+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - MSDOS 32-BIT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-1 + + s92 started at 09:28:59 on 17-Sep-1999 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P2(1)/n CELL 0.71073 12.476 14.045 15.134 90.00 109.33 90.00 ZERR 8.00 0.002 0.003 0.003 0.00 0.03 0.00 LATT 1 SYMM .5-X, .5+Y, .5-Z SFAC C H N O S CL UNIT 88 80 24 16 8 8 V = 2502.37 F(000) = 1168.0 Mu = 0.47 mm-1 Cell Wt = 2269.84 Rho = 1.506 FMAP 2 OMIT 4 1 3 OMIT -1 3 8 OMIT 0 2 7 OMIT 0 3 7 PLAN 10 ACTA L.S. 4 BOND WGHT 0.082600 2.902300 FVAR 0.23139 S1 5 0.75462 0.68325 0.02775 11.00000 0.04429 0.03703 = 0.03113 -0.00304 0.01409 0.00358 CL1 6 0.84205 0.21817 -0.08631 11.00000 0.08465 0.03335 = 0.09258 0.00101 0.04046 -0.00126 O1 4 0.79104 0.78059 0.03041 11.00000 0.05732 0.03643 = 0.04393 -0.01152 0.01810 -0.00317 O2 4 0.74404 0.64121 0.11077 11.00000 0.05648 0.05776 = 0.02637 0.00275 0.01702 0.00879 N1 3 0.32734 0.62638 -0.28318 11.00000 0.03966 0.06526 = 0.04731 0.01377 0.00923 -0.00897 N2 3 0.84984 0.62380 -0.00242 11.00000 0.03821 0.03140 = 0.03900 0.00311 0.01696 0.00191 N3 3 0.86402 0.49788 -0.09619 11.00000 0.03970 0.02870 = 0.03851 0.00306 0.01574 -0.00039 C1 1 0.42420 0.64392 -0.20907 11.00000 0.03933 0.03435 = 0.04466 0.00620 0.01828 0.00533 C2 1 0.43988 0.60217 -0.12177 11.00000 0.03991 0.04083 = 0.04630 0.01022 0.02085 -0.00167 C3 1 0.53985 0.61502 -0.04917 11.00000 0.04622 0.03971 = 0.03649 0.00967 0.01935 0.00546 C4 1 0.62605 0.66998 -0.06162 11.00000 0.03783 0.03231 = 0.02883 0.00220 0.01386 0.00688 C5 1 0.60979 0.71370 -0.14866 11.00000 0.03926 0.03876 = 0.03770 0.00505 0.01980 -0.00334 C6 1 0.51101 0.70016 -0.21995 11.00000 0.04418 0.03930 = 0.03660 0.00846 0.02083 0.00118 C7 1 0.84227 0.52453 -0.01988 11.00000 0.02725 0.03140 = 0.03658 0.00210 0.00935 0.00349 C8 1 0.81981 0.46086 0.04168 11.00000 0.04358 0.04383 = 0.03874 0.01032 0.01854 0.00788 C9 1 0.81861 0.36541 0.02254 11.00000 0.04769 0.03794 = 0.04922 0.01281 0.02212 0.00084 C10 1 0.84157 0.33727 -0.05715 11.00000 0.04319 0.02806 = 0.05968 0.00028 0.01994 -0.00249 C11 1 0.86524 0.40414 -0.11367 11.00000 0.04883 0.03333 = 0.04545 0.00053 0.02051 -0.00140 H1A 2 0.26215 0.61298 -0.27619 11.00000 0.06755 H1B 2 0.32163 0.65721 -0.33465 11.00000 0.05089 H2A 2 0.87048 0.65257 -0.03676 11.00000 0.04550 H3 2 0.54970 0.58781 0.01603 11.00000 0.06187 H4 2 0.38034 0.56408 -0.10815 11.00000 0.06130 H5 2 0.67174 0.75554 -0.15783 11.00000 0.05172 H6 2 0.50237 0.72732 -0.27381 11.00000 0.03945 H8 2 0.80826 0.48541 0.09730 11.00000 0.04024 H9 2 0.80040 0.31597 0.05617 11.00000 0.05354 H11 2 0.87818 0.38586 -0.17602 11.00000 0.05912 S21 5 0.99616 -0.44630 -0.28844 11.00000 0.04288 0.03854 = 0.03976 0.00508 0.02046 0.00427 CL21 6 0.92514 0.01894 -0.15627 11.00000 0.13123 0.03210 = 0.20409 -0.00383 0.12056 -0.00550 O21 4 0.98701 -0.54323 -0.26280 11.00000 0.06600 0.03819 = 0.04756 0.00896 0.03064 0.01240 O22 4 1.10645 -0.40442 -0.26676 11.00000 0.03938 0.07144 = 0.05506 0.00531 0.01860 -0.00094 N21 3 0.75309 -0.39205 -0.69023 11.00000 0.09090 0.08789 = 0.04155 0.00095 0.02016 0.01636 N22 3 0.92407 -0.38697 -0.23405 11.00000 0.04991 0.03020 = 0.03812 0.00395 0.02438 -0.00311 N23 3 0.90778 -0.26109 -0.14309 11.00000 0.04345 0.02745 = 0.05379 -0.00347 0.02392 -0.00615 C21 1 0.81141 -0.40671 -0.59740 11.00000 0.06890 