+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 10:33:36 on 02-Oct-2003 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P2(1)/c CELL 0.71069 8.8770 17.6790 15.7110 90.000 103.859 90.000 ZERR 4.00 0.0050 0.0050 0.0050 0.005 0.005 0.005 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H P FE BR UNIT 88 136 8 4 8 V = 2393.85 F(000) = 1168.0 Mu = 4.11 mm-1 Cell Wt = 2304.41 Rho = 1.598 MERG 2 OMIT -3.00 55.00 OMIT 0 6 3 EXTI 0.00136 SHEL 7 0.77 BOND $H FMAP 2 PLAN 5 SIZE 0.08 0.18 0.32 ACTA WGHT 0.02650 2.04700 L.S. 9 TEMP -153.00 FVAR 0.53672 C1 1 -0.073654 0.144401 0.361206 11.00000 0.01812 0.01960 = 0.01825 0.00047 0.00371 0.00071 C2 1 0.039072 0.097250 0.333528 11.00000 0.01923 0.01632 = 0.01463 -0.00049 0.00051 -0.00085 C3 1 0.128909 0.148984 0.295331 11.00000 0.02079 0.02027 = 0.01617 0.00160 0.00303 -0.00235 AFIX 43 H3 2 0.214278 0.135306 0.271868 11.00000 -1.20000 AFIX 0 C4 1 0.071084 0.223686 0.297858 11.00000 0.02826 0.01870 = 0.01694 0.00326 0.00238 -0.00314 AFIX 43 H4 2 0.110066 0.267775 0.275973 11.00000 -1.20000 AFIX 0 C5 1 -0.054849 0.220964 0.338708 11.00000 0.02334 0.01684 = 0.02137 -0.00011 -0.00120 0.00308 AFIX 43 H5 2 -0.115478 0.262684 0.349108 11.00000 -1.20000 AFIX 0 C6 1 0.162735 0.245938 0.530218 11.00000 0.02166 0.01729 = 0.01821 -0.00329 0.00602 0.00046 C7 1 0.302301 0.253634 0.500077 11.00000 0.01838 0.01624 = 0.01785 -0.00209 0.00335 -0.00111 C8 1 0.363004 0.178033 0.502418 11.00000 0.01995 0.01817 = 0.01724 -0.00115 -0.00007 0.00210 AFIX 43 H8 2 0.454696 0.163929 0.485258 11.00000 -1.20000 AFIX 0 C9 1 0.264208 0.127590 0.534480 11.00000 0.02720 0.01730 = 0.02128 0.00269 -0.00102 -0.00049 AFIX 43 H9 2 0.279010 0.074592 0.542301 11.00000 -1.20000 AFIX 0 C10 1 0.140455 0.169832 0.552663 11.00000 0.02390 0.02513 = 0.01866 0.00074 0.00472 -0.00697 AFIX 43 H10 2 0.058096 0.150841 0.575551 11.00000 -1.20000 AFIX 0 C11 1 0.238206 -0.027552 0.317305 11.00000 0.02474 0.01767 = 0.02419 -0.00141 0.00863 0.00131 AFIX 13 H11 2 0.241495 -0.003905 0.259958 11.00000 -1.20000 AFIX 0 C12 1 0.376114 0.000979 0.388079 11.00000 0.02176 0.02697 = 0.03436 -0.00312 0.00310 0.00332 AFIX 137 H12A 2 0.371014 -0.020205 0.444964 11.00000 -1.50000 H12B 2 0.372724 0.056316 0.390784 11.00000 -1.50000 H12C 2 0.473002 -0.014887 0.373857 11.00000 -1.50000 AFIX 0 C13 1 0.251306 -0.113846 0.309740 11.00000 0.03708 0.02026 = 0.03870 -0.00847 0.01055 0.00564 AFIX 137 H13A 2 0.354459 -0.126877 0.301935 11.00000 -1.50000 H13B 2 0.172004 -0.131918 0.259197 11.00000 -1.50000 H13C 2 0.235808 -0.137772 0.363264 11.00000 -1.50000 AFIX 0 C14 1 -0.086167 -0.032231 0.234842 11.00000 0.02521 0.01737 = 0.02414 -0.00196 0.00216 -0.00323 AFIX 13 H14 2 -0.073969 -0.087949 0.227802 11.00000 -1.20000 AFIX 0 C15 1 -0.057079 0.004618 0.152639 11.00000 0.04176 0.04268 = 0.01969 -0.00318 0.00160 -0.01378 AFIX 137 H15A 2 -0.133185 -0.014113 0.101064 11.00000 -1.50000 H15B 2 0.047783 -0.007946 0.147287 11.00000 -1.50000 H15C 2 -0.067115 0.059627 0.156662 11.00000 -1.50000 AFIX 0 C16 1 -0.254424 -0.019514 0.239185 11.00000 0.02515 0.03385 = 0.02898 -0.00237 -0.00233 -0.00250 AFIX 137 H16A 2 -0.272823 0.034723 0.244710 11.00000 -1.50000 H16B 2 -0.274179 -0.046243 0.290073 11.00000 -1.50000 H16C 2 -0.324180 -0.038867 0.185559 11.00000 -1.50000 AFIX 0 C17 1 0.502851 0.369536 0.586335 11.00000 0.02395 0.01739 = 0.02328 -0.00144 0.00666 -0.00313 AFIX 13 H17 2 0.560749 0.416620 0.578829 11.00000 -1.20000 AFIX 0 C18 1 0.624696 0.311156 0.629650 11.00000 0.03036 0.02742 = 0.02061 -0.00026 0.00276 -0.00145 AFIX 137 H18A 2 0.679104 0.329186 0.687890 11.00000 -1.50000 H18B 2 0.699414 0.303990 0.593440 11.00000 -1.50000 H18C 2 0.573535 0.262936 0.635336 11.00000 -1.50000 AFIX 0 C19 1 0.399385 0.389627 0.647335 11.00000 0.02897 