0.148 0.203 1.000 Number in group 325. 299. 314. 311. 310. 310. 309. 306. 310. 313. GooF 1.011 1.024 1.077 1.002 1.030 1.043 0.953 1.037 0.914 1.041 K 1.657 1.131 1.006 0.964 1.002 0.977 0.978 1.000 1.015 1.038 Resolution(A) 0.95 0.98 1.02 1.07 1.13 1.20 1.29 1.42 1.63 2.03 inf Number in group 312. 310. 316. 304. 311. 317. 311. 307. 308. 311. GooF 1.008 0.979 0.974 0.988 0.949 0.948 1.033 1.016 1.070 1.161 K 1.061 1.079 1.041 1.033 1.008 0.999 1.003 1.016 1.038 1.015 R1 0.129 0.129 0.105 0.093 0.070 0.063 0.060 0.057 0.044 0.043 Recommended weighting scheme: WGHT 0.0428 20.4506 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) -6 4 5 7890.52 5404.31 4.89 0.118 2.13 -8 2 3 1638.68 887.77 3.38 0.048 2.77 -15 5 10 116.76 936.30 3.26 0.049 1.31 -1 1 1 663.99 290.25 3.17 0.027 9.10 -21 3 20 5746.05 3908.69 3.11 0.100 1.01 -8 4 12 499.19 1041.77 3.09 0.052 1.52 -10 0 10 15663.13 11891.16 3.08 0.175 2.17 8 4 11 576.79 121.54 3.07 0.018 1.08 -1 7 14 808.71 87.93 3.04 0.015 1.00 -20 0 18 27879.85 21920.83 2.97 0.238 1.16 -1 3 8 8330.39 6621.95 2.94 0.131 2.01 4 2 6 7153.16 5573.61 2.92 0.120 2.06 -20 2 23 2260.68 1296.72 2.84 0.058 0.96 0 2 0 485.00 184.54 2.78 0.022 5.02 -22 2 19 15395.92 12252.10 2.77 0.178 1.05 -2 2 8 10299.76 8436.02 2.77 0.148 2.34 -26 2 12 1246.59 28.23 2.76 0.009 1.01 0 6 16 17447.78 14196.50 2.65 0.191 0.97 6 8 4 21154.33 17064.36 2.64 0.210 1.11 -2 4 6 -0.21 225.43 2.64 0.024 2.06 -10 4 15 143.39 623.01 2.63 0.040 1.31 -19 1 6 513.98 70.97 2.63 0.014 1.36 10 2 1 1446.63 470.10 2.62 0.035 1.92 12 6 7 966.48 0.98 2.60 0.002 1.00 18 2 2 1161.80 1823.65 2.59 0.069 1.12 -10 8 3 2154.35 3222.00 2.59 0.091 1.13 -16 6 14 13716.83 11270.91 2.58 0.171 1.10 -9 3 20 16.31 537.37 2.57 0.037 1.07 -4 2 2 1836.58 1325.89 2.56 0.058 4.02 -21 3 22 2625.83 1581.12 2.55 0.064 0.96 18 0 6 4031.35 2791.39 2.53 0.085 0.98 10 8 5 3659.38 2488.95 2.51 0.080 0.98 -3 7 1 23204.03 19479.88 2.50 0.224 1.41 11 7 2 -227.80 611.51 2.49 0.040 1.12 6 4 15 614.14 33.11 2.49 0.009 0.96 -7 5 2 549.55 905.16 2.48 0.048 1.76 -14 2 13 269.13 696.32 2.47 0.042 1.54 0 4 9 1642.61 2298.36 2.46 0.077 1.62 -22 2 21 7277.02 5642.29 2.45 0.121 0.99 -4 6 9 166.42 568.06 2.44 0.038 1.39 -7 7 4 24163.54 20261.29 2.44 0.229 1.34 4 6 14 1268.47 320.20 2.42 0.029 0.96 -8 4 4 3150.47 2469.96 2.41 0.080 2.01 -19 5 10 1058.93 415.11 2.41 0.033 1.15 -1 1 15 3705.29 4676.23 2.41 0.110 1.30 -24 4 12 2546.43 1643.30 2.40 0.065 1.02 -23 3 13 949.83 237.58 2.37 0.025 1.10 0 6 6 -152.92 89.13 2.36 0.015 1.48 -2 8 10 1173.79 1791.32 2.36 0.068 1.07 -1 9 6 50317.02 43084.63 2.35 0.333 1.06 Bond lengths and angles C1 - Distance Angles C2 1.4014 (0.0072) C15 1.4040 (0.0072) 117.58 (0.46) P1 1.8070 (0.0052) 117.45 (0.39) 124.96 (0.40) C1 - C2 C15 C2 - Distance Angles C3 1.3687 (0.0072) C1 1.4014 (0.0072) 123.27 (0.49) H2 0.9500 118.37 118.37 C2 - C3 C1 C3 - Distance Angles C2 1.3687 (0.0072) C5 1.4242 (0.0073) 119.45 (0.47) C4 1.5091 (0.0070) 121.11 (0.47) 119.43 (0.45) C3 - C2 C5 C4 - Distance Angles C3 1.5091 (0.0070) H4A 0.9800 109.47 H4B 0.9800 109.47 109.47 H4C 0.9800 109.47 109.47 109.47 C4 - C3 H4A H4B C5 - Distance Angles N1 1.3330 (0.0077) C3 1.4242 (0.0073) 119.21 (0.57) C6 1.4317 (0.0075) 122.06 (0.56) 118.73 (0.45) C5 - N1 C3 C6 - Distance Angles C15 1.4037 (0.0072) C5 1.4317 (0.0075) 119.30 (0.47) C7 1.4674 (0.0076) 120.26 (0.48) 120.43 (0.46) C6 - C15 C5 C7 - Distance Angles O1 1.2213 (0.0061) C6 1.4674 (0.0076) 122.90 (0.50) C8 1.4935 (0.0076) 118.36 (0.48) 118.73 (0.47) C7 - O1 C6 C8 - Distance Angles C9 1.3841 (0.0075) C13 1.4013 (0.0072) 119.78 (0.49) C7 1.4935 (0.0076) 119.41 (0.48) 120.77 (0.47) C8 - C9 C13 C9 - Distance Angles C8 1.3841 (0.0075) C10 1.3967 (0.0077) 119.75 (0.52) H9 0.9500 120.12 120.12 C9 - C8 C10 C10 - Distance Angles C11 1.3797 (0.0079) C9 1.3967 (0.0077) 120.11 (0.54) H10 0.9500 119.94 119.94 C10 - C11 C9 C11 - Distance Angles C10 1.3797 (0.0079) C12 1.3857 (0.0077) 120.78 (0.53) H11 0.9500 119.61 119.61 C11 - C10 C12 C12 - Distance Angles C11 1.3857 (0.0077) C13 1.3931 (0.0072) 119.28 (0.52) H12 0.9500 120.36 120.36 C12 - C11 C13 C13 - Distance Angles C12 1.3931 (0.0072) C8 1.4013 (0.0072) 120.22 (0.49) C14 1.4615 (0.0074) 119.59 (0.48) 120.16 (0.46) C13 - C12 C8 C14 - Distance Angles O2 1.2203 (0.0059) C13 1.4615 (0.0074) 122.09 (0.47) C15 1.4976 (0.0073) 118.82 (0.47) 119.07 (0.46) C14 - O2 C13 C15 - Distance Angles C6 1.4037 (0.0072) C1 1.4040 (0.0072) 121.46 (0.47) C14 1.4976 (0.0073) 120.07 (0.47) 118.34 (0.45) C15 - C6 C1 C16 - Distance Angles C17 1.3871 (0.0073) C21 1.3971 (0.0074) 119.67 (0.49) P1 1.8119 (0.0052) 121.40 (0.40) 118.89 (0.40) C16 - C17 C21 C17 - Distance Angles C16 1.3871 (0.0073) C18 1.3929 (0.0074) 119.46 (0.51) H17 0.9500 120.27 120.27 C17 - C16 C18 C18 - Distance Angles C19 1.3606 (0.0075) C17 1.3929 (0.0074) 120.35 (0.53) H18 0.9500 119.83 119.83 C18 - C19 C17 C19 - Distance Angles C18 1.3606 (0.0076) C20 1.3733 (0.0077) 120.97 (0.52) H19 0.9500 119.51 119.51 C19 - C18 C20 C20 - Distance Angles C19 1.3733 (0.0077) C21 1.3870 (0.0074) 119.82 (0.53) H20 0.9500 120.09 120.09 C20 - C19 C21 C21 - Distance Angles C20 1.3870 (0.0074) C16 1.3971 (0.0074) 119.71 (0.52) H21 0.9500 120.15 120.15 C21 - C20 C16 C22 - Distance Angles C23 1.3768 (0.0072) C27 1.4049 (0.0075) 119.90 (0.50) P1 1.7947 (0.0054) 120.00 (0.41) 119.93 (0.41) C22 - C23 C27 C23 - Distance Angles C22 1.3768 (0.0072) C24 1.3817 (0.0075) 120.16 (0.50) H23 0.9500 119.92 119.92 C23 - C22 C24 C24 - Distance Angles C23 1.3817 (0.0075) C25 1.3917 (0.0078) 120.10 (0.52) H24 0.9500 119.95 119.95 C24 - C23 C25 C25 - Distance Angles C26 1.3866 (0.0078) C24 1.3917 (0.0078) 119.82 (0.54) H25 0.9500 120.09 120.09 C25 - C26 C24 C26 - Distance Angles C27 1.3761 (0.0079) C25 1.3866 (0.0078) 120.22 (0.54) H26 0.9500 119.89 119.89 C26 - C27 C25 C27 - Distance Angles C26 1.3761 (0.0079) C22 1.4049 (0.0076) 119.76 (0.53) H27 0.9500 120.12 120.12 C27 - C26 C22 C28 - Distance