+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - MSDOS 32-BIT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-1 + + s92 started at 13:53:40 on 11-Oct-1999 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P-1 CELL 0.71073 9.748 10.889 12.473 80.32 79.02 74.54 ZERR 4.00 0.002 0.002 0.002 0.03 0.03 0.03 LATT 1 SFAC C H N O S CL UNIT 48 44 8 8 4 4 V = 1243.02 F(000) = 584.0 Mu = 0.47 mm-1 Cell Wt = 1130.95 Rho = 1.511 OMIT 0 0 1 ACTA PLAN 5 FMAP 2 L.S. 4 BOND WGHT 0.054900 0.162700 FVAR 0.43717 S1 5 0.01704 0.88049 0.76492 11.00000 0.02451 0.02636 = 0.02649 -0.00033 -0.00631 -0.00620 CL1 6 0.61115 0.87936 0.34152 11.00000 0.02493 0.04070 = 0.04160 -0.00905 -0.00012 -0.00732 O1 4 -0.13125 0.87632 0.78174 11.00000 0.02547 0.03955 = 0.03438 -0.00059 -0.00564 -0.01358 O2 4 0.12110 0.77406 0.80880 11.00000 0.03223 0.02689 = 0.03429 0.00276 -0.00912 -0.00243 N1 3 0.06034 0.90152 0.63149 11.00000 0.02333 0.02947 = 0.02562 -0.00348 -0.00766 -0.00228 N2 3 0.19648 0.94928 0.46645 11.00000 0.02463 0.02715 = 0.03037 -0.00449 -0.00638 -0.00451 C1 1 0.02962 1.35226 0.95457 11.00000 0.04157 0.03917 = 0.03393 -0.01151 0.00424 -0.01600 C2 1 0.03176 1.23701 0.90210 11.00000 0.02660 0.03399 = 0.02540 -0.00578 0.00348 -0.01180 C3 1 -0.07444 1.23847 0.84152 11.00000 0.03137 0.02940 = 0.03940 -0.00429 -0.00513 -0.00117 C4 1 -0.07848 1.13156 0.79852 11.00000 0.02844 0.03316 = 0.03603 -0.00593 -0.01236 -0.00274 C5 1 0.02683 1.01909 0.81496 11.00000 0.02137 0.02717 = 0.02469 -0.00251 -0.00317 -0.00635 C6 1 0.13572 1.01456 0.87384 11.00000 0.02380 0.03479 = 0.03841 -0.00777 -0.01052 -0.00052 C7 1 0.13719 1.12380 0.91597 11.00000 0.02700 0.04331 = 0.04319 -0.01487 -0.00882 -0.00907 C8 1 0.19879 0.89336 0.56984 11.00000 0.02297 0.02159 = 0.02872 -0.00860 -0.00622 -0.00574 C9 1 0.32228 0.94370 0.39901 11.00000 0.03054 0.02980 = 0.02950 -0.00295 -0.00629 -0.00645 C10 1 0.45285 0.88268 0.43339 11.00000 0.02325 0.02449 = 0.03515 -0.00860 -0.00388 -0.00445 C11 1 0.45496 0.82449 0.54003 11.00000 0.02355 0.03063 = 0.03934 -0.00742 -0.01104 -0.00015 C12 1 0.32630 0.82869 0.61044 11.00000 0.02831 0.03267 = 0.02905 -0.00466 -0.00841 -0.00382 H1A 2 -0.01294 0.95033 0.59866 11.00000 0.02876 H1B 2 0.12479 1.36185 0.96022 11.00000 0.05882 H1C 2 -0.02374 1.35057 1.02586 11.00000 0.05264 H1D 2 -0.02681 1.42904 0.91657 11.00000 0.06530 H3 2 -0.14565 1.31417 0.83114 11.00000 0.05704 H4 2 -0.15625 1.13446 0.75819 11.00000 0.04726 H6 2 0.20369 0.93479 0.88635 11.00000 0.03098 H7 2 0.20860 1.12332 0.95810 11.00000 0.04400 H9 2 0.31327 0.98604 0.32276 11.00000 0.03724 H11 2 0.54698 0.78075 0.56431 11.00000 0.02937 H12 2 0.32732 0.79053 0.68265 11.00000 0.03150 S21 5 0.48313 0.38798 0.76739 11.00000 0.02335 0.02570 = 0.02641 -0.00206 -0.00697 -0.00411 CL21 6 -0.10910 0.71473 0.50016 11.00000 0.02420 0.04061 = 0.05050 -0.01013 -0.01324 0.00353 O21 4 0.62631 0.30896 0.74750 11.00000 0.02769 0.02917 = 0.03483 -0.00523 -0.01045 0.00122 O22 4 0.37337 0.33863 0.84029 11.00000 0.03327 0.03382 = 0.03027 0.00223 -0.00584 -0.01346 N21 3 0.43644 0.42960 0.64462 11.00000 0.01827 0.03203 = 0.02533 -0.00317 -0.00402 -0.00336 N22 3 0.30313 0.55312 0.51452 