0.03386 = 0.02888 -0.01513 0.00992 -0.00888 AFIX 137 H19A 2 0.345018 0.344184 0.659639 11.00000 -1.50000 H19B 2 0.323367 0.427744 0.619378 11.00000 -1.50000 H19C 2 0.463055 0.409908 0.702322 11.00000 -1.50000 AFIX 0 C20 1 0.538157 0.313946 0.420102 11.00000 0.01940 0.02047 = 0.02310 0.00076 0.00823 0.00138 AFIX 13 H20 2 0.604153 0.274588 0.456949 11.00000 -1.20000 AFIX 0 C21 1 0.638876 0.383243 0.413391 11.00000 0.01985 0.02496 = 0.02916 0.00074 0.00744 -0.00189 AFIX 137 H21A 2 0.717339 0.369463 0.381610 11.00000 -1.50000 H21B 2 0.690310 0.400697 0.472400 11.00000 -1.50000 H21C 2 0.573278 0.423808 0.381878 11.00000 -1.50000 AFIX 0 C22 1 0.469849 0.281170 0.328616 11.00000 0.02803 0.02770 = 0.02641 -0.00274 0.01355 -0.00267 AFIX 137 H22A 2 0.402073 0.318810 0.292711 11.00000 -1.50000 H22B 2 0.409631 0.235667 0.333800 11.00000 -1.50000 H22C 2 0.554194 0.268090 0.300873 11.00000 -1.50000 AFIX 0 P1 3 0.048670 -0.005680 0.342214 11.00000 0.02050 0.01328 = 0.01921 0.00111 0.00386 -0.00047 P2 3 0.382914 0.343612 0.474611 11.00000 0.01886 0.01418 = 0.02018 -0.00025 0.00531 -0.00038 FE1 4 0.139985 0.180480 0.423397 11.00000 0.01857 0.01299 = 0.01661 0.00033 0.00311 -0.00067 BR1 5 -0.230487 0.111822 0.415780 11.00000 0.02099 0.02746 = 0.03173 -0.00130 0.00973 -0.00080 BR2 5 0.025272 0.325008 0.541653 11.00000 0.02344 0.03042 = 0.03569 -0.01026 0.00992 0.00199 HKLF 4 Covalent radii and connectivity table for s92 in P2(1)/c C 0.770 H 0.320 P 1.100 FE 1.240 BR 1.140 C1 - C5 C2 Br1 Fe1 C2 - C3 C1 P1 Fe1 C3 - C4 C2 Fe1 C4 - C5 C3 Fe1 C5 - C4 C1 Fe1 C6 - C10 C7 Br2 Fe1 C7 - C6 C8 P2 Fe1 C8 - C9 C7 Fe1 C9 - C10 C8 Fe1 C10 - C9 C6 Fe1 C11 - C12 C13 P1 C12 - C11 C13 - C11 C14 - C15 C16 P1 C15 - C14 C16 - C14 C17 - C19 C18 P2 C18 - C17 C19 - C17 C20 - C22 C21 P2 C21 - C20 C22 - C20 P1 - C2 C11 C14 P2 - C7 C20 C17 Fe1 - C6 C1 C10 C5 C9 C4 C3 C8 C2 C7 Br1 - C1 Br2 - C6 h k l Fo^2 Sigma Why rejected 1 0 3 40.95 5.12 observed but should be systematically absent 0 11 0 21.05 5.26 observed but should be systematically absent 0 5 0 21.05 5.26 observed but should be systematically absent 0 0 5 24.93 4.99 observed but should be systematically absent 0 5 0 22.57 5.64 observed but should be systematically absent 0 5 0 21.00 5.25 observed but should be systematically absent 1 0 3 25.60 5.12 observed but should be systematically absent -8 0 11 188.92 44.47 observed but should be systematically absent 31965 Reflections read, of which 687 rejected -11 =< h =< 11, -22 =< k =< 22, -20 =< l =< 20, Max. 2-theta = 54.97 8 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -2 19 1 122.66 13.63 2 71.08 -9 0 2 27.88 4.94 3 27.51 2 Inconsistent equivalents 5485 Unique reflections, of which 0 suppressed R(int) = 0.0997 R(sigma) = 0.0521 Friedel opposites merged Maximum memory for data reduction = 3161 / 54562 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 = 3939 / 315220 wR2 = 0.0848 before cycle 1 for 5485 data and 253 / 253 parameters GooF = S = 1.075; Restrained GooF = 1.075 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 2.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.53672 0.00078 -0.001 OSF 2 0.00136 0.00026 -0.014 EXTI Mean shift/esd = 0.003 Maximum = 0.023 for U23 Br2 Max. shift = 0.000 A for H22C Max. dU = 0.000 for C14 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3939 / 315220 wR2 = 0.0848 before cycle 2 for 5485 data and 253 / 253 parameters GooF = S = 1.075; Restrained GooF = 1.075 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 2.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.53672 0.00078 -0.001 OSF 2 0.00136 0.00026 -0.004 EXTI Mean shift/esd = 0.001 Maximum = 0.008 for U23 Br2 Max. shift = 0.000 A for H22C Max. dU = 0.000 for C14 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3939 / 315220 wR2 = 0.0847 before cycle 3 for 5485 data and 253 / 253 parameters GooF = S = 1.075; Restrained GooF = 1.075 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 2.