0.04848 = 0.03278 0.00044 0.01994 0.01976 C22 1 0.76255 -0.46018 -0.54230 11.00000 0.05421 0.06555 = 0.04411 -0.01417 0.02433 -0.00795 C23 1 0.82072 -0.47164 -0.44775 11.00000 0.05062 0.04698 = 0.04063 -0.00041 0.02448 -0.00325 C24 1 0.92541 -0.43056 -0.40766 11.00000 0.04339 0.03372 = 0.03848 0.00247 0.02247 0.00419 C25 1 0.97565 -0.37950 -0.46191 11.00000 0.05603 0.03964 = 0.04408 0.00553 0.02742 -0.00056 C26 1 0.91872 -0.36739 -0.55569 11.00000 0.06972 0.03993 = 0.04423 0.00550 0.03127 -0.00078 C27 1 0.92923 -0.28808 -0.21971 11.00000 0.03903 0.03187 = 0.04630 0.00367 0.02085 -0.00238 C28 1 0.95112 -0.22357 -0.28186 11.00000 0.07594 0.04321 = 0.06334 0.00841 0.04019 -0.00271 C29 1 0.95028 -0.12837 -0.26260 11.00000 0.08193 0.03798 = 0.09231 0.01444 0.05587 0.00170 C210 1 0.92739 -0.09937 -0.18380 11.00000 0.06247 0.02596 = 0.10197 0.00493 0.04780 -0.00564 C211 1 0.90703 -0.16652 -0.12530 11.00000 0.05354 0.03447 = 0.07409 -0.00164 0.03717 -0.00106 H21A 2 0.79696 -0.37133 -0.72150 11.00000 0.07771 H21B 2 0.68959 -0.42609 -0.71828 11.00000 0.07535 H22A 2 0.90396 -0.41502 -0.19481 11.00000 0.03476 H22 2 0.69538 -0.48138 -0.56925 11.00000 0.05794 H23 2 0.78432 -0.50245 -0.41342 11.00000 0.04643 H25 2 1.05301 -0.35808 -0.43736 11.00000 0.04805 H26 2 0.95912 -0.33976 -0.58938 11.00000 0.04992 H28 2 0.95856 -0.24942 -0.34322 11.00000 0.08388 H29 2 0.95975 -0.07595 -0.31914 11.00000 0.09454 H211 2 0.89364 -0.15234 -0.06701 11.00000 0.06820 HKLF 4 1 -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000-1.0000 Covalent radii and connectivity table for s92 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 CL 0.990 S1 - O2 O1 N2 C4 Cl1 - C10 O1 - S1 O2 - S1 N1 - C1 N2 - C7 S1 N3 - C7 C11 C1 - N1 C6 C2 C2 - C3 C1 C3 - C2 C4 C4 - C3 C5 S1 C5 - C6 C4 C6 - C5 C1 C7 - N3 C8 N2 C8 - C9 C7 C9 - C8 C10 C10 - C11 C9 Cl1 C11 - N3 C10 S21 - O21 O22 N22 C24 Cl21 - C210 O21 - S21 O22 - S21 N21 - C21 N22 - C27 S21 N23 - C27 C211 C21 - N21 C26 C22 C22 - C23 C21 C23 - C24 C22 C24 - C23 C25 S21 C25 - C26 C24 C26 - C25 C21 C27 - N23 C28 N22 C28 - C29 C27 C29 - C28 C210 C210 - C211 C29 Cl21 C211 - N23 C210 h k l Fo^2 Sigma Why rejected -1 0 2 0.99 0.22 observed but should be systematically absent 22952 Reflections read, of which 601 rejected -14 =< h =< 14, -16 =< k =< 16, -18 =< l =< 18, Max. 2-theta = 50.10 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 4 0 0 7.32 0.64 4 12.96 4 3 0 10.97 0.47 8 3.20 4 4 0 5.97 0.50 8 4.07 -5 0 1 33.30 2.83 4 27.90 3 3 1 19.96 0.62 8 6.53 3 4 1 19.24 0.72 8 3.98 1 0 3 89.76 2.81 4 26.75 1 4 3 39.52 1.47 6 8.00 -2 3 5 5.10 0.57 4 3.12 1 15 5 4.38 0.78 5 4.12 2 0 6 2.95 0.82 3 6.41 -3 1 6 2.31 0.61 4 4.89 -2 1 6 24.85 1.50 4 22.12 -5 13 6 0.93 0.19 5 1.17 -11 10 7 4.19 0.77 3 3.89 -12 1 14 -0.49 0.74 5 3.69 -1 4 16 11.47 1.30 5 7.67 17 Inconsistent equivalents 4417 Unique reflections, of which 0 suppressed R(int) = 0.0868 R(sigma) = 0.0579 Friedel opposites merged Maximum memory for data reduction = 2695 / 44249 Least-squares cycle 1 Maximum vector length = 511 Memory required = 3640 / 521974 wR2 = 0.1770 before cycle 1 for 4417 data and 405 / 405 parameters GooF = S = 1.110; Restrained GooF = 1.110 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0826 * P )^2 + 2.