11.00000 0.02359 0.02681 = 0.02585 -0.00393 -0.00536 -0.00529 C21 1 0.52670 0.86830 0.92809 11.00000 0.04167 0.03415 = 0.04709 -0.01173 -0.01534 -0.00533 C22 1 0.51591 0.74857 0.88856 11.00000 0.02912 0.02868 = 0.03126 -0.00485 -0.01428 -0.00027 C23 1 0.61487 0.69651 0.80208 11.00000 0.02664 0.03461 = 0.04377 -0.00835 -0.00533 -0.01055 C24 1 0.60476 0.58717 0.76464 11.00000 0.02479 0.03498 = 0.03233 -0.01049 -0.00013 -0.00620 C25 1 0.49340 0.52893 0.81364 11.00000 0.02181 0.02479 = 0.02456 -0.00164 -0.00973 -0.00246 C26 1 0.39395 0.57960 0.89944 11.00000 0.02234 0.03173 = 0.03034 -0.00161 -0.00463 -0.00427 C27 1 0.40588 0.68847 0.93663 11.00000 0.02852 0.03352 = 0.02879 -0.00646 -0.00511 0.00016 C28 1 0.30061 0.49685 0.61767 11.00000 0.02198 0.02442 = 0.02950 -0.00878 -0.00591 -0.00422 C29 1 0.17801 0.61733 0.48087 11.00000 0.02727 0.02704 = 0.02943 -0.00328 -0.00741 -0.00308 C210 1 0.04744 0.62751 0.54972 11.00000 0.02163 0.02693 = 0.03651 -0.01220 -0.00800 -0.00068 C211 1 0.04570 0.56947 0.65582 11.00000 0.02174 0.05192 = 0.03703 -0.00913 -0.00076 -0.00256 C212 1 0.17323 0.50207 0.69122 11.00000 0.02602 0.05922 = 0.02567 0.00033 -0.00272 -0.00721 H21A 2 0.50642 0.43945 0.59816 11.00000 0.03025 H21B 2 0.47060 0.94751 0.89017 11.00000 0.07050 H21C 2 0.48769 0.87076 1.00381 11.00000 0.07728 H21D 2 0.62077 0.87976 0.91998 11.00000 0.09512 H23 2 0.69044 0.73967 0.76489 11.00000 0.04071 H24 2 0.66980 0.54942 0.70767 11.00000 0.04004 H26 2 0.32006 0.53628 0.93468 11.00000 0.03371 H27 2 0.33473 0.72683 0.99729 11.00000 0.04772 H29 2 0.18568 0.65493 0.40570 11.00000 0.02484 H211 2 -0.04397 0.57777 0.70053 11.00000 0.05507 H212 2 0.17977 0.46045 0.76110 11.00000 0.05563 HKLF 4 Covalent radii and connectivity table for s92 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 CL 0.990 S1 - O2 O1 N1 C5 Cl1 - C10 O1 - S1 O2 - S1 N1 - C8 S1 N2 - C8 C9 C1 - C2 C2 - C7 C3 C1 C3 - C4 C2 C4 - C3 C5 C5 - C4 C6 S1 C6 - C7 C5 C7 - C6 C2 C8 - N2 C12 N1 C9 - N2 C10 C10 - C11 C9 Cl1 C11 - C10 C12 C12 - C11 C8 S21 - O22 O21 N21 C25 Cl21 - C210 O21 - S21 O22 - S21 N21 - C28 S21 N22 - C28 C29 C21 - C22 C22 - C23 C27 C21 C23 - C24 C22 C24 - C23 C25 C25 - C26 C24 S21 C26 - C25 C27 C27 - C26 C22 C28 - N22 C212 N21 C29 - N22 C210 C210 - C211 C29 Cl21 C211 - C210 C212 C212 - C211 C28 11439 Reflections read, of which 1 rejected -11 =< h =< 11, -12 =< k =< 12, -14 =< l =< 14, Max. 2-theta = 50.02 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 0 1 0 0.27 0.09 2 0.58 -9 2 1 10.29 1.06 3 6.08 -1 11 5 127.74 8.52 2 47.64 3 Inconsistent equivalents 4330 Unique reflections, of which 0 suppressed R(int) = 0.0343 R(sigma) = 0.0456 Friedel opposites merged Maximum memory for data reduction = 2740 / 43120 Least-squares cycle 1 Maximum vector length = 511 Memory required = 3714 / 533442 wR2 = 0.0980 before cycle 1 for 4330 data and 413 / 413 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43717 0.00077 0.002 OSF Mean shift/esd = 0.005 Maximum = 0.087 for z S21 Max. shift = 0.000 A for H23 Max. dU = 0.000 for H21D Least-squares cycle 2 Maximum vector length = 511 Memory required = 3714 / 533442 wR2 = 0.0980 before cycle 2 for 4330 data