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.53672 0.00078 0.001 OSF 2 0.00136 0.00026 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H19C Max. dU = 0.000 for C22 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3939 / 315220 wR2 = 0.0848 before cycle 4 for 5485 data and 253 / 253 parameters GooF = S = 1.075; Restrained GooF = 1.075 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 2.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.53672 0.00078 0.000 OSF 2 0.00136 0.00026 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y Br2 Max. shift = 0.000 A for H15B Max. dU = 0.000 for C14 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3939 / 315220 wR2 = 0.0847 before cycle 5 for 5485 data and 253 / 253 parameters GooF = S = 1.075; Restrained GooF = 1.075 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 2.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.53672 0.00078 0.000 OSF 2 0.00136 0.00026 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y Br2 Max. shift = 0.000 A for C10 Max. dU = 0.000 for C3 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3939 / 315220 wR2 = 0.0847 before cycle 6 for 5485 data and 253 / 253 parameters GooF = S = 1.075; Restrained GooF = 1.075 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 2.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.53672 0.00078 0.000 OSF 2 0.00136 0.00026 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y Br2 Max. shift = 0.000 A for H12C Max. dU = 0.000 for C17 Least-squares cycle 7 Maximum vector length = 511 Memory required = 3939 / 315220 wR2 = 0.0847 before cycle 7 for 5485 data and 253 / 253 parameters GooF = S = 1.075; Restrained GooF = 1.075 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 2.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.53672 0.00078 0.000 OSF 2 0.00136 0.00026 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y Br2 Max. shift = 0.000 A for H22B Max. dU = 0.000 for C4 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3939 / 315220 wR2 = 0.0847 before cycle 8 for 5485 data and 253 / 253 parameters GooF = S = 1.075; Restrained GooF = 1.075 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 2.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.53672 0.00078 0.000 OSF 2 0.00136 0.00026 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y Br2 Max. shift = 0.000 A for H18B Max. dU = 0.000 for C8 Least-squares cycle 9 Maximum vector length = 511 Memory required = 3939 / 315220 wR2 = 0.0847 before cycle 9 for 5485 data and 253 / 253 parameters GooF = S = 1.075; Restrained GooF = 1.075 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 2.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.53672 0.00078 0.000 OSF 2 0.00136 0.00026 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y Br2 Max. shift = 0.000 A for H12A Max. dU = 0.000 for C15 Largest correlation matrix elements 0.601 EXTI / OSF Idealized hydrogen atom generation before cycle 10 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C3 ** H3 0.2143 0.1353 0.2719 43 0.950 0.000 C3 C4 C2 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C4 ** H4 0.1101 0.2678 0.2760 43 0.950 0.000 C4 C5 C3 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C5 ** H5 -0.1155 0.2627 0.3491 43 0.950 0.000 C5 C4 C1 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C8 ** H8 0.4547 0.1639 0.4853 43 0.950 0.000 C8 C9 C7 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C9 ** H9 0.2790 0.0746 0.5423 43 0.950 0.000 C9 C10 C8 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C10 ** H10 0.0581 0.1508 