Angles C29 1.3785 (0.0075) C33 1.3926 (0.0071) 120.31 (0.48) P1 1.8192 (0.0052) 120.69 (0.39) 118.82 (0.41) C28 - C29 C33 C29 - Distance Angles C28 1.3785 (0.0075) C30 1.3939 (0.0074) 119.86 (0.49) H29 0.9500 120.07 120.07 C29 - C28 C30 C30 - Distance Angles C31 1.3828 (0.0075) C29 1.3939 (0.0074) 119.66 (0.53) H30 0.9500 120.17 120.17 C30 - C31 C29 C31 - Distance Angles C32 1.3730 (0.0077) C30 1.3828 (0.0075) 120.67 (0.51) H31 0.9500 119.67 119.67 C31 - C32 C30 C32 - Distance Angles C31 1.3730 (0.0077) C33 1.3925 (0.0075) 120.04 (0.51) H32 0.9500 119.98 119.98 C32 - C31 C33 C33 - Distance Angles C32 1.3925 (0.0075) C28 1.3926 (0.0071) 119.45 (0.52) H33 0.9500 120.27 120.27 C33 - C32 C28 N1 - Distance Angles C5 1.3330 (0.0077) H1B 0.6224 (0.0484) 120.54 (5.50) H1A 0.9148 (0.0754) 119.27 (4.59) 119.91 (7.60) N1 - C5 H1B O1 - Distance Angles C7 1.2213 (0.0061) O1 - O2 - Distance Angles C14 1.2203 (0.0059) O2 - P1 - Distance Angles C22 1.7947 (0.0054) C1 1.8070 (0.0052) 114.30 (0.25) C16 1.8119 (0.0052) 114.25 (0.24) 112.00 (0.24) C28 1.8192 (0.0052) 104.38 (0.24) 105.27 (0.24) 105.47 (0.24) P1 - C22 C1 C16 FMAP and GRID set by program FMAP 2 1 36 GRID -0.758 -2 -1 0.758 2 1 R1 = 0.0694 for 3107 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.50 at 0.1519 0.5149 0.0299 [ 1.30 A from C12 ] Deepest hole -0.42 at 0.1433 0.0957 0.0898 [ 1.65 A from BR1 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 3694 / 36624 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1519 0.5149 0.0299 1.00000 0.05 0.50 1.30 C12 1.53 C11 1.80 H12 2.00 C13 Q2 1 0.0995 0.1565 -0.0302 1.00000 0.05 0.44 1.36 BR1 1.93 H1A 2.22 H4B 2.47 H4C Q3 1 0.2048 0.1621 0.0926 1.00000 0.05 0.40 1.28 BR1 2.20 H23 2.34 H27 2.44 H26 Q4 1 0.2428 0.1648 0.4106 1.00000 0.05 0.34 1.43 C33 1.48 C28 1.86 C32 1.93 C29 Q5 1 0.1611 0.0185 0.2705 1.00000 0.05 0.33 1.76 C33 1.86 H33 1.91 H2 2.12 H25 Q6 1 0.0232 0.1651 0.1582 1.00000 0.05 0.33 0.90 C3 1.16 C2 1.73 C5 1.86 H2 Q7 1 0.1961 0.6571 0.5106 1.00000 0.05 0.32 1.52 H18 1.79 H32 2.23 H31 2.34 BR1 Q8 1 0.3585 0.1870 0.2084 1.00000 0.05 0.32 1.56 H26 1.61 C20 1.78 C19 1.90 C21 Q9 1 0.1244 0.1482 0.0476 1.00000 0.05 0.31 1.05 BR1 2.20 H1A 2.56 H24 2.78 C7 Q10 1 0.1792 0.1556 0.0133 1.00000 0.05 0.31 0.98 BR1 1.97 H31 2.68 H18 2.73 H30 Shortest distances between peaks (including symmetry equivalents) 2 9 1.52 3 10 1.55 2 10 1.78 3 9 1.80 7 10 1.94 9 10 2.02 1 7 2.27 3 7 2.53 2 3 2.65 1 4 2.79 2 7 2.89 Time profile in seconds ----------------------- 0.23: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.02: Analyse other restraints etc. 1.34: 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 1.78: Structure factors and derivatives 2.89: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.73: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.17: Fourier summations 0.09: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 14:02:16 Total CPU time: 7.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++