and 413 / 413 parameters GooF = S = 1.048; Restrained GooF = 1.048 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43717 0.00077 0.001 OSF Mean shift/esd = 0.002 Maximum = 0.029 for z S21 Max. shift = 0.000 A for H21C Max. dU = 0.000 for H21A Least-squares cycle 3 Maximum vector length = 511 Memory required = 3714 / 533442 wR2 = 0.0980 before cycle 3 for 4330 data and 413 / 413 parameters GooF = S = 1.048; Restrained GooF = 1.048 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43717 0.00077 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for U13 C24 Max. shift = 0.000 A for H21C Max. dU = 0.000 for H21D Least-squares cycle 4 Maximum vector length = 511 Memory required = 3714 / 533442 wR2 = 0.0980 before cycle 4 for 4330 data and 413 / 413 parameters GooF = S = 1.048; Restrained GooF = 1.048 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43717 0.00077 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z S1 Max. shift = 0.000 A for H21B Max. dU = 0.000 for H3 No correlation matrix elements larger than 0.500 s92 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S1 0.01704 0.88049 0.76492 1.00000 0.02451 0.02636 0.02649 -0.00033 -0.00631 -0.00620 0.02581 0.00073 0.00005 0.00005 0.00004 0.00000 0.00028 0.00031 0.00031 0.00023 0.00021 0.00021 0.00015 Cl1 0.61115 0.87936 0.34152 1.00000 0.02493 0.04070 0.04160 -0.00905 -0.00012 -0.00732 0.03607 0.00081 0.00005 0.00006 0.00005 0.00000 0.00029 0.00036 0.00036 0.00027 0.00023 0.00023 0.00017 O1 -0.13125 0.87632 0.78174 1.00000 0.02547 0.03955 0.03438 -0.00059 -0.00564 -0.01358 0.03235 0.00210 0.00015 0.00015 0.00013 0.00000 0.00076 0.00096 0.00090 0.00072 0.00062 0.00066 0.00037 O2 0.12110 0.77406 0.80880 1.00000 0.03223 0.02689 0.03429 0.00276 -0.00912 -0.00243 0.03230 0.00219 0.00015 0.00014 0.00012 0.00000 0.00080 0.00086 0.00091 0.00069 0.00065 0.00063 0.00036 N1 0.06034 0.90152 0.63149 1.00000 0.02333 0.02947 0.02562 -0.00348 -0.00766 -0.00227 0.02640 0.00249 0.00018 0.00017 0.00014 0.00000 0.00092 0.00105 0.00103 0.00080 0.00075 0.00075 0.00041 N2 0.19648 0.94928 0.46645 1.00000 0.02463 0.02715 0.03037 -0.00449 -0.00638 -0.00451 0.02732 0.00244 0.00017 0.00017 0.00015 0.00000 0.00091 0.00103 0.00108 0.00081 0.00073 0.00073 0.00041 C1 0.02962 1.35226 0.95457 1.00000 0.04157 0.03917 0.03393 -0.01151 0.00424 -0.01600 0.03754 0.00366 0.00029 0.00026 0.00022 0.00000 0.00145 0.00159 0.00149 0.00119 0.00113 0.00119 0.00058 C2 0.03176 1.23701 0.90210 1.00000 0.02660 0.03399 0.02540 -0.00578 0.00348 -0.01180 0.02856 0.00305 0.00021 0.00021 0.00017 0.00000 0.00110 0.00132 0.00118 0.00098 0.00085 0.00093 0.00049 C3 -0.07444 1.23847 0.84152 1.00000 0.03137 0.02940 0.03940 -0.00429 -0.00513 -0.00117 0.03463 0.00353 0.00025 0.00024 0.00020 0.00000 0.00122 0.00136 0.00142 0.00109 0.00099 0.00098 0.00054 C4 -0.07848 1.13156 0.79852 1.00000 0.02844 0.03316 0.03603 -0.00593 -0.01236 -0.00274 0.03225 0.00330 0.00023 0.00022 0.00020 0.00000 0.00116 0.00136 0.00133 0.00104 0.00096 0.00094 0.00052 C5 0.02683 1.01909 0.81496 1.00000 0.02137 0.02717 0.02469 -0.00251 -0.00317 -0.00635 0.02445 0.00286 0.00020 0.00020 0.00017 0.00000 0.00100 0.00120 0.00114 