0.5756 43 0.950 0.000 C10 C9 C6 H11 0.2415 -0.0039 0.2600 13 1.000 0.000 C11 C12 C13 P1 H12A 0.3710 -0.0202 0.4450 137 0.980 0.000 C12 C11 H12A H12B 0.3727 0.0563 0.3908 137 0.980 0.000 C12 C11 H12A H12C 0.4730 -0.0149 0.3739 137 0.980 0.000 C12 C11 H12A H13A 0.3545 -0.1269 0.3019 137 0.980 0.000 C13 C11 H13A H13B 0.1720 -0.1319 0.2592 137 0.980 0.000 C13 C11 H13A H13C 0.2358 -0.1378 0.3633 137 0.980 0.000 C13 C11 H13A H14 -0.0740 -0.0879 0.2278 13 1.000 0.000 C14 C15 C16 P1 H15A -0.1332 -0.0141 0.1011 137 0.980 0.000 C15 C14 H15A H15B 0.0478 -0.0079 0.1473 137 0.980 0.000 C15 C14 H15A H15C -0.0671 0.0596 0.1567 137 0.980 0.000 C15 C14 H15A H16A -0.2728 0.0347 0.2447 137 0.980 0.000 C16 C14 H16A H16B -0.2742 -0.0462 0.2901 137 0.980 0.000 C16 C14 H16A H16C -0.3242 -0.0389 0.1856 137 0.980 0.000 C16 C14 H16A H17 0.5607 0.4166 0.5788 13 1.000 0.000 C17 C19 C18 P2 H18A 0.6791 0.3292 0.6879 137 0.980 0.000 C18 C17 H18A H18B 0.6994 0.3040 0.5934 137 0.980 0.000 C18 C17 H18A H18C 0.5735 0.2629 0.6353 137 0.980 0.000 C18 C17 H18A H19A 0.3450 0.3442 0.6596 137 0.980 0.000 C19 C17 H19A H19B 0.3234 0.4277 0.6194 137 0.980 0.000 C19 C17 H19A H19C 0.4631 0.4099 0.7023 137 0.980 0.000 C19 C17 H19A H20 0.6042 0.2746 0.4569 13 1.000 0.000 C20 C22 C21 P2 H21A 0.7173 0.3695 0.3816 137 0.980 0.000 C21 C20 H21A H21B 0.6903 0.4007 0.4724 137 0.980 0.000 C21 C20 H21A H21C 0.5733 0.4238 0.3819 137 0.980 0.000 C21 C20 H21A H22A 0.4021 0.3188 0.2927 137 0.980 0.000 C22 C20 H22A H22B 0.4096 0.2357 0.3338 137 0.980 0.000 C22 C20 H22A H22C 0.5542 0.2681 0.3009 137 0.980 0.000 C22 C20 H22A s92 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.07365 0.14440 0.36121 1.00000 0.01811 0.01960 0.01825 0.00047 0.00371 0.00071 0.01876 0.00510 0.00030 0.00015 0.00018 0.00000 0.00129 0.00135 0.00142 0.00110 0.00108 0.00105 0.00055 C2 0.03907 0.09725 0.33353 1.00000 0.01923 0.01632 0.01462 -0.00049 0.00050 -0.00085 0.01732 0.00491 0.00030 0.00015 0.00017 0.00000 0.00128 0.00128 0.00133 0.00103 0.00104 0.00103 0.00054 C3 0.12891 0.14899 0.29533 1.00000 0.02079 0.02028 0.01617 0.00160 0.00303 -0.00235 0.01931 0.00513 0.00032 0.00015 0.00018 0.00000 0.00131 0.00136 0.00137 0.00109 0.00107 0.00108 0.00055 H3 0.21428 0.13531 0.27187 1.00000 0.02318 0.00000 0.00000 C4 0.07108 0.22369 0.29786 1.00000 0.02825 0.01870 0.01694 0.00326 0.00238 -0.00314 0.02181 0.00533 0.00033 0.00016 0.00018 0.00000 0.00147 0.00136 0.00142 0.00110 0.00114 0.00113 0.00058 H4 0.11007 0.26777 0.27597 1.00000 0.02617 0.00000 0.00000 C5 -0.05485 0.22096 0.33871 1.00000 0.02334 0.01684 0.02137 -0.00011 -0.00120 0.00308 0.02163 0.00524 0.00032 0.00015 0.00019 0.00000 0.00140 0.00133 0.00149 0.00111 0.00115 0.00108 0.00059 H5 -0.11548 0.26268 0.34911 1.00000 0.02595 0.00000 0.00000 C6 0.16274 0.24594 0.53022 1.00000 0.02166 0.01729 0.01821 -0.00330 0.00601 0.00046 0.01884 0.00514 0.00031 0.00015 0.00018 0.00000 0.00133 0.00130 0.00139 0.00107 0.00109 0.00106 0.00055 C7 0.30230 0.25363 0.50008 1.00000 0.01837 0.01625 0.01784 -0.00209 0.00334 -0.00111 0.01766 0.00495 0.00030 0.00015 0.00018 0.00000 0.00128 0.00128 0.00139 0.00105 0.00106 0.00102 0.00054 C8 0.36300 0.17803 0.50242 1.00000 0.01995 0.01817 0.01723 -0.00115 -0.00007 0.00209 0.01922 0.00511 0.00032 0.00015 0.00018 0.00000 0.00134 0.00136 0.00143 0.00106 0.00110 0.00103 0.00057 H8 0.45470 0.16393 0.48526 1.00000 0.02306 0.00000 0.00000 C9 0.26421 0.12759 0.53448 1.00000 0.02720 0.01730 0.02128 0.00270 -0.00103 -0.00049 0.02308 0.00531 0.00033 0.00016 0.00019 0.00000 0.00147 0.00134 0.00151 0.00114 0.00118 0.00112 0.00060 H9 0.27901 0.07459 0.54230 1.00000 0.02770 0.00000 0.00000 C10 0.14046 0.16983 0.55266 1.00000 0.02389 0.02513 0.01865 0.00074 0.00472 -0.00697 0.02262 0.00536 0.00034 0.00016 0.00019 