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23139 0.00071 -0.005 OSF Mean shift/esd = 0.003 Maximum = 0.050 for y S21 Max. shift = 0.000 A for H5 Max. dU = 0.000 for H21B Least-squares cycle 2 Maximum vector length = 511 Memory required = 3640 / 521974 wR2 = 0.1770 before cycle 2 for 4417 data and 405 / 405 parameters GooF = S = 1.110; Restrained GooF = 1.110 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0826 * P )^2 + 2.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23139 0.00071 -0.002 OSF Mean shift/esd = 0.001 Maximum = 0.017 for y S21 Max. shift = 0.000 A for H2A Max. dU = 0.000 for H21B Least-squares cycle 3 Maximum vector length = 511 Memory required = 3640 / 521974 wR2 = 0.1770 before cycle 3 for 4417 data and 405 / 405 parameters GooF = S = 1.110; Restrained GooF = 1.110 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0826 * P )^2 + 2.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23139 0.00071 0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U23 C210 Max. shift = 0.000 A for H5 Max. dU = 0.000 for H21B Least-squares cycle 4 Maximum vector length = 511 Memory required = 3640 / 521974 wR2 = 0.1770 before cycle 4 for 4417 data and 405 / 405 parameters GooF = S = 1.110; Restrained GooF = 1.110 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0826 * P )^2 + 2.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23139 0.00071 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H21B Max. dU = 0.000 for H1A Largest correlation matrix elements 0.744 U13 Cl21 / U33 Cl21 0.549 U13 C210 / U33 C210 0.508 U13 C5 / U33 C5 0.729 U13 Cl21 / U11 Cl21 0.542 U13 C211 / U11 C211 0.506 U13 O21 / U33 O21 0.662 z Cl21 / x Cl21 0.526 U13 C25 / U11 C25 0.506 U13 C26 / U33 C26 0.604 U13 C29 / U11 C29 0.525 U13 C28 / U33 C28 0.505 U13 C22 / U11 C22 0.591 U12 Cl21 / U23 Cl21 0.521 U13 C211 / U33 C211 0.503 U13 C6 / U11 C6 0.589 U13 C29 / U33 C29 0.517 U13 C26 / U11 C26 0.501 U13 C23 / U11 C23 0.562 U13 C210 / U11 C210 0.510 U13 O21 / U11 O21 0.561 U13 C28 / U11 C28 0.510 U13 C5 / U11 C5 s92 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S1 0.75462 0.68325 0.02775 1.00000 0.04429 0.03703 0.03113 -0.00304 0.01409 0.00358 0.03708 0.00192 0.00008 0.00007 0.00007 0.00000 0.00056 0.00055 0.00052 0.00038 0.00042 0.00041 0.00028 Cl1 0.84205 0.21817 -0.08631 1.00000 0.08465 0.03335 0.09258 0.00101 0.04046 -0.00126 0.06743 0.00282 0.00012 0.00008 0.00010 0.00000 0.00090 0.00060 0.00099 0.00056 0.00077 0.00055 0.00040 O1 0.79104 0.78059 0.03041 1.00000 0.05732 0.03643 0.04393 -0.01152 0.01810 -0.00317 0.04556 0.00539 0.00025 0.00019 0.00019 0.00000 0.00176 0.00155 0.00163 0.00120 0.00137 0.00127 0.00070 O2 0.74404 0.64121 0.11077 1.00000 0.05648 0.05776 0.02637 0.00275 0.01702 0.00879 0.04605 0.00582 0.00025 0.00021 0.00018 0.00000 0.00175 0.00181 0.00139 0.00123 0.00127 0.00140 0.00071 N1 0.32734 0.62638 -0.28318 1.00000 0.03966 0.06526 0.04731 0.01377 0.00923 -0.00897 0.05203 0.00789 0.00034 0.00030 0.00030 0.00000 0.00217 0.00262 0.00235 0.00192 0.00181 0.00180 0.00099 N2 0.84984 0.62380 -0.00242 1.00000 0.03821 0.03140 0.03900 0.00311 0.01696 0.00191 0.03517 0.00660 0.00028 0.00023 0.00025 0.00000 0.00180 0.00175 0.00189 0.00144 0.00154 0.00136 0.00075 N3 0.86402 0.49788 -0.09619 1.00000 0.03970 0.02870 0.03851 0.00306 0.01574 -0.00039 0.03494 0.00615 0.00026 0.00021 0.00022 0.00000 0.00172 0.00161 0.00178 0.00130 0.00142 0.00132 0.00071 C1 0.42420 0.64392 -0.20907 1.00000 