0.00091 0.00081 0.00084 0.00046 C6 0.13572 1.01456 0.87384 1.00000 0.02380 0.03479 0.03841 -0.00777 -0.01052 -0.00052 0.03244 0.00321 0.00023 0.00023 0.00019 0.00000 0.00111 0.00141 0.00138 0.00108 0.00094 0.00096 0.00052 C7 0.13719 1.12380 0.91597 1.00000 0.02700 0.04331 0.04319 -0.01487 -0.00882 -0.00907 0.03611 0.00332 0.00024 0.00024 0.00021 0.00000 0.00119 0.00152 0.00147 0.00115 0.00101 0.00102 0.00056 C8 0.19879 0.89336 0.56984 1.00000 0.02297 0.02159 0.02872 -0.00860 -0.00622 -0.00574 0.02339 0.00272 0.00020 0.00019 0.00017 0.00000 0.00103 0.00113 0.00121 0.00090 0.00082 0.00082 0.00045 C9 0.32228 0.94370 0.39901 1.00000 0.03054 0.02980 0.02950 -0.00295 -0.00629 -0.00645 0.02997 0.00315 0.00022 0.00022 0.00019 0.00000 0.00119 0.00130 0.00130 0.00101 0.00093 0.00093 0.00050 C10 0.45285 0.88268 0.43339 1.00000 0.02325 0.02449 0.03515 -0.00860 -0.00388 -0.00445 0.02738 0.00293 0.00021 0.00020 0.00018 0.00000 0.00108 0.00119 0.00134 0.00097 0.00088 0.00084 0.00049 C11 0.45496 0.82449 0.54003 1.00000 0.02355 0.03063 0.03934 -0.00742 -0.01104 -0.00015 0.03120 0.00317 0.00023 0.00022 0.00019 0.00000 0.00110 0.00128 0.00140 0.00103 0.00094 0.00089 0.00051 C12 0.32630 0.82869 0.61044 1.00000 0.02831 0.03267 0.02905 -0.00466 -0.00841 -0.00382 0.03006 0.00314 0.00023 0.00022 0.00020 0.00000 0.00114 0.00133 0.00132 0.00104 0.00091 0.00092 0.00050 H1A -0.01294 0.95033 0.59866 1.00000 0.02876 0.03191 0.00246 0.00220 0.00185 0.00000 0.00594 H1B 0.12479 1.36185 0.96022 1.00000 0.05882 0.04154 0.00318 0.00264 0.00230 0.00000 0.00820 H1C -0.02374 1.35057 1.02586 1.00000 0.05264 0.03731 0.00281 0.00254 0.00244 0.00000 0.00793 H1D -0.02681 1.42904 0.91657 1.00000 0.06530 0.04139 0.00312 0.00300 0.00252 0.00000 0.00921 H3 -0.14565 1.31417 0.83114 1.00000 0.05704 0.03871 0.00288 0.00281 0.00231 0.00000 0.00811 H4 -0.15625 1.13446 0.75819 1.00000 0.04726 0.03698 0.00268 0.00243 0.00212 0.00000 0.00712 H6 0.20369 0.93479 0.88635 1.00000 0.03098 0.03140 0.00239 0.00229 0.00184 0.00000 0.00593 H7 0.20860 1.12332 0.95810 1.00000 0.04400 0.03628 0.00259 0.00233 0.00207 0.00000 0.00699 H9 0.31327 0.98604 0.32276 1.00000 0.03724 0.03335 0.00238 0.00231 0.00210 0.00000 0.00636 H11 0.54698 0.78075 0.56431 1.00000 0.02937 0.03113 0.00236 0.00212 0.00180 0.00000 0.00583 H12 0.32732 0.79053 0.68265 1.00000 0.03150 0.03225 0.00229 0.00222 0.00204 0.00000 0.00617 S21 0.48313 0.38798 0.76739 1.00000 0.02335 0.02570 0.02641 -0.00206 -0.00697 -0.00411 0.02522 0.00073 0.00005 0.00005 0.00004 0.00000 0.00027 0.00030 0.00031 0.00023 0.00020 0.00021 0.00015 Cl21 -0.10910 0.71473 0.50016 1.00000 0.02420 0.04061 0.05050 -0.01013 -0.01324 0.00353 0.03909 0.00083 0.00005 0.00006 0.00005 0.00000 0.00029 0.00036 0.00039 0.00028 0.00024 0.00023 0.00018 O21 0.62631 0.30896 0.74750 1.00000 0.02769 0.02917 0.03483 -0.00523 -0.01045 0.00122 0.03122 0.00208 0.00015 0.00014 0.00012 0.00000 0.00078 0.00088 0.00091 0.00069 0.00064 0.00062 0.00036 O22 0.37337 0.33863 0.84029 1.00000 0.03327 0.03382 0.03027 0.00223 -0.00584 -0.01346 0.03203 0.00210 0.00015 0.00015 0.00012 0.00000 0.00082 0.00090 0.00087 0.00069 0.00064 0.00067 0.00036 N21 0.43644 0.42960 