0.00000 0.00144 0.00148 0.00148 0.00117 0.00116 0.00114 0.00060 H10 0.05810 0.15084 0.57555 1.00000 0.02715 0.00000 0.00000 C11 0.23821 -0.02755 0.31731 1.00000 0.02474 0.01767 0.02419 -0.00141 0.00863 0.00131 0.02173 0.00538 0.00032 0.00015 0.00019 0.00000 0.00142 0.00133 0.00152 0.00114 0.00117 0.00110 0.00058 H11 0.24150 -0.00391 0.25996 1.00000 0.02608 0.00000 0.00000 C12 0.37611 0.00098 0.38808 1.00000 0.02176 0.02696 0.03436 -0.00311 0.00310 0.00332 0.02831 0.00571 0.00033 0.00017 0.00021 0.00000 0.00146 0.00156 0.00182 0.00133 0.00130 0.00119 0.00067 H12A 0.37101 -0.02020 0.44496 1.00000 0.04246 0.00000 0.00000 H12B 0.37272 0.05632 0.39078 1.00000 0.04246 0.00000 0.00000 H12C 0.47300 -0.01489 0.37386 1.00000 0.04246 0.00000 0.00000 C13 0.25131 -0.11385 0.30974 1.00000 0.03707 0.02027 0.03870 -0.00846 0.01055 0.00564 0.03176 0.00626 0.00039 0.00016 0.00023 0.00000 0.00174 0.00150 0.00191 0.00134 0.00147 0.00127 0.00072 H13A 0.35446 -0.12688 0.30194 1.00000 0.04764 0.00000 0.00000 H13B 0.17201 -0.13192 0.25919 1.00000 0.04764 0.00000 0.00000 H13C 0.23580 -0.13777 0.36326 1.00000 0.04764 0.00000 0.00000 C14 -0.08617 -0.03223 0.23484 1.00000 0.02520 0.01736 0.02413 -0.00196 0.00216 -0.00322 0.02287 0.00527 0.00032 0.00016 0.00019 0.00000 0.00143 0.00136 0.00152 0.00117 0.00117 0.00112 0.00059 H14 -0.07397 -0.08795 0.22780 1.00000 0.02744 0.00000 0.00000 C15 -0.05708 0.00462 0.15264 1.00000 0.04175 0.04268 0.01969 -0.00318 0.00160 -0.01378 0.03568 0.00608 0.00040 0.00020 0.00021 0.00000 0.00190 0.00197 0.00167 0.00141 0.00140 0.00153 0.00078 H15A -0.13319 -0.01411 0.10106 1.00000 0.05352 0.00000 0.00000 H15B 0.04778 -0.00795 0.14729 1.00000 0.05352 0.00000 0.00000 H15C -0.06711 0.05963 0.15666 1.00000 0.05352 0.00000 0.00000 C16 -0.25442 -0.01951 0.23919 1.00000 0.02515 0.03384 0.02897 -0.00237 -0.00233 -0.00250 0.03082 0.00585 0.00034 0.00019 0.00021 0.00000 0.00154 0.00175 0.00174 0.00138 0.00129 0.00129 0.00070 H16A -0.27282 0.03472 0.24471 1.00000 0.04622 0.00000 0.00000 H16B -0.27418 -0.04624 0.29007 1.00000 0.04622 0.00000 0.00000 H16C -0.32418 -0.03887 0.18556 1.00000 0.04622 0.00000 0.00000 C17 0.50285 0.36954 0.58634 1.00000 0.02395 0.01738 0.02328 -0.00144 0.00665 -0.00313 0.02137 0.00529 0.00032 0.00016 0.00019 0.00000 0.00140 0.00134 0.00151 0.00113 0.00117 0.00109 0.00058 H17 0.56075 0.41662 0.57883 1.00000 0.02564 0.00000 0.00000 C18 0.62470 0.31116 0.62965 1.00000 0.03036 0.02742 0.02060 -0.00026 0.00277 -0.00146 0.02669 0.00581 0.00035 0.00017 0.00020 0.00000 0.00159 0.00157 0.00159 0.00122 0.00127 0.00124 0.00065 H18A 0.67911 0.32919 0.68789 1.00000 0.04004 0.00000 0.00000 H18B 0.69941 0.30399 0.59344 1.00000 0.04004 0.00000 0.00000 H18C 0.57354 0.26294 0.63534 1.00000 0.04004 0.00000 0.00000 C19 0.39938 0.38963 0.64733 1.00000 0.02897 0.03386 0.02887 -0.01512 0.00992 -0.00888 0.03006 0.00569 0.00036 0.00018 0.00021 0.00000 0.00157 0.00176 0.00170 0.00137 0.00133 0.00130 0.00070 H19A 0.34502 0.34418 0.65964 1.00000 0.04509 0.00000 0.00000 H19B 0.32337 0.42774 0.61938 1.00000 0.04509 0.00000 0.00000 H19C 0.46305 0.40991 0.70232 1.00000 0.04509 0.00000 0.00000 C20 0.53816 0.31395 0.42010 1.00000 0.01940 0.02047 0.02310 0.00076 0.00822 0.00138 0.02046 0.00542 0.00032 0.00015 0.00019 0.00000 0.00134 0.00138 0.00154 0.00112 0.00116 0.00106 0.00058 H20 0.60415 0.27459 0.45695 1.00000 0.02455 0.00000 0.00000 C21 0.63888 0.38324 0.41339 1.00000 0.01985 0.02496 0.02916 0.00074 0.00744 -0.00189 0.02439 0.00555 0.00032 0.00016 0.00020 0.00000 0.00137 0.00151 0.00166 0.00123 0.00120 0.00113 0.00062 H21A 0.71734 0.36946 0.38161 1.00000 0.03658 0.00000 0.00000 H21B 0.69031 0.40070 0.47240 1.00000 0.03658 0.00000 0.00000 H21C 0.57328 0.42381 0.38188 1.00000 0.03658 0.00000 0.00000 C22 0.46985 