0.03933 0.03435 0.04466 0.00620 0.01828 0.00533 0.03836 0.00817 0.00033 0.00027 0.00028 0.00000 0.00214 0.00204 0.00230 0.00168 0.00188 0.00163 0.00090 C2 0.43988 0.60217 -0.12177 1.00000 0.03991 0.04083 0.04630 0.01022 0.02085 -0.00167 0.04071 0.00860 0.00035 0.00029 0.00030 0.00000 0.00218 0.00222 0.00236 0.00178 0.00191 0.00174 0.00093 C3 0.53985 0.61502 -0.04917 1.00000 0.04622 0.03971 0.03649 0.00967 0.01935 0.00546 0.03941 0.00846 0.00034 0.00028 0.00029 0.00000 0.00232 0.00219 0.00220 0.00170 0.00188 0.00176 0.00092 C4 0.62605 0.66998 -0.06162 1.00000 0.03783 0.03231 0.02883 0.00220 0.01386 0.00688 0.03229 0.00735 0.00031 0.00025 0.00025 0.00000 0.00200 0.00191 0.00188 0.00146 0.00159 0.00155 0.00081 C5 0.60979 0.71370 -0.14866 1.00000 0.03926 0.03876 0.03770 0.00505 0.01980 -0.00334 0.03682 0.00791 0.00033 0.00028 0.00027 0.00000 0.00215 0.00213 0.00216 0.00165 0.00183 0.00170 0.00088 C6 0.51101 0.70016 -0.21995 1.00000 0.04418 0.03930 0.03660 0.00846 0.02083 0.00118 0.03818 0.00834 0.00034 0.00029 0.00029 0.00000 0.00227 0.00214 0.00220 0.00176 0.00187 0.00175 0.00089 C7 0.84227 0.52453 -0.01988 1.00000 0.02725 0.03140 0.03658 0.00210 0.00935 0.00349 0.03205 0.00713 0.00029 0.00026 0.00026 0.00000 0.00177 0.00191 0.00201 0.00153 0.00154 0.00143 0.00080 C8 0.81981 0.46086 0.04168 1.00000 0.04358 0.04383 0.03874 0.01032 0.01854 0.00788 0.04083 0.00874 0.00034 0.00030 0.00029 0.00000 0.00230 0.00234 0.00225 0.00181 0.00186 0.00177 0.00094 C9 0.81861 0.36541 0.02254 1.00000 0.04769 0.03794 0.04922 0.01281 0.02212 0.00084 0.04344 0.00899 0.00036 0.00030 0.00031 0.00000 0.00241 0.00227 0.00252 0.00188 0.00202 0.00182 0.00099 C10 0.84157 0.33727 -0.05715 1.00000 0.04319 0.02806 0.05968 0.00028 0.01994 -0.00249 0.04292 0.00834 0.00035 0.00027 0.00032 0.00000 0.00223 0.00197 0.00268 0.00183 0.00202 0.00166 0.00097 C11 0.86524 0.40414 -0.11367 1.00000 0.04883 0.03333 0.04545 0.00053 0.02051 -0.00140 0.04132 0.00832 0.00035 0.00028 0.00030 0.00000 0.00234 0.00208 0.00239 0.00174 0.00196 0.00174 0.00093 H1A 0.26215 0.61298 -0.27619 1.00000 0.06755 0.10803 0.00495 0.00356 0.00376 0.00000 0.01619 H1B 0.32163 0.65721 -0.33465 1.00000 0.05089 0.09262 0.00388 0.00336 0.00358 0.00000 0.01324 H2A 0.87048 0.65257 -0.03676 1.00000 0.04550 0.09120 0.00389 0.00328 0.00333 0.00000 0.01399 H3 0.54970 0.58781 0.01603 1.00000 0.06187 0.09461 0.00394 0.00344 0.00353 0.00000 0.01367 H4 0.38034 0.56408 -0.10815 1.00000 0.06130 0.09480 0.00414 0.00345 0.00331 0.00000 0.01367 H5 0.67174 0.75554 -0.15783 1.00000 0.05172 0.08777 0.00379 0.00321 0.00298 0.00000 0.01200 H6 0.50237 0.72732 -0.27381 1.00000 0.03945 0.07979 0.00336 0.00293 0.00299 0.00000 0.01114 H8 0.80826 0.48541 0.09730 1.00000 0.04024 0.08047 0.00338 0.00288 0.00301 0.00000 0.01087 H9 0.80040 0.31597 0.05617 1.00000 0.05354 0.09033 0.00383 0.00336 0.00328 0.00000 0.01287 H11 0.87818 0.38586 -0.17602 1.00000 0.05912 0.09411 0.00402 0.00322 0.00356 0.00000 0.01350 S21 0.99616 -0.44630 -0.28844 1.00000 0.04288 0.03854 0.03976 0.00508 0.02046 0.00427 0.03871 0.00206 0.00008 0.00007 0.00007 0.00000 0.00056 0.00056 0.00057 0.00041 0.00045 0.00041 0.00028 Cl21 0.92514 0.01894 -0.15627 1.00000 0.13123 0.03210 0.20409 -0.00383 0.12056 -0.00550 0.10635 0.00434 0.00017 0.00009 0.00017 0.00000 0.00144 0.00067 0.00213 0.00088 0.00153 0.00074 0.00073 O21 0.98701 -0.54323 -0.26280 1.00000 0.06600 0.03819 0.04756 0.00896 0.03064 0.01240 0.04765 0.00619 0.00026 0.00020 0.00020 0.00000 0.00193 0.00155 0.00168 0.00126 0.00149 0.00134 0.00073 O22 1.10645 -0.40442 -0.26676 1.00000 0.03938 0.07144 0.05506 0.00531 0.01860 -0.00094 0.05456 0.00626 0.00024 0.00024 0.00022 0.00000 0.00162 0.00211 0.00188 0.00156 0.00141 0.00145 0.00079 N21 0.75309 -0.39205 -0.69023 1.00000 0.09090 0.08789 0.04155 0.00095 0.02016 0.01636 0.07388 0.01256 0.00057 0.00043 0.00032 0.00000 0.00390 0.00368 0.00257 0.00236 0.00272 0.00313 0.00140 N22 0.92407 -0.38697 -0.23405 1.00000 0.04991 0.03020 0.03812 0.00395 0.02438 -0.00311 0.03698 0.00665 0.00029 0.00022 0.00024 0.00000 0.00198 0.00172 0.00186 0.00139 0.00161 0.00141 0.00077 N23 0.90778 -0.26109 -0.14309 1.00000 0.04345 0.02745 0.05379 -0.00347 0.02392 -0.00615 0.03962 0.00639 0.00027 0.00022 0.00024 0.00000 0.00183 0.00162 0.00208 0.00145 0.00162 0.00138 0.00077 C21 0.81141 -0.40671 -0.59740 1.00000 0.06890 0.04848 0.03278 0.00044 0.01994 0.01976 0.04928 0.00936 0.00041 0.00032 0.00028 0.00000 0.00298 0.00248 0.00223 0.00180 0.00213 0.00221 0.00110 C22 0.76255 -0.46018 -0.54230 1.00000 0.05421 0.06555 0.04411 -0.01417 0.02433 -0.00795 0.05263 0.00999 0.00045 0.00036 0.00033 0.00000 0.00288 0.00307 0.00260 0.00222 0.00229 0.00237 0.00115 C23 0.82072 -0.47164 -0.44775 1.00000 0.05062 0.04698 0.04063 -0.00041 0.02448 -0.00325 0.04375 0.00862 0.00037 0.00031 0.00030 0.00000 0.00253 0.00245 0.00237 0.00187 0.00206 0.00195 0.00099 C24 0.92541 -0.43056 -0.40766 1.00000 0.04339 0.03372 0.03848 0.00247 0.02247 0.00419 0.03632 0.00784 0.00032 0.00026 0.00027 0.00000 0.00214 0.00198 0.00212 0.00161 0.00176 0.00168 0.00086 C25 0.97565 -0.37950 -0.46191 1.00000 0.05603 0.03964 0.04408 0.00553 0.02742 -0.00056 0.04390 0.00952 0.00041 0.00030 0.00031 0.00000 0.00272 0.00227 0.00244 0.00179 0.00214 0.00196 0.00099 C26 0.91872 -0.36739 -0.55569 1.00000 0.06972 0.03993 0.04423 0.00550 0.03127 -0.00078 0.04822 0.00963 0.00043 0.00030 0.00032 0.00000 0.00308 0.00234 0.00253 0.00187 0.00241 0.00215 0.00108 C27 0.92923 -0.28808 -0.21971 1.00000 0.03903 0.03187 0.04630 0.00367 0.02085 -0.00238 0.03740 0.00785 0.00032 0.00027 0.00028 0.00000 0.00207 0.00203 0.00232 0.00165 0.00183 0.00159 0.00088 C28 0.95112 -0.22357 -0.28186 1.00000 0.07594 0.04321 0.06334 0.00841 0.04019 -0.00271 0.05658 0.01086 0.00045 0.00033 0.00037 0.00000 0.00326 0.00256 0.00307 0.00218 0.00268 0.00224 0.00121 C29 0.95028 -0.12837 -0.26260 1.00000 0.08193 0.03798 0.09231 0.01444 0.05587 0.00170 0.06404 0.01201 0.00048 0.00033 0.00042 0.00000 0.00355 0.00251 0.00401 0.00246 0.00323 0.00233 0.00141 C210 0.92739 -0.09937 -0.18380 1.00000 0.06247 0.02596 0.10197 0.00493 0.04780 -0.00564 0.05837 0.01068 0.00041 0.00029 0.00041 0.00000 0.00287 0.00210 0.00401 0.00227 0.00287 0.00194 0.00131 C211 0.90703 -0.16652 -0.12530 1.00000 0.05354 0.03447 0.07409 -0.00164 0.03717 -0.00106 0.05005 0.00982 0.00039 0.00030 0.00038 0.00000 0.00260 0.00226 0.00331 0.00210 0.00246 0.00190 0.00111 H21A 0.79696 -0.37133 -0.72150 1.00000 0.07771 0.12058 0.00526 0.00400 0.00454 0.00000 0.02003 H21B 0.68959 -0.42609 -0.71828 1.00000 0.07535 0.12411 0.00523 0.00420 0.00420 0.00000 0.01958 H22A 0.90396 -0.41502 -0.19481 1.00000 0.03476 0.07927 0.00333 0.00296 0.00295 0.00000 0.01104 H22 0.69538 -0.48138 -0.56925 1.00000 0.05794 0.10159 0.00437 0.00351 0.00347 0.00000 0.01466 H23 0.78432 -0.50245 -0.41342 1.00000 0.04643 0.08339 0.00362 0.00305 0.00307 0.00000 0.01203 H25 1.05301 -0.35808 -0.43736 1.00000 0.04805 0.09416 0.00413 0.00308 0.00320 0.00000 0.01227 H26 0.95912 -0.33976 -0.58938 1.00000 0.04992 0.08834 0.00384 0.00317 0.00329 0.00000 0.01250 H28 0.95856 -0.24942 -0.34322 1.00000 0.08388 0.11251 0.00463 0.00408 0.00414 0.00000 0.01749 H29 0.95975 -0.07595 -0.31914 1.00000 0.09454 0.11681 0.00500 0.00433 0.00429 0.00000 0.01873 H211 0.89364 -0.15234 -0.06701 1.00000 0.06820 0.10324 0.00439 0.00365 0.00383 0.00000 0.01557 Final Structure Factor Calculation for s92 in P2(1)/n Total number of l.s. parameters = 405 Maximum vector length = 511 Memory required = 3235 / 25039 wR2 = 0.1770 before cycle 5 for 4417 data and 0 / 405 parameters GooF = S = 1.110; Restrained GooF = 1.110 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0826 * P )^2 + 2.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0598 for 3306 Fo > 4sig(Fo) and 0.0820 for all 4417 data wR2 = 0.1770, GooF = S = 1.110, Restrained GooF = 1.110 for all data Occupancy sum of asymmetric unit = 36.00 for non-hydrogen and 20.00 for hydrogen atoms Principal mean square atomic displacements U 0.0461 0.0374 0.0277 S1 0.0977 0.0714 0.0332 Cl1 0.0579 0.0510 0.0278 O1 0.0660 0.0484 0.0238 O2 0.0797 0.0400 0.0364 N1 0.0426 0.0327 0.0302 N2 0.0414 0.0361 0.0273 N3 0.0493 0.0349 0.0308 C1 0.0543 0.0418 0.0261 C2 0.0526 0.0387 0.0269 C3 0.0426 0.0282 0.0262 C4 0.0441 0.0422 0.0242 C5 0.0494 0.0407 0.0244 C6 0.0377 0.0331 0.0253 C7 0.0555 0.0368 0.0302 C8 0.0583 0.0450 0.0270 C9 0.0597 0.0416 0.0275 C10 0.0511 0.0399 0.0329 C11 0.0495 0.0359 0.0307 S21 0.2263 0.0611 0.0317 Cl21 may be split into 0.9401 0.0186 -0.1455 and 0.9102 0.0193 -0.1670 0.0739 0.0363 0.0327 O21 0.0732 0.0536 0.0369 O22 0.1077 0.0733 0.0406 N21 0.0531 0.0351 0.0228 N22 0.0569 0.0368 0.0252 N23 0.0816 0.0382 0.0280 C21 0.0749 0.0501 0.0328 C22 0.0549 0.0462 0.0301 C23 0.0491 0.0327 0.0271 C24 0.0599 0.0427 0.0290 C25 0.0718 0.0435 0.0294 C26 0.0489 0.0365 0.0268 C27 0.0837 0.0531 0.0330 C28 0.1096 0.0524 0.0301 C29 0.1059 0.0470 0.0223 C210 0.0790 0.0368 0.0344 C211 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.019 0.029 0.040 0.053 0.067 0.087 0.119 0.177 1.000 Number in group 458. 437. 440. 436. 443. 434. 447. 437. 440. 445. GooF 1.258 1.103 1.222 1.123 0.969 1.273 0.922 1.050 1.014 1.109 K 4.799 1.384 1.131 1.013 0.967 1.001 0.997 1.024 1.039 0.994 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.25 1.44 1.80 inf Number in group 449. 444. 431. 449. 445. 434. 447. 442. 432. 444. GooF 0.886 0.864 0.906 0.977 1.015 1.056 1.144 1.182 1.331 1.551 K 1.005 0.992 0.991 1.023 1.027 1.038 1.052 1.037 1.045 0.970 R1 0.203 0.166 0.133 0.103 0.087 0.066 0.057 0.053 0.056 0.063 Recommended weighting scheme: WGHT 0.0826 2.9024 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 2 4 751.19 167.45 11.34 0.061 2.18 2 7 5 720.10 199.07 8.97 0.066 1.51 5 8 2 212.25 0.99 8.52 0.005 1.33 1 2 6 268.00 51.02 8.28 0.033 2.10 -11 4 4 229.16 0.07 8.12 0.001 1.08 -10 1 3 427.56 128.98 6.95 0.053 1.24 6 4 1 1151.48 524.87 6.90 0.107 1.65 6 9 1 136.97 16.80 6.82 0.019 1.20 7 9 0 319.55 95.20 6.42 0.046 1.14 3 9 4 108.31 0.07 6.33 0.001 1.29 4 12 3 88.39 0.90 5.78 0.004 1.03 -1 5 8 88.51 9.37 5.46 0.014 1.55 -3 11 10 208.44 28.64 5.45 0.025 0.98 -6 2 13 228.96 71.68 5.17 0.040 1.12 1 9 6 264.07 113.46 5.00 0.050 1.27 2 6 5 1045.30 623.64 4.79 0.117 1.64 8 4 3 144.49 29.89 4.73 0.026 1.21 4 3 3 120.32 37.58 4.73 0.029 1.99 -2 1 9 2129.65 1335.43 4.61 0.171 1.67 6 11 1 155.69 47.22 4.51 0.032 1.05 3 10 4 1097.09 673.60 4.38 0.122 1.20 -5 5 12 61.67 2.00 4.35 0.007 1.13 7 12 0 84.86 14.28 4.23 0.018 0.96 4 5 3 1038.74 656.92 4.19 0.120 1.73 6 2 5 129.51 34.89 4.17 0.028 1.39 -8 8 1 76.93 17.37 4.10 0.020 1.15 5 1 2 3612.15 2489.77 4.06 0.234 2.02 9 7 5 65.97 0.92 3.93 0.004 0.94 6 6 1 251.75 133.12 3.88 0.054 1.46 2 4 5 60.42 12.40 3.86 0.017 1.92 3 12 4 80.86 18.91 3.84 0.020 1.04 9 3 5 107.48 30.04 3.84 0.026 1.04 7 10 0 134.17 53.22 3.82 0.034 1.08 -7 5 14 53.00 0.01 3.73 0.000 0.97 -10 2 3 966.16 632.93 3.68 0.118 1.22 -1 7 8 947.40 607.07 3.67 0.115 1.36 -8 6 1 36.42 0.05 3.65 0.001 1.27 -6 7 13 83.94 17.36 3.58 0.020 0.99 -3 5 7 76.69 16.98 3.51 0.019 1.69 6 5 4 65.12 9.09 3.38 0.014 1.34 6 4 5 382.65 204.27 3.33 0.067 1.31 -12 1 5 46.28 0.16 3.23 0.002 1.04 -2 1 1 3974.25 5495.22 3.19 0.347 5.68 7 9 4 86.90 16.61 3.17 0.019 1.02 3 4 8 102.54 32.42 3.16 0.027 1.34 -5 6 12 58.12 9.25 3.07 0.014 1.10 5 5 2 717.06 504.66 3.03 0.105 1.65 3 4 4 306.18 465.76 3.03 0.101 1.92 -4 2 11 1049.47 743.65 2.99 0.128 1.34 -2 8 9 120.71 59.99 2.96 0.036 1.21 Bond lengths and angles S1 - Distance Angles O2 1.4333 (0.0029) O1 1.4370 (0.0029) 119.17 (0.17) N2 1.6360 (0.0034) 108.69 (0.18) 103.96 (0.18) C4 1.7322 (0.0038) 108.06 (0.18) 109.07 (0.17) 107.31 (0.17) S1 - O2 O1 N2 Cl1 - Distance Angles C10 1.7304 (0.0040) Cl1 - O1 - Distance Angles S1 1.4370 (0.0029) O1 - O2 - Distance Angles S1 1.4333 (0.0029) O2 - N1 - Distance Angles C1 1.3717 (0.0057) N1 - N2 - Distance Angles C7 1.4163 (0.0048) S1 1.6360 (0.0034) 123.01 (0.27) N2 - C7 N3 - Distance Angles C7 1.3247 (0.0048) C11 1.3441 (0.0050) 117.86 (0.33) N3 - C7 C1 - Distance Angles N1 1.3717 (0.0057) C6 1.3936 (0.0056) 120.92 (0.38) C2 1.3988 (0.0056) 120.46 (0.38) 118.56 (0.38) C1 - N1 C6 C2 - Distance Angles C3 1.3740 (0.0059) C1 1.3988 (0.0056) 120.42 (0.37) C2 - C3 C3 - Distance Angles C2 1.3740 (0.0059) C4 1.3864 (0.0056) 120.27 (0.36) C3 - C2 C4 - Distance Angles C3 1.3864 (0.0056) C5 1.4059 (0.0052) 119.52 (0.35) S1 1.7322 (0.0038) 120.89 (0.29) 119.58 (0.29) C4 - C3 C5 C5 - Distance Angles C6 1.3560 (0.0057) C4 1.4059 (0.0052) 119.71 (0.36) C5 - C6 C6 - Distance Angles C5 1.3560 (0.0057) C1 1.3936 (0.0056) 121.51 (0.38) C6 - C5 C7 - Distance Angles N3 1.3247 (0.0048) C8 1.3854 (0.0054) 123.32 (0.35) N2 1.4163 (0.0048) 114.87 (0.32) 121.73 (0.36) C7 - N3 C8 C8 - Distance Angles C9 1.3704 (0.0059) C7 1.3854 (0.0054) 118.68 (0.39) C8 - C9 C9 - Distance Angles C8 1.3704 (0.0059) C10 1.3862 (0.0062) 118.15 (0.38) C9 - C8 C10 - Distance Angles C11 1.3669 (0.0058) C9 1.3862 (0.0062) 119.88 (0.38) Cl1 1.7304 (0.0040) 119.00 (0.35) 121.11 (0.32) C10 - C11 C9 C11 - Distance Angles N3 1.3441 (0.0050) C10 1.3669 (0.0058) 122.07 (0.40) C11 - N3 S21 - Distance Angles O21 1.4305 (0.0029) O22 1.4311 (0.0031) 119.07 (0.19) N22 1.6343 (0.0034) 104.00 (0.17) 108.83 (0.19) C24 1.7403 (0.0040) 110.09 (0.18) 107.74 (0.19) 106.42 (0.18) S21 - O21 O22 N22 Cl21 - Distance Angles C210 1.7157 (0.0044) Cl21 - O21 - Distance Angles S21 1.4305 (0.0029) O21 - O22 - Distance Angles S21 1.4311 (0.0031) O22 - N21 - Distance Angles C21 1.3670 (0.0062) N21 - N22 - Distance Angles C27 1.4040 (0.0049) S21 1.6343 (0.0034) 125.28 (0.28) N22 - C27 N23 - Distance Angles C27 1.3286 (0.0051) C211 1.3560 (0.0052) 117.99 (0.35) N23 - C27 C21 - Distance Angles N21 1.3670 (0.0062) C26 1.3915 (0.0068) 120.75 (0.49) C22 1.4026 (0.0066) 120.23 (0.52) 119.01 (0.40) C21 - N21 C26 C22 - Distance Angles C23 1.3830 (0.0065) C21 1.4026 (0.0066) 119.66 (0.45) C22 - C23 C23 - Distance Angles C24 1.3720 (0.0058) C22 1.3830 (0.0065) 120.36 (0.41) C23 - C24 C24 - Distance Angles C23 1.3720 (0.0058) C25 1.3863 (0.0055) 120.43 (0.39) S21 1.7403 (0.0040) 119.15 (0.30) 120.40 (0.33) C24 - C23 C25 C25 - Distance Angles C26 1.3713 (0.0064) C24 1.3863 (0.0055) 119.75 (0.43) C25 - C26 C26 - Distance Angles C25 1.3713 (0.0064) C21 1.3915 (0.0068) 120.75 (0.41) C26 - C25 C27 - Distance Angles N23 1.3286 (0.0051) C28 1.3965 (0.0058) 122.93 (0.38) N22 1.4040 (0.0049) 113.89 (0.32) 123.16 (0.38) C27 - N23 C28 C28 - Distance Angles C29 1.3692 (0.0067) C27 1.3965 (0.0058) 118.24 (0.46) C28 - C29 C29 - Distance Angles C28 1.3692 (0.0067) C210 1.3767 (0.0074) 119.45 (0.43) C29 - C28 C210 - Distance Angles C211 1.3735 (0.0066) C29 1.3767 (0.0074) 119.40 (0.42) Cl21 1.7157 (0.0044) 119.15 (0.41) 121.44 (0.35) C210 - C211 C29 C211 - Distance Angles N23 1.3560 (0.0052) C210 1.3735 (0.0066) 121.98 (0.46) C211 - N23 FMAP and GRID set by program FMAP 2 3 20 GRID -1.471 -2 -2 1.471 2 2 R1 = 0.0815 for 4417 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.50 at 0.7177 0.4529 0.0034 [ 1.22 A from C8 ] Deepest hole -0.50 at 0.7208 0.7218 0.0482 [ 0.81 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 3196 / 24235 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7177 0.4529 0.0034 1.00000 0.05 0.50 1.22 C8 1.56 H8 1.71 C9 1.98 C7 Q2 1 1.0560 -0.0551 -0.2196 1.00000 0.05 0.49 1.61 H29 1.63 C29 1.68 H21B 1.96 C210 Q3 1 0.5403 0.8144 -0.1819 1.00000 0.05 0.35 1.65 C5 1.70 C6 1.76 H5 1.79 H6 Q4 1 0.9369 -0.0574 -0.3549 1.00000 0.05 0.31 0.58 H29 1.68 C29 2.56 C28 2.70 C210 Q5 1 0.9152 0.2791 -0.0149 1.00000 0.05 0.31 1.24 C10 1.44 CL1 1.92 C9 2.12 H9 Q6 1 0.7977 -0.0153 -0.1543 1.00000 0.05 0.30 1.67 CL21 1.68 H23 2.17 C210 2.42 H211 Q7 1 0.7003 0.8151 -0.0306 1.00000 0.05 0.30 1.29 O1 2.02 H5 2.07 S1 2.22 C4 Q8 1 0.4638 0.8141 -0.2821 1.00000 0.05 0.29 1.30 H6 1.85 C6 2.14 O21 2.48 H11 Q9 1 0.2466 0.6159 -0.1679 1.00000 0.05 0.28 1.71 H1A 1.77 H4 1.91 O22 2.03 H8 Q10 1 1.1637 -0.3617 -0.4679 1.00000 0.05 0.28 1.60 H25 1.96 O1 2.32 H1B 2.39 C25 Shortest distances between peaks (including symmetry equivalents) 7 10 1.35 3 8 1.50 2 4 2.09 1 4 2.43 3 7 2.49 1 9 2.57 Time profile in seconds ----------------------- 0.11: 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. 1.81: 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 11.15: Structure factors and derivatives 43.05: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 4.57: Solve l.s. equations 0.00: Generate HTAB table 0.11: Other dependent quantities, CIF, tables 0.59: Analysis of variance 0.39: Merge reflections for Fourier and .fcf 0.28: Fourier summations 0.20: Peaksearch 0.05: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 09:30:02 Total elapsed time: 62.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++