+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - MSDOS 32-BIT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-1 + + s92 started at 11:08:05 on 16-Sep-1999 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P-1 CELL 0.71073 9.933 11.528 12.703 115.74 100.11 95.54 ZERR 4.00 0.002 0.002 0.003 0.03 0.03 0.03 LATT 1 SFAC C H N O S BR UNIT 44 40 12 8 4 4 V = 1265.19 F(000) = 656.0 Mu = 3.41 mm-1 Cell Wt = 1312.76 Rho = 1.723 FMAP 2 ACTA PLAN 10 L.S. 4 BOND WGHT 0.049700 FVAR 0.19116 BR1 6 0.59401 0.22560 0.10565 11.00000 0.02552 0.04097 = 0.05078 0.01737 0.00518 -0.00113 S1 5 -0.06856 -0.11714 -0.30521 11.00000 0.02500 0.03766 = 0.02622 0.00986 0.00636 0.00847 O1 4 -0.20298 -0.18385 -0.31133 11.00000 0.02117 0.04756 = 0.03444 0.00948 0.00553 0.00409 O2 4 -0.06605 -0.02523 -0.35285 11.00000 0.04123 0.04156 = 0.03547 0.01764 0.01179 0.01831 N1 3 0.27999 -0.49171 -0.53506 11.00000 0.04734 0.03830 = 0.04266 0.02458 0.02586 0.02258 N2 3 0.00518 -0.04555 -0.16214 11.00000 0.02446 0.04583 = 0.02622 0.01148 0.01249 0.00423 N3 3 0.17835 0.06128 0.01134 11.00000 0.02275 0.03991 = 0.02681 0.01312 0.00586 0.00356 C1 1 0.19422 -0.41066 -0.48638 11.00000 0.02575 0.02679 = 0.03080 0.01084 0.00902 0.00087 C2 1 0.15227 -0.40323 -0.38326 11.00000 0.02630 0.03205 = 0.03081 0.01765 0.00539 0.00495 C3 1 0.07204 -0.31555 -0.32900 11.00000 0.02422 0.03735 = 0.02495 0.01301 0.00711 0.00175 C4 1 0.03133 -0.23027 -0.37429 11.00000 0.02252 0.02793 = 0.02342 0.00788 0.00220 0.00201 C5 1 0.06888 -0.23777 -0.47739 11.00000 0.02562 0.02556 = 0.02525 0.00925 0.00321 0.00139 C6 1 0.14701 -0.32771 -0.53299 11.00000 0.02940 0.03374 = 0.02413 0.01254 0.00834 0.00244 C7 1 0.14252 0.02316 -0.10583 11.00000 0.02110 0.02884 = 0.03000 0.01045 0.00633 0.00795 C8 1 0.23353 0.04791 -0.16802 11.00000 0.03249 0.03853 = 0.02453 0.01143 0.01086 0.00370 C9 1 0.36828 0.10957 -0.10673 11.00000 0.03061 0.03381 = 0.03647 0.01431 0.01539 0.00279 C10 1 0.40867 0.14566 0.01532 11.00000 0.02541 0.02546 = 0.04054 0.01412 0.00894 0.00309 C11 1 0.31085 0.12319 0.07187 11.00000 0.03211 0.03501 = 0.02629 0.01235 0.00433 0.00322 H1A 2 0.30711 -0.55053 -0.50805 11.00000 0.05039 H1B 2 0.28901 -0.50443 -0.60961 11.00000 0.04948 H2A 2 -0.03239 -0.05395 -0.12859 11.00000 0.02252 H2 2 0.18643 -0.45287 -0.35063 11.00000 0.02794 H3 2 0.04399 -0.31374 -0.26342 11.00000 0.01974 H5 2 0.04423 -0.18399 -0.50855 11.00000 0.01777 H6 2 0.17671 -0.33617 -0.60351 11.00000 0.03161 H8 2 0.20798 0.01916 -0.25147 11.00000 0.02056 H9 2 0.43622 0.13381 -0.14356 11.00000 0.05776 H11 2 0.33319 0.14752 0.16088 11.00000 0.03709 BR21 6 0.92850 0.29196 -0.00636 11.00000 0.02883 0.05008 = 0.04113 0.02051 0.01330 0.00326 S21 5 1.46049 0.37314 -0.29748 11.00000 0.03103 0.03450 = 0.02555 0.01541 0.01028 0.00686 O21 4 1.59462 0.44828 -0.27825 