0.64462 1.00000 0.01827 0.03203 0.02533 -0.00317 -0.00402 -0.00336 0.02570 0.00249 0.00018 0.00017 0.00015 0.00000 0.00088 0.00107 0.00102 0.00081 0.00075 0.00073 0.00040 N22 0.30313 0.55312 0.51452 1.00000 0.02359 0.02681 0.02585 -0.00393 -0.00536 -0.00529 0.02528 0.00236 0.00017 0.00017 0.00014 0.00000 0.00090 0.00101 0.00103 0.00079 0.00070 0.00072 0.00040 C21 0.52670 0.86830 0.92809 1.00000 0.04167 0.03415 0.04709 -0.01173 -0.01534 -0.00533 0.03975 0.00361 0.00030 0.00025 0.00025 0.00000 0.00150 0.00152 0.00173 0.00124 0.00125 0.00114 0.00060 C22 0.51591 0.74857 0.88856 1.00000 0.02912 0.02868 0.03126 -0.00485 -0.01428 -0.00027 0.02955 0.00301 0.00022 0.00021 0.00018 0.00000 0.00113 0.00125 0.00126 0.00098 0.00093 0.00090 0.00050 C23 0.61487 0.69651 0.80208 1.00000 0.02664 0.03461 0.04377 -0.00835 -0.00533 -0.01055 0.03399 0.00321 0.00023 0.00023 0.00020 0.00000 0.00114 0.00137 0.00146 0.00111 0.00099 0.00098 0.00054 C24 0.60476 0.58717 0.76464 1.00000 0.02479 0.03498 0.03233 -0.01049 -0.00013 -0.00620 0.03073 0.00323 0.00023 0.00022 0.00019 0.00000 0.00110 0.00137 0.00132 0.00108 0.00094 0.00093 0.00051 C25 0.49340 0.52893 0.81364 1.00000 0.02181 0.02479 0.02456 -0.00164 -0.00973 -0.00246 0.02367 0.00283 0.00020 0.00020 0.00017 0.00000 0.00100 0.00114 0.00112 0.00088 0.00081 0.00080 0.00045 C26 0.39395 0.57960 0.89944 1.00000 0.02234 0.03173 0.03034 -0.00161 -0.00463 -0.00427 0.02877 0.00314 0.00022 0.00021 0.00018 0.00000 0.00105 0.00130 0.00126 0.00101 0.00088 0.00091 0.00050 C27 0.40588 0.68847 0.93663 1.00000 0.02852 0.03352 0.02879 -0.00646 -0.00511 0.00016 0.03136 0.00330 0.00023 0.00023 0.00019 0.00000 0.00114 0.00135 0.00128 0.00103 0.00094 0.00093 0.00051 C28 0.30061 0.49685 0.61767 1.00000 0.02198 0.02442 0.02950 -0.00878 -0.00591 -0.00422 0.02465 0.00277 0.00020 0.00020 0.00017 0.00000 0.00102 0.00117 0.00125 0.00094 0.00083 0.00082 0.00046 C29 0.17801 0.61733 0.48087 1.00000 0.02727 0.02704 0.02943 -0.00328 -0.00741 -0.00308 0.02820 0.00305 0.00022 0.00021 0.00019 0.00000 0.00115 0.00125 0.00132 0.00101 0.00090 0.00090 0.00049 C210 0.04744 0.62751 0.54972 1.00000 0.02163 0.02693 0.03651 -0.01220 -0.00800 -0.00068 0.02789 0.00289 0.00021 0.00020 0.00018 0.00000 0.00106 0.00121 0.00138 0.00100 0.00089 0.00085 0.00049 C211 0.04570 0.56947 0.65582 1.00000 0.02174 0.05192 0.03703 -0.00913 -0.00076 -0.00256 0.03822 0.00358 0.00024 0.00025 0.00021 0.00000 0.00120 0.00163 0.00148 0.00120 0.00098 0.00104 0.00059 C212 0.17323 0.50207 0.69122 1.00000 0.02602 0.05922 0.02567 0.00033 -0.00272 -0.00721 0.03842 0.00370 0.00024 0.00027 0.00020 0.00000 0.00116 0.00173 0.00133 0.00119 0.00092 0.00106 0.00059 H21A 0.50642 0.43945 0.59816 1.00000 0.03025 0.03294 0.00257 0.00221 0.00196 0.00000 0.00639 H21B 0.47060 0.94751 0.89017 1.00000 0.07050 0.04294 0.00328 0.00311 0.00262 0.00000 0.00937 H21C 0.48769 0.87076 1.00381 1.00000 0.07728 0.04619 0.00334 0.00304 0.00294 0.00000 0.01065 H21D 0.62077 0.87976 0.91998 1.00000 0.09512 0.05337 0.00414 0.00341 0.00305 0.00000 0.01197 H23 0.69044 0.73967 0.76489 1.00000 0.04071 0.03387 0.00253 0.00229 0.00200 0.00000 0.00661 H24 0.66980 0.54942 0.70767 1.00000 