0.28117 0.32862 1.00000 0.02803 0.02770 0.02641 -0.00274 0.01355 -0.00267 0.02619 0.00575 0.00035 0.00017 0.00020 0.00000 0.00152 0.00157 0.00163 0.00125 0.00128 0.00123 0.00064 H22A 0.40207 0.31881 0.29271 1.00000 0.03929 0.00000 0.00000 H22B 0.40964 0.23566 0.33380 1.00000 0.03929 0.00000 0.00000 H22C 0.55419 0.26809 0.30087 1.00000 0.03929 0.00000 0.00000 P1 0.04867 -0.00568 0.34221 1.00000 0.02049 0.01328 0.01921 0.00111 0.00386 -0.00047 0.01781 0.00132 0.00008 0.00004 0.00005 0.00000 0.00035 0.00033 0.00038 0.00027 0.00028 0.00026 0.00016 P2 0.38291 0.34361 0.47461 1.00000 0.01886 0.01418 0.02018 -0.00025 0.00531 -0.00038 0.01763 0.00134 0.00008 0.00004 0.00005 0.00000 0.00034 0.00033 0.00038 0.00027 0.00029 0.00026 0.00016 Fe1 0.13999 0.18048 0.42340 1.00000 0.01857 0.01299 0.01661 0.00033 0.00311 -0.00067 0.01624 0.00072 0.00004 0.00002 0.00003 0.00000 0.00020 0.00019 0.00021 0.00014 0.00016 0.00014 0.00010 Br1 -0.23049 0.11182 0.41578 1.00000 0.02099 0.02746 0.03172 -0.00130 0.00973 -0.00080 0.02615 0.00056 0.00003 0.00002 0.00002 0.00000 0.00015 0.00017 0.00018 0.00012 0.00012 0.00011 0.00010 Br2 0.02527 0.32501 0.54165 1.00000 0.02344 0.03042 0.03569 -0.01026 0.00992 0.00199 0.02937 0.00058 0.00003 0.00002 0.00002 0.00000 0.00016 0.00018 0.00020 0.00013 0.00014 0.00012 0.00010 Final Structure Factor Calculation for s92 in P2(1)/c Total number of l.s. parameters = 253 Maximum vector length = 511 Memory required = 3686 / 24017 wR2 = 0.0847 before cycle 10 for 5485 data and 0 / 253 parameters GooF = S = 1.075; Restrained GooF = 1.075 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 2.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0346 for 4676 Fo > 4sig(Fo) and 0.0448 for all 5485 data wR2 = 0.0847, GooF = S = 1.075, Restrained GooF = 1.075 for all data Occupancy sum of asymmetric unit = 27.00 for non-hydrogen and 34.00 for hydrogen atoms Principal mean square atomic displacements U 0.0199 0.0190 0.0174 C1 0.0223 0.0165 0.0132 C2 0.0241 0.0182 0.0156 C3 0.0316 0.0195 0.0143 C4 0.0316 0.0184 0.0150 C5 0.0219 0.0209 0.0138 C6 0.0196 0.0188 0.0145 C7 0.0257 0.0172 0.0147 C8 0.0341 0.0195 0.0156 C9 0.0320 0.0189 0.0169 C10 0.0267 0.0219 0.0165 C11 0.0383 0.0264 0.0201 C12 0.0427 0.0384 0.0142 C13 0.0298 0.0233 0.0155 C14 0.0571 0.0319 0.0180 C15 0.0389 0.0345 0.0191 C16 0.0257 0.0223 0.0161 C17 0.0328 0.0271 0.0201 C18 0.0485 0.0258 0.0159 C19 0.0246 0.0203 0.0164 C20 0.0293 0.0256 0.0183 C21 0.0346 0.0260 0.0179 C22 0.0214 0.0190 0.0130 P1 0.0203 0.0184 0.0141 P2 0.0195 0.0163 0.0129 Fe1 0.0325 0.0271 0.0189 Br1 0.0438 0.0266 0.0177 Br2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.020 0.036 0.055 0.075 0.098 0.123 0.154 0.199 0.271 1.000 Number in group 577. 541. 540. 540. 546. 555. 540. 552. 544. 550. GooF 1.154 1.091 1.120 1.194 0.963 1.053 0.963 1.070 1.037 1.080 K 1.575 1.116 1.045 1.004 0.998 0.998 1.004 1.008 1.007 1.005 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.65 inf Number in group 560. 553. 548. 545. 545. 545. 545. 550. 543. 551. GooF 0.993 0.968 1.009 1.022 0.951 0.946 0.919 0.986 1.155 1.618 K 0.979 1.020 1.026 1.023 1.023 1.006 1.011 0.995 0.999 1.006 R1 0.099 0.078 0.072 0.060 0.051 0.039 0.030 0.027 0.025 0.028 Recommended weighting scheme: WGHT 0.0264 2.0516 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) 0 6 6 208.86 12.15 5.71 0.013 1.92 -1 1 4 424.83 268.49 4.89 0.060 3.76 0 3 6 161.04 44.53 4.87 0.024 2.33 -3 6 1 238.05 128.97 4.80 0.042 2.09 -2 6 5 92.24 28.25 4.67 0.019 2.04 2 0 4 4026.79 2861.51 4.62 0.196 2.57 0 5 5 83.89 15.86 4.58 0.015 2.31 2 2 2 180.19 93.37 4.46 0.035 3.19 2 2 5 387.34 240.85 4.27 0.057 2.18 -3 6 9 77.10 10.30 4.16 0.012 1.43 -2 4 7 3034.77 2529.48 4.07 0.184 1.94 2 1 7 28417.29 24073.16 4.07 0.568 1.77 