11.00000 0.03366 0.03950 = 0.03355 0.01788 0.01409 0.00082 O22 4 1.34572 0.36599 -0.38743 11.00000 0.03666 0.04214 = 0.02739 0.01835 0.00673 0.01140 N21 3 1.50863 -0.16324 -0.37987 11.00000 0.02651 0.03678 = 0.04250 0.01737 0.00947 0.00697 N22 3 1.42247 0.44188 -0.16675 11.00000 0.02190 0.03525 = 0.02584 0.01202 0.00460 -0.00081 N23 3 1.31789 0.43243 -0.02128 11.00000 0.02681 0.03324 = 0.02681 0.01275 0.00727 0.00364 C21 1 1.49997 -0.03899 -0.36351 11.00000 0.02514 0.03663 = 0.02865 0.01475 0.01642 0.00834 C22 1 1.61085 0.06581 -0.29119 11.00000 0.02066 0.03923 = 0.02390 0.01209 0.00664 0.00522 C23 1 1.59904 0.19109 -0.27212 11.00000 0.02126 0.03655 = 0.02479 0.00995 0.00828 0.00096 C24 1 1.47650 0.21396 -0.32652 11.00000 0.02927 0.03062 = 0.02069 0.00962 0.00920 0.00865 C25 1 1.36675 0.10988 -0.40119 11.00000 0.02375 0.03681 = 0.02338 0.01281 0.00932 0.00756 C26 1 1.37759 -0.01528 -0.41902 11.00000 0.02111 0.03395 = 0.02519 0.00965 0.00699 0.00160 C27 1 1.30169 0.40124 -0.13820 11.00000 0.03093 0.02964 = 0.03112 0.01671 0.00991 0.01036 C28 1 1.17455 0.33520 -0.22335 11.00000 0.02969 0.04180 = 0.02869 0.01461 0.00635 0.00296 C29 1 1.06290 0.30161 -0.18488 11.00000 0.03380 0.03254 = 0.02757 0.01069 0.00243 0.00612 C210 1 1.07965 0.33454 -0.06447 11.00000 0.02575 0.03311 = 0.03849 0.01630 0.00972 0.00357 C211 1 1.20729 0.40070 0.01501 11.00000 0.02876 0.03482 = 0.02996 0.01342 0.01097 0.00608 H21A 2 1.58930 -0.18163 -0.36593 11.00000 0.02631 H21B 2 1.44268 -0.22496 -0.42323 11.00000 0.03651 H22A 2 1.48643 0.47889 -0.11280 11.00000 0.01762 H22 2 1.69748 0.05771 -0.25017 11.00000 0.02465 H23 2 1.66866 0.25854 -0.22709 11.00000 0.01305 H25 2 1.27938 0.12186 -0.44370 11.00000 0.03500 H26 2 1.30631 -0.08728 -0.47197 11.00000 0.03119 H28 2 1.17776 0.32448 -0.29852 11.00000 0.04795 H29 2 0.97500 0.25022 -0.24119 11.00000 0.04049 H211 2 1.23239 0.43104 0.11270 11.00000 0.02271 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 BR 1.140 Br1 - C10 S1 - O2 O1 N2 C4 O1 - S1 O2 - S1 N1 - C1 N2 - C7 S1 N3 - C7 C11 C1 - N1 C6 C2 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 S1 C5 - C6 C4 C6 - C5 C1 C7 - N3 C8 N2 C8 - C9 C7 C9 - C8 C10 C10 - C11 C9 Br1 C11 - N3 C10 Br21 - C210 S21 - O22 O21 N22 C24 O21 - S21 O22 - S21 N21 - C21 N22 - C27 S21 N23 - C211 C27 C21 - N21 C22 C26 C22 - C23 C21 C23 - C22 C24 C24 - C25 C23 S21 C25 - C26 C24 C26 - C25 C21 C27 - N23 C28 N22 C28 - C29 C27 C29 - C28 C210 C210 - C211 C29 Br21 C211 - N23 C210 15587 Reflections read, of which 0 rejected -11 =< h =< 11, -13 =< k =< 13, -14 =< l =< 15, Max. 2-theta = 50.14 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 6 -8 9 -0.25 0.25 2 2.27 -2 -12 10 -0.10 0.80 4 9.74 2 Inconsistent equivalents 4468 Unique reflections, of which 0 suppressed R(int) = 0.0747 R(sigma) = 0.0671 Friedel