0.04004 0.03416 0.00257 0.00239 0.00212 0.00000 0.00671 H26 0.32006 0.53628 0.93468 1.00000 0.03371 0.03197 0.00241 0.00220 0.00188 0.00000 0.00607 H27 0.33473 0.72683 0.99729 1.00000 0.04772 0.03537 0.00272 0.00246 0.00215 0.00000 0.00724 H29 0.18568 0.65493 0.40570 1.00000 0.02484 0.03007 0.00212 0.00207 0.00194 0.00000 0.00558 H211 -0.04397 0.57777 0.70053 1.00000 0.05507 0.03866 0.00294 0.00261 0.00232 0.00000 0.00791 H212 0.17977 0.46045 0.76110 1.00000 0.05563 0.03948 0.00280 0.00267 0.00246 0.00000 0.00820 Final Structure Factor Calculation for s92 in P-1 Total number of l.s. parameters = 413 Maximum vector length = 511 Memory required = 3301 / 25039 wR2 = 0.0980 before cycle 5 for 4330 data and 0 / 413 parameters GooF = S = 1.048; Restrained GooF = 1.048 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0368 for 3530 Fo > 4sig(Fo) and 0.0488 for all 4330 data wR2 = 0.0980, GooF = S = 1.048, Restrained GooF = 1.048 for all data Occupancy sum of asymmetric unit = 36.00 for non-hydrogen and 22.00 for hydrogen atoms Principal mean square atomic displacements U 0.0299 0.0253 0.0223 S1 0.0452 0.0389 0.0242 Cl1 0.0427 0.0330 0.0214 O1 0.0395 0.0361 0.0214 O2 0.0330 0.0267 0.0195 N1 0.0314 0.0272 0.0234 N2 0.0529 0.0321 0.0277 C1 0.0375 0.0291 0.0191 C2 0.0406 0.0380 0.0253 C3 0.0420 0.0323 0.0225 C4 0.0275 0.0247 0.0211 C5 0.0438 0.0332 0.0204 C6 0.0521 0.0340 0.0223 C7 0.0316 0.0229 0.0157 C8 0.0317 0.0304 0.0278 C9 0.0365 0.0239 0.0217 C10 0.0431 0.0309 0.0196 C11 0.0363 0.0299 0.0239 C12 0.0280 0.0271 0.0206 S21 0.0562 0.0419 0.0192 Cl21 0.0411 0.0317 0.0209 O21 0.0405 0.0308 0.0248 O22 0.0338 0.0253 0.0180 N21 0.0278 0.0256 0.0224 N22 0.0554 0.0350 0.0289 C21 0.0419 0.0282 0.0185 C22 0.0447 0.0337 0.0236 C23 0.0395 0.0298 0.0229 C24 0.0293 0.0262 0.0156 C25 0.0350 0.0293 0.0220 C26 0.0416 0.0282 0.0243 C27 0.0330 0.0216 0.0194 C28 0.0325 0.0287 0.0234 C29 0.0421 0.0221 0.0194 C210 0.0554 0.0383 0.0209 C211 0.0636 0.0272 0.0245 C212 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.025 0.038 0.053 0.071 0.090 0.113 0.147 0.207 1.000 Number in group 453. 428. 429. 435. 434. 418. 435. 431. 432. 435. GooF 0.888 1.063 1.020 1.135 1.137 1.113 0.956 1.017 0.993 1.139 K 1.195 1.024 0.980 0.973 0.962 0.979 0.996 1.012 1.029 1.004 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.07 1.15 1.26 1.45 1.81 inf Number in group 434. 443. 429. 432. 438. 424. 431. 430. 433. 436. GooF 1.074 0.935 0.905 0.962 0.966 0.969 0.929 0.873 1.258 1.461 K 0.972 1.001 1.015 1.032 1.030 1.030 1.042 1.027 1.027 0.969 R1 0.123 0.087 0.065 0.060 0.052 0.042 0.033 0.030 0.034 0.036 Recommended weighting scheme: WGHT 0.0549 0.1627 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) 1 0 1 659.38 1420.17 8.55 0.246 7.99 4 -2 1 27.56 12.93 4.98 0.023 1.95 0 -10 7 238.28 442.83 4.91 0.137 0.85 4 0 4 19.96 6.09 4.61 0.016 2.00 1 1 7 55.58 34.47 4.47 0.038 1.78 -2 -10 7 492.68 786.50 4.01 0.183 0.85 -4 -4 3 137.72 182.82 3.96 0.088 1.64 -2 -4 2 267.46 341.12 3.65 0.120 2.20 0 1 0 1.44 12.85 3.46 0.023 10.41 -4 4 0 182.32 136.43 3.38 0.076 1.56 3 3 0 219.92 273.59 3.34 0.108 2.65 3 7 0 49.51 71.08 3.32 0.055 1.49 -9 -4 6 90.56 