3 2 0 1193.90 925.94 3.98 0.111 2.73 2 1 6 5073.52 4168.58 3.91 0.236 1.98 3 6 3 1001.38 783.23 3.89 0.102 1.80 2 2 1 72.20 27.73 3.83 0.019 3.58 0 7 1 292.51 184.10 3.74 0.050 2.49 1 3 1 6385.42 5476.62 3.70 0.271 4.46 -4 2 6 234.35 352.67 3.68 0.069 1.84 0 2 5 3038.64 3665.71 3.58 0.222 2.88 -2 2 4 191.55 119.34 3.41 0.040 3.07 0 9 12 70.76 5.37 3.40 0.008 1.07 1 0 6 423.08 275.70 3.39 0.061 2.29 2 4 8 298.64 198.98 3.39 0.052 1.51 0 7 7 80.93 26.95 3.38 0.019 1.65 0 3 1 2337.32 2750.38 3.35 0.192 5.50 0 7 4 2432.26 2876.59 3.28 0.196 2.11 2 1 8 11732.82 10291.58 3.23 0.372 1.60 -9 6 7 303.60 167.59 3.21 0.047 0.92 0 10 2 394.55 290.27 3.20 0.062 1.72 -6 1 19 221.49 60.86 3.19 0.029 0.78 2 3 4 7655.39 6748.28 3.17 0.301 2.35 -6 1 2 213.30 143.52 3.14 0.044 1.47 -4 1 1 115.20 65.98 3.12 0.030 2.19 -3 16 10 40.98 171.31 3.10 0.048 0.89 0 2 7 1460.71 1229.47 3.10 0.128 2.12 1 3 7 5380.16 4644.63 3.10 0.250 1.90 2 4 2 86.22 45.15 3.08 0.025 2.70 3 1 3 3506.92 3013.21 3.07 0.201 2.26 6 11 4 271.54 416.65 3.04 0.075 0.99 -4 3 3 1708.32 2010.11 3.02 0.164 2.04 -6 16 7 5779.64 4808.63 3.01 0.254 0.86 2 3 5 19038.13 16755.00 3.00 0.474 2.10 3 2 6 2222.82 1867.92 2.96 0.158 1.68 5 4 15 510.73 317.88 2.93 0.065 0.78 3 3 9 548.54 413.61 2.93 0.074 1.29 -4 18 3 581.28 399.66 2.91 0.073 0.90 0 6 11 1097.06 1354.44 2.90 0.135 1.25 -1 7 1 46.97 15.79 2.89 0.015 2.42 -11 1 10 -53.47 123.35 2.89 0.041 0.78 Bond lengths and angles C1 - Distance Angles C5 1.4189 (0.0039) C2 1.4470 (0.0037) 110.10 (0.23) Br1 1.8913 (0.0027) 123.14 (0.20) 126.72 (0.20) Fe1 2.0175 (0.0028) 70.49 (0.15) 71.95 (0.15) 125.83 (0.14) C1 - C5 C2 Br1 C2 - Distance Angles C3 1.4359 (0.0037) C1 1.4470 (0.0037) 104.59 (0.23) P1 1.8253 (0.0027) 130.21 (0.21) 125.11 (0.20) Fe1 2.0869 (0.0026) 69.04 (0.15) 66.81 (0.15) 130.36 (0.14) C2 - C3 C1 P1 C3 - Distance Angles C4 1.4209 (0.0039) C2 1.4359 (0.0037) 109.87 (0.24) Fe1 2.0672 (0.0028) 69.86 (0.16) 70.52 (0.15) H3 0.9500 125.07 125.07 126.15 C3 - C4 C2 Fe1 C4 - Distance Angles C5 1.4169 (0.0040) C3 1.4209 (0.0039) 108.10 (0.24) Fe1 2.0663 (0.0029) 68.92 (0.16) 69.93 (0.15) H4 0.9500 125.95 125.95 126.77 C4 - C5 C3 Fe1 C5 - Distance Angles C4 1.4169 (0.0040) C1 1.4189 (0.0039) 107.33 (0.24) Fe1 2.0424 (0.0028) 70.74 (0.16) 68.61 (0.15) H5 0.9500 126.33 126.33 125.89 C5 - C4 C1 Fe1 C6 - Distance Angles C10 1.4167 (0.0038) C7 1.4348 (0.0037) 110.81 (0.23) Br2 1.8922 (0.0027) 123.12 (0.20) 126.07 (0.20) Fe1 2.0085 (0.0027) 70.65 (0.16) 72.59 (0.15) 124.54 (0.15) C6 - C10 C7 Br2 C7 - Distance Angles C6 1.4348 (0.0037) C8 1.4383 (0.0036) 104.55 (0.22) P2 1.8275 (0.0027) 124.69 (0.20) 130.58 (0.20) Fe1 2.0901 (0.0027) 66.49 (0.15) 69.03 (0.15) 131.64 (0.15) C7 - C6 C8 P2 C8 - Distance Angles C9 1.4247 (0.0039) C7 1.4383 (0.0036) 109.40 (0.24) Fe1 2.0700 (0.0029) 69.14 (0.16) 70.53 (0.15) H8 0.9500 125.30 125.30 126.63 C8 - C9 C7 Fe1 C9 - Distance Angles C10 1.4130 (0.0041) C8 1.4247 (0.0039) 108.35 (0.25) Fe1 2.0528 (0.0028) 69.26 (0.16) 70.43 (0.16) H9 0.9500 125.82 125.82 126.06 C9 - C10 C8 Fe1 C10 - Distance Angles C9 1.4130 (0.0041) C6 1.4167 (0.0038) 106.86 (0.24) Fe1 2.0386 (0.0030) 70.34 (0.17) 68.37 (0.16) H10 0.9500 126.57 126.57 126.27 C10 - C9 C6 Fe1 C11 - Distance Angles C12 1.5288 (0.0041) C13 1.5368 (0.0039) 108.76 (0.24) P1 1.8571 (0.0029) 112.71 (0.20) 108.19 (0.20) H11 1.0000 109.04 109.04 109.04 C11 - C12 C13 P1 C12 - Distance Angles C11 1.5288 (0.0041) H12A 0.9800 109.47 H12B 0.9800 109.47 109.47 H12C 0.9800 109.47 109.47 109.47 C12 - C11 H12A H12B C13 - Distance Angles C11 1.5368 (0.0039) H13A 0.9800 109.47 H13B 0.9800 109.47 109.47 H13C 0.9800 109.47 109.47 109.47 C13 - C11 H13A H13B C14 - Distance Angles C15 1.5227 (0.0042) C16 1.5281 (0.0042) 109.94 (0.26) P1 1.8792 (0.0030) 