opposites merged Maximum memory for data reduction = 2671 / 44908 Least-squares cycle 1 Maximum vector length = 511 Memory required = 3628 / 521974 wR2 = 0.1050 before cycle 1 for 4468 data and 405 / 405 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0497 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19116 0.00033 -0.013 OSF Mean shift/esd = 0.003 Maximum = 0.076 for z Br21 Max. shift = 0.000 A for C4 Max. dU = 0.000 for H1A Least-squares cycle 2 Maximum vector length = 511 Memory required = 3628 / 521974 wR2 = 0.1050 before cycle 2 for 4468 data and 405 / 405 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0497 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19116 0.00033 0.003 OSF Mean shift/esd = 0.001 Maximum = 0.025 for z Br21 Max. shift = 0.000 A for H26 Max. dU = 0.000 for H28 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3628 / 521974 wR2 = 0.1050 before cycle 3 for 4468 data and 405 / 405 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0497 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19116 0.00033 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z H11 Max. shift = 0.000 A for H11 Max. dU = 0.000 for H1A Least-squares cycle 4 Maximum vector length = 511 Memory required = 3628 / 521974 wR2 = 0.1050 before cycle 4 for 4468 data and 405 / 405 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0497 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19116 0.00033 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for x Br1 Max. shift = 0.000 A for H11 Max. dU = 0.000 for H11 Largest correlation matrix elements 0.667 U23 O22 / U22 O22 0.657 U23 O21 / U33 O21 0.645 U23 N21 / U33 N21 0.665 U23 Br21 / U22 Br21 0.657 U23 C27 / U33 C27 0.643 U23 C25 / U22 C25 0.663 U23 C27 / U22 C27 0.655 U23 C2 / U22 C2 0.643 U23 C24 / U22 C24 0.662 U23 S21 / U22 S21 0.652 U23 O21 / U22 O21 0.642 U23 C21 / U22 C21 0.660 U23 C2 / U33 C2 0.649 U23 N1 / U22 N1 0.642 U23 C10 / U33 C10 0.660 U23 Br21 / U33 Br21 0.648 U23 N1 / U33 N1 0.642 U23 N21 / U22 N21 0.660 U23 O22 / U33 O22 0.648 U23 C21 / U33 C21 0.641 U23 N22 / U33 N22 0.659 U23 S21 / U33 S21 0.646 U23 C210 / U33 C210 0.640 U23 C210 / U22 C210 s92 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Br1 0.59401 0.22560 0.10565 1.00000 0.02552 0.04097 0.05078 0.01737 0.00518 -0.00113 0.04164 0.00113 0.00004 0.00005 0.00004 0.00000 0.00025 0.00028 0.00033 0.00025 0.00020 0.00020 0.00016 S1 -0.06856 -0.11714 -0.30521 1.00000 0.02500 0.03766 0.02622 0.00986 0.00636 0.00847 0.03125 0.00264 0.00010 0.00011 0.00010 0.00000 0.00054 0.00061 0.00059 0.00052 0.00044 0.00047 0.00026 O1 -0.20298 -0.18385 -0.31133 1.00000 0.02117 0.04756 0.03444 0.00948 0.00553 0.00409 0.03828 0.00719 0.00028 0.00030 0.00027 0.00000 0.00149 0.00187 0.00179 0.00160 0.00129 0.00139 0.00072 O2 -0.06605 -0.02523 -0.35285 1.00000 0.04123 0.04156 0.03547 0.01764 0.01179 0.01831 0.03833 0.00751 0.00031 0.00029 0.00026 0.00000 0.00177 0.00179 0.00181 0.00157 0.00141 0.00151 0.00073 N1 0.27999 -0.49171 -0.53506 1.00000 0.04734 0.03830 0.04266 0.02458 0.02586 0.02258 0.03739 0.01023 0.00039 0.00037 0.00038 0.00000 0.00236 0.00222 0.00249 0.00211 0.00197 0.00191 0.00092 N2 0.00518 -0.04555 -0.16214 1.00000 0.02446 0.04583 0.02622 0.01148 0.01249 0.00423 0.03340 0.00983 0.00040 0.00041 0.00036 0.00000 0.00207 0.00241 0.00217 0.00196 0.00173 0.00175 0.00092 N3 0.17835 0.06128 0.01134 1.00000 0.02275 0.03991 0.02681 0.01312 0.00586 0.00356 0.03088 0.00847 0.00033 0.00034 0.00031 0.00000 0.00180 0.00208 0.00203 0.00180 0.00149 0.00158 0.00079 C1 0.19422 -0.41066 -0.48638 1.00000 0.02575 0.02679 0.03080 0.01084 0.00902 0.00087 0.02871 0.00995 0.00040 0.00038 0.00038 0.00000 0.00216 0.00219 0.00247 0.00205 0.00182 0.00182 0.00092 C2 0.15227 -0.40323 -0.38326 1.00000 0.02630 0.03205 0.03081 0.01765 0.00539 0.00495 0.02880 0.01014 0.00041 0.00041 0.00038 0.00000 0.00218 0.00231 0.00243 0.00215 0.00183 0.00188 0.00093 C3 0.07204 -0.31555 -0.32900 1.00000 0.02422 0.03735 0.02495 0.01301 0.00711 0.00175 0.02950 0.01023 0.00041 0.00041 0.00039 0.00000 0.00213 0.00247 0.00234 0.00213 0.00181 0.00186 0.00092 C4 0.03133 -0.23027 -0.37429 1.00000 0.02252 0.02793 0.02342 0.00788 0.00220 0.00201 0.02679 0.00960 0.00039 0.00039 0.00035 0.00000 0.00202 0.00215 0.00220 0.00192 0.00167 0.00173 0.00087 C5 0.06888 -0.23777 -0.47739 1.00000 0.02562 0.02556 0.02525 0.00925 0.00321 0.00139 0.02708 0.00963 0.00040 0.00039 0.00036 0.00000 0.00215 0.00217 0.00231 0.00200 0.00175 0.00179 0.00090 C6 0.14701 -0.32771 -0.53299 1.00000 0.02940 0.03374 0.02413 0.01254 0.00834 0.00244 0.02941 0.01025 0.00042 0.00041 0.00038 0.00000 0.00223 0.00236 0.00232 0.00208 0.00184 0.00190 0.00092 C7 0.14252 0.02316 -0.10583 1.00000 0.02110 0.02884 0.03000 0.01045 0.00633 0.00795 0.02756 0.01014 0.00040 0.00039 0.00038 0.00000 0.00202 0.00219 0.00238 0.00200 0.00172 0.00175 0.00088 C8 0.23353 0.04791 -0.16802 1.00000 0.03249 0.03853 0.02453 0.01143 0.01086 0.00370 0.03271 0.01104 0.00044 0.00043 0.00040 0.00000 0.00242 0.00254 0.00253 0.00220 0.00193 0.00201 0.00097 C9 0.36828 0.10957 -0.10673 1.00000 0.03061 0.03381 0.03647 0.01431 0.01539 0.00279 0.03359 0.01100 0.00044 0.00042 0.00041 0.00000 0.00242 0.00244 0.00268 0.00224 0.00205 0.00200 0.00099 C10 0.40867 0.14566 0.01532 1.00000 0.02541 0.02546 0.04054 0.01412 0.00894 0.00309 0.03089 0.01030 0.00041 0.00039 0.00039 0.00000 0.00215 0.00214 0.00274 0.00213 0.00191 0.00177 0.00095 C11 0.31085 0.12319 0.07187 1.00000 0.03211 0.03501 0.02629 0.01235 0.00433 0.00322 0.03243 0.01083 0.00044 0.00042 0.00041 0.00000 0.00241 0.00242 0.00243 0.00212 0.00189 0.00196 