126.29 3.27 0.073 0.86 -3 -4 1 27.83 39.83 3.26 0.041 2.16 4 -4 1 213.69 167.84 3.24 0.085 1.55 0 -5 5 198.06 148.27 3.21 0.079 1.49 -1 -4 5 36.33 56.37 3.19 0.049 1.66 3 -1 3 251.61 310.90 3.17 0.115 2.42 3 1 5 371.18 302.49 3.15 0.113 2.14 -5 -4 3 69.41 89.93 3.14 0.062 1.47 11 0 0 -9.78 60.42 3.12 0.051 0.84 11 0 1 32.65 105.93 3.12 0.067 0.85 5 11 6 118.30 159.65 3.11 0.082 0.93 -1 -3 1 6.28 14.25 3.09 0.025 3.25 -1 -2 4 256.46 202.09 3.07 0.093 2.40 -7 -2 4 128.25 162.55 3.06 0.083 1.17 11 4 7 34.17 74.72 3.06 0.056 0.85 1 -1 4 45.41 61.04 3.02 0.051 2.76 6 8 8 45.35 65.29 2.98 0.053 1.03 1 -1 12 40.15 67.35 2.94 0.054 1.00 6 4 0 38.07 25.94 2.92 0.033 1.50 -4 2 2 -0.38 5.85 2.91 0.016 1.81 -9 -7 3 42.70 68.60 2.91 0.054 0.89 0 -5 3 551.57 450.59 2.89 0.138 1.77 4 8 3 0.96 10.67 2.86 0.021 1.29 1 5 0 50.81 36.92 2.83 0.040 2.15 2 11 2 29.98 2.90 2.83 0.011 0.99 -10 0 3 109.59 152.06 2.83 0.080 0.88 4 2 5 64.18 49.27 2.82 0.046 1.90 4 -3 3 335.33 402.70 2.81 0.131 1.63 -7 -4 2 101.60 127.28 2.81 0.074 1.23 5 3 3 151.09 183.91 2.80 0.088 1.82 1 -5 3 281.47 342.84 2.76 0.121 1.69 -3 -1 3 78.17 62.26 2.76 0.051 2.29 -9 -8 1 17.42 31.86 2.76 0.037 0.91 6 2 2 286.60 235.29 2.75 0.100 1.62 -1 3 1 741.60 880.44 2.74 0.194 2.97 4 -3 2 27.25 37.62 2.73 0.040 1.70 -4 3 4 250.05 303.28 2.72 0.114 1.48 1 8 11 7.88 27.94 2.71 0.034 0.92 Bond lengths and angles S1 - Distance Angles O2 1.4293 (0.0016) O1 1.4324 (0.0015) 119.87 (0.09) N1 1.6298 (0.0019) 108.75 (0.10) 104.06 (0.10) C5 1.7586 (0.0021) 108.18 (0.10) 107.99 (0.10) 107.37 (0.10) S1 - O2 O1 N1 Cl1 - Distance Angles C10 1.7338 (0.0021) Cl1 - O1 - Distance Angles S1 1.4324 (0.0015) O1 - O2 - Distance Angles S1 1.4293 (0.0016) O2 - N1 - Distance Angles C8 1.4087 (0.0026) S1 1.6298 (0.0019) 127.80 (0.15) N1 - C8 N2 - Distance Angles C8 1.3319 (0.0028) C9 1.3415 (0.0027) 118.37 (0.18) N2 - C8 C1 - Distance Angles C2 1.5035 (0.0033) C1 - C2 - Distance Angles C7 1.3879 (0.0033) C3 1.3886 (0.0032) 117.65 (0.21) C1 1.5035 (0.0033) 121.05 (0.21) 121.25 (0.22) C2 - C7 C3 C3 - Distance Angles C4 1.3736 (0.0034) C2 1.3886 (0.0032) 121.85 (0.22) C3 - C4 C4 - Distance Angles C3 1.3736 (0.0034) C5 1.3861 (0.0030) 119.36 (0.21) C4 - C3 C5 - Distance Angles C4 1.3861 (0.0030) C6 1.3876 (0.0029) 120.38 (0.21) S1 1.7586 (0.0021) 119.26 (0.16) 120.32 (0.17) C5 - C4 C6 C6 - Distance Angles C7 1.3832 (0.0033) C5 1.3876 (0.0029) 118.97 (0.22) C6 - C7 C7 - Distance Angles C6 1.3832 (0.0033) C2 1.3879 (0.0033) 121.77 (0.21) C7 - C6 C8 - Distance Angles N2 1.3319 (0.0028) C12 1.3966 (0.0030) 122.77 (0.19) N1 1.4087 (0.0026) 113.20 (0.17) 123.98 (0.20) C8 - N2 C12 C9 - Distance Angles N2 1.3415 (0.0027) C10 1.3807 (0.0030) 122.26 (0.21) C9 - N2 C10 - Distance Angles C11 1.3751 (0.0032) C9 1.3807 (0.0030) 119.28 (0.20) Cl1 1.7338 (0.0021) 121.05 (0.16) 119.66 (0.17) C10 - C11 C9 C11 - Distance Angles C10 1.3751 (0.0032) C12 1.3820 (0.0031) 119.22 (0.20) C11 - C10 C12 - Distance Angles C11 1.3820 (0.0031) C8 1.3966 (0.0030) 118.09 (0.22) C12 - C11 S21 - Distance Angles O22 1.4254 (0.0016) O21 1.4316 (0.0016) 120.24 (0.10) N21 1.6370 (0.0019) 109.33 (0.09) 103.70 (0.10) C25 1.7608 (0.0021) 