116.97 (0.20) 110.02 (0.21) H14 1.0000 106.42 106.42 106.42 C14 - C15 C16 P1 C15 - Distance Angles C14 1.5227 (0.0042) H15A 0.9800 109.47 H15B 0.9800 109.47 109.47 H15C 0.9800 109.47 109.47 109.47 C15 - C14 H15A H15B C16 - Distance Angles C14 1.5281 (0.0042) H16A 0.9800 109.47 H16B 0.9800 109.47 109.47 H16C 0.9800 109.47 109.47 109.47 C16 - C14 H16A H16B C17 - Distance Angles C19 1.5198 (0.0039) C18 1.5315 (0.0040) 110.27 (0.25) P2 1.8787 (0.0030) 110.69 (0.20) 115.63 (0.20) H17 1.0000 106.57 106.57 106.57 C17 - C19 C18 P2 C18 - Distance Angles C17 1.5315 (0.0040) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - C17 H18A H18B C19 - Distance Angles C17 1.5198 (0.0040) H19A 0.9800 109.47 H19B 0.9800 109.47 109.47 H19C 0.9800 109.47 109.47 109.47 C19 - C17 H19A H19B C20 - Distance Angles C22 1.5336 (0.0041) C21 1.5351 (0.0038) 110.07 (0.24) P2 1.8636 (0.0028) 111.54 (0.19) 108.30 (0.19) H20 1.0000 108.96 108.96 108.96 C20 - C22 C21 P2 C21 - Distance Angles C20 1.5351 (0.0038) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C21 - C20 H21A H21B C22 - Distance Angles C20 1.5336 (0.0041) H22A 0.9800 109.47 H22B 0.9800 109.47 109.47 H22C 0.9800 109.47 109.47 109.47 C22 - C20 H22A H22B P1 - Distance Angles C2 1.8253 (0.0028) C11 1.8571 (0.0029) 102.72 (0.12) C14 1.8792 (0.0030) 100.00 (0.12) 99.98 (0.13) P1 - C2 C11 P2 - Distance Angles C7 1.8275 (0.0027) C20 1.8636 (0.0028) 103.13 (0.12) C17 1.8787 (0.0030) 99.89 (0.12) 100.49 (0.13) P2 - C7 C20 Fe1 - Distance Angles C6 2.0085 (0.0027) C1 2.0175 (0.0028) 118.79 (0.11) C10 2.0386 (0.0030) 40.97 (0.11) 103.34 (0.11) C5 2.0424 (0.0028) 104.03 (0.11) 40.91 (0.11) 118.73 (0.12) C9 2.0528 (0.0029) 68.04 (0.11) 121.26 (0.11) 40.40 (0.12) 155.79 (0.12) C4 2.0663 (0.0029) 122.15 (0.11) 68.01 (0.11) 156.14 (0.12) 40.34 (0.11) 162.89 (0.12) C3 2.0672 (0.0028) 160.10 (0.11) 67.88 (0.11) 158.91 (0.11) 67.97 (0.11) 126.54 (0.11) 40.21 (0.11) C8 2.0700 (0.0029) 67.70 (0.11) 159.53 (0.11) 68.11 (0.12) 159.56 (0.11) 40.43 (0.11) 127.02 (0.11) 113.19 (0.11) C2 2.0869 (0.0027) 155.85 (0.11) 41.24 (0.10) 120.47 (0.11) 69.33 (0.11) 108.07 (0.11) 68.52 (0.11) 40.44 (0.10) C7 2.0901 (0.0027) 40.92 (0.10) 155.93 (0.11) 69.29 (0.11) 121.20 (0.11) 68.66 (0.11) 109.09 (0.11) 126.38 (0.11) Fe1 - C6 C1 C10 C5 C9 C4 C3 Br1 - Distance Angles C1 1.8913 (0.0027) Br1 - Br2 - Distance Angles C6 1.8922 (0.0027) Br2 - FMAP and GRID set by program FMAP 2 2 23 GRID -1.250 -2 -2 1.250 2 2 R1 = 0.0429 for 5485 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.62 at 0.7733 0.1635 0.4207 [ 0.92 A from BR1 ] Deepest hole -0.58 at 0.9781 0.1528 0.0313 [ 0.57 A from BR2 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 3664 / 25078 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.2267 0.1635 0.4207 1.00000 0.05 0.62 0.92 BR1 1.85 C1 2.42 H5 2.44 C5 Q2 1 -0.2271 0.0555 0.4199 1.00000 0.05 0.57 1.00 BR1 2.40 C1 2.45 H9 2.68 H16B Q3 1 0.1212 0.2755 0.5431 1.00000 0.05 0.52 0.70 C6 1.22 BR2 1.88 C10 1.93 C7 Q4 1 -0.1521 0.1187 0.3781 1.00000 0.05 0.52 0.92 C1 1.02 BR1 2.02 C2 2.16 C5 Q5 1 -0.0485 0.3203 0.5848 1.00000 0.05 0.51 1.05 BR2 2.29 H18B 2.43 H15C 2.60 C6 Shortest distances between peaks (including symmetry equivalents) 1 4 1.31 2 4 1.53 1 2 1.91 3 5 1.95 Time profile in seconds ----------------------- 0.08: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 2.63: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 6.33: Structure factors and derivatives 8.08: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.63: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.14: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.09: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 10:33:54 Total CPU time: 18.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++