0.00096 H1A 0.30711 -0.55053 -0.50805 1.00000 0.05039 0.11751 0.00483 0.00472 0.00445 0.00000 0.01361 H1B 0.28901 -0.50443 -0.60961 1.00000 0.04948 0.12087 0.00486 0.00465 0.00476 0.00000 0.01423 H2A -0.03239 -0.05395 -0.12859 1.00000 0.02252 0.11489 0.00478 0.00446 0.00411 0.00000 0.01392 H2 0.18643 -0.45287 -0.35063 1.00000 0.02794 0.09685 0.00403 0.00388 0.00360 0.00000 0.01069 H3 0.04399 -0.31374 -0.26342 1.00000 0.01974 0.09089 0.00372 0.00353 0.00350 0.00000 0.00957 H5 0.04423 -0.18399 -0.50855 1.00000 0.01777 0.08736 0.00364 0.00353 0.00320 0.00000 0.00951 H6 0.17671 -0.33617 -0.60351 1.00000 0.03161 0.10227 0.00419 0.00393 0.00387 0.00000 0.01076 H8 0.20798 0.01916 -0.25147 1.00000 0.02056 0.09646 0.00376 0.00364 0.00370 0.00000 0.00980 H9 0.43622 0.13381 -0.14356 1.00000 0.05776 0.12340 0.00522 0.00477 0.00453 0.00000 0.01449 H11 0.33319 0.14752 0.16088 1.00000 0.03709 0.10949 0.00424 0.00409 0.00419 0.00000 0.01163 Br21 0.92850 0.29196 -0.00636 1.00000 0.02883 0.05008 0.04113 0.02051 0.01330 0.00326 0.03987 0.00115 0.00004 0.00005 0.00004 0.00000 0.00025 0.00031 0.00030 0.00025 0.00020 0.00021 0.00016 S21 1.46049 0.37314 -0.29748 1.00000 0.03103 0.03450 0.02555 0.01541 0.01028 0.00686 0.02926 0.00265 0.00011 0.00010 0.00009 0.00000 0.00056 0.00059 0.00058 0.00051 0.00044 0.00046 0.00025 O21 1.59462 0.44828 -0.27825 1.00000 0.03366 0.03950 0.03355 0.01788 0.01409 0.00082 0.03482 0.00721 0.00029 0.00029 0.00026 0.00000 0.00164 0.00171 0.00176 0.00154 0.00136 0.00138 0.00069 O22 1.34572 0.36599 -0.38743 1.00000 0.03666 0.04214 0.02739 0.01835 0.00673 0.01140 0.03438 0.00716 0.00029 0.00028 0.00025 0.00000 0.00168 0.00176 0.00164 0.00151 0.00131 0.00143 0.00069 N21 1.50863 -0.16324 -0.37987 1.00000 0.02651 0.03678 0.04250 0.01737 0.00947 0.00697 0.03538 0.01099 0.00045 0.00040 0.00037 0.00000 0.00216 0.00233 0.00252 0.00212 0.00186 0.00197 0.00089 N22 1.42247 0.44188 -0.16675 1.00000 0.02190 0.03525 0.02584 0.01202 0.00460 -0.00081 0.02908 0.00955 0.00037 0.00036 0.00034 0.00000 0.00190 0.00209 0.00206 0.00184 0.00168 0.00166 0.00079 N23 1.31789 0.43243 -0.02128 1.00000 0.02681 0.03324 0.02681 0.01275 0.00727 0.00364 0.02942 0.00835 0.00033 0.00033 0.00031 0.00000 0.00183 0.00194 0.00199 0.00173 0.00150 0.00155 0.00077 C21 1.49997 -0.03899 -0.36351 1.00000 0.02514 0.03663 0.02865 0.01475 0.01642 0.00834 0.02870 0.01038 0.00040 0.00040 0.00037 0.00000 0.00213 0.00243 0.00235 0.00211 0.00179 0.00189 0.00092 C22 1.61085 0.06581 -0.29119 1.00000 0.02066 0.03923 0.02390 0.01209 0.00664 0.00522 0.02872 0.01028 0.00041 0.00042 0.00037 0.00000 0.00213 0.00252 0.00227 0.00209 0.00174 0.00189 0.00092 C23 1.59904 0.19109 -0.27212 1.00000 0.02126 0.03655 0.02479 0.00995 0.00828 0.00096 0.02908 0.01112 0.00042 0.00044 0.00038 0.00000 0.00216 0.00254 0.00235 