108.04 (0.10) 107.90 (0.09) 106.90 (0.10) S21 - O22 O21 N21 Cl21 - Distance Angles C210 1.7326 (0.0021) Cl21 - O21 - Distance Angles S21 1.4316 (0.0016) O21 - O22 - Distance Angles S21 1.4254 (0.0016) O22 - N21 - Distance Angles C28 1.4044 (0.0026) S21 1.6370 (0.0019) 127.57 (0.16) N21 - C28 N22 - Distance Angles C28 1.3275 (0.0027) C29 1.3396 (0.0026) 118.42 (0.18) N22 - C28 C21 - Distance Angles C22 1.5043 (0.0033) C21 - C22 - Distance Angles C23 1.3904 (0.0033) C27 1.3913 (0.0031) 118.55 (0.21) C21 1.5043 (0.0033) 120.60 (0.21) 120.84 (0.22) C22 - C23 C27 C23 - Distance Angles C24 1.3829 (0.0032) C22 1.3904 (0.0033) 120.89 (0.21) C23 - C24 C24 - Distance Angles C23 1.3829 (0.0032) C25 1.3922 (0.0029) 119.58 (0.21) C24 - C23 C25 - Distance Angles C26 1.3812 (0.0030) C24 1.3922 (0.0029) 120.27 (0.21) S21 1.7608 (0.0021) 120.35 (0.16) 119.36 (0.17) C25 - C26 C24 C26 - Distance Angles C25 1.3812 (0.0030) C27 1.3830 (0.0032) 119.58 (0.21) C26 - C25 C27 - Distance Angles C26 1.3830 (0.0032) C22 1.3913 (0.0031) 121.13 (0.21) C27 - C26 C28 - Distance Angles N22 1.3275 (0.0027) C212 1.3901 (0.0030) 122.36 (0.19) N21 1.4044 (0.0026) 114.29 (0.18) 123.33 (0.20) C28 - N22 C212 C29 - Distance Angles N22 1.3396 (0.0026) C210 1.3821 (0.0030) 122.38 (0.21) C29 - N22 C210 - Distance Angles C211 1.3664 (0.0033) C29 1.3821 (0.0030) 118.87 (0.20) Cl21 1.7326 (0.0021) 121.73 (0.17) 119.39 (0.17) C210 - C211 C29 C211 - Distance Angles C210 1.3664 (0.0033) C212 1.3759 (0.0034) 119.39 (0.22) C211 - C210 C212 - Distance Angles C211 1.3759 (0.0034) C28 1.3901 (0.0030) 118.57 (0.23) C212 - C211 FMAP and GRID set by program FMAP 2 1 24 GRID -2.381 -2 -2 2.381 2 2 R1 = 0.0485 for 4330 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.22 at 0.1129 0.2850 0.4970 [ 0.05 A from CL21 ] Deepest hole -0.39 at 0.0237 0.0615 0.2653 [ 0.74 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 3134 / 22713 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0918 1.2797 0.7126 1.00000 0.05 0.21 1.55 H3 1.62 C3 1.77 C4 1.82 H4 Q2 1 0.6402 0.7675 0.5004 1.00000 0.05 0.21 1.08 H11 1.75 C11 2.15 C10 2.17 CL1 Q3 1 0.1732 0.9898 0.4770 1.00000 0.05 0.21 0.47 N2 1.44 C8 1.60 C9 1.89 H1A Q4 1 0.0332 0.6951 0.4411 1.00000 0.05 0.21 1.42 CL21 1.44 H29 1.44 C210 1.56 C29 Q5 1 0.5442 0.4727 0.5567 1.00000 0.05 0.20 0.68 H21A 1.48 N21 1.56 N22 2.09 H21A Shortest distances between peaks (including symmetry equivalents) 5 5 1.73 1 4 1.89 Time profile in seconds ----------------------- 0.11: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.06: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.88: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.06: Set up l.s. refinement 0.00: Generate idealized H-atoms 7.96: Structure factors and derivatives 44.40: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 5.04: Solve l.s. equations 0.00: Generate HTAB table 0.11: Other dependent quantities, CIF, tables 0.61: Analysis of variance 0.33: Merge reflections for Fourier and .fcf 0.19: Fourier summations 0.25: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 13:54:40 Total elapsed time: 60.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++