0.00216 0.00182 0.00202 0.00092 C24 1.47650 0.21396 -0.32652 1.00000 0.02927 0.03062 0.02069 0.00962 0.00920 0.00865 0.02703 0.00986 0.00040 0.00039 0.00035 0.00000 0.00218 0.00226 0.00214 0.00195 0.00175 0.00188 0.00089 C25 1.36675 0.10988 -0.40119 1.00000 0.02375 0.03681 0.02338 0.01281 0.00932 0.00756 0.02775 0.01026 0.00041 0.00041 0.00036 0.00000 0.00212 0.00244 0.00224 0.00209 0.00177 0.00188 0.00090 C26 1.37759 -0.01528 -0.41902 1.00000 0.02111 0.03395 0.02519 0.00965 0.00699 0.00160 0.02833 0.01068 0.00042 0.00042 0.00038 0.00000 0.00210 0.00245 0.00235 0.00212 0.00177 0.00192 0.00091 C27 1.30169 0.40124 -0.13820 1.00000 0.03093 0.02964 0.03112 0.01671 0.00991 0.01036 0.02888 0.01041 0.00042 0.00039 0.00038 0.00000 0.00227 0.00223 0.00247 0.00209 0.00186 0.00186 0.00092 C28 1.17455 0.33520 -0.22335 1.00000 0.02969 0.04180 0.02869 0.01461 0.00635 0.00296 0.03441 0.01115 0.00044 0.00044 0.00043 0.00000 0.00237 0.00266 0.00257 0.00231 0.00194 0.00202 0.00101 C29 1.06290 0.30161 -0.18488 1.00000 0.03380 0.03254 0.02757 0.01069 0.00243 0.00612 0.03321 0.01129 0.00047 0.00043 0.00040 0.00000 0.00252 0.00242 0.00247 0.00215 0.00201 0.00206 0.00098 C210 1.07965 0.33454 -0.06447 1.00000 0.02575 0.03311 0.03849 0.01630 0.00972 0.00357 0.03241 0.01077 0.00042 0.00041 0.00040 0.00000 0.00221 0.00235 0.00268 0.00223 0.00194 0.00189 0.00097 C211 1.20729 0.40070 0.01501 1.00000 0.02876 0.03482 0.02996 0.01342 0.01097 0.00608 0.03122 0.01091 0.00042 0.00042 0.00041 0.00000 0.00231 0.00239 0.00246 0.00216 0.00188 0.00193 0.00095 H21A 1.58930 -0.18163 -0.36593 1.00000 0.02631 0.10153 0.00453 0.00391 0.00365 0.00000 0.01106 H21B 1.44268 -0.22496 -0.42323 1.00000 0.03651 0.12212 0.00500 0.00458 0.00430 0.00000 0.01367 H22A 1.48643 0.47889 -0.11280 1.00000 0.01762 0.10445 0.00425 0.00397 0.00373 0.00000 0.01124 H22 1.69748 0.05771 -0.25017 1.00000 0.02465 0.09616 0.00416 0.00359 0.00347 0.00000 0.00999 H23 1.66866 0.25854 -0.22709 1.00000 0.01305 0.09775 0.00399 0.00367 0.00333 0.00000 0.00901 H25 1.27938 0.12186 -0.44370 1.00000 0.03500 0.10520 0.00446 0.00401 0.00383 0.00000 0.01106 H26 1.30631 -0.08728 -0.47197 1.00000 0.03119 0.10942 0.00431 0.00422 0.00384 0.00000 0.01120 H28 1.17776 0.32448 -0.29852 1.00000 0.04795 0.12100 0.00478 0.00464 0.00465 0.00000 0.01374 H29 0.97500 0.25022 -0.24119 1.00000 0.04049 0.11729 0.00479 0.00443 0.00409 0.00000 0.01230 H211 1.23239 0.43104 0.11270 1.00000 0.02271 0.09330 0.00367 0.00354 0.00357 0.00000 0.00965 Final Structure Factor Calculation for s92 in P-1 Total number of l.s. parameters = 405 Maximum vector length = 511 Memory required = 3223 / 25039 wR2 = 0.1050 before cycle 5 for 4468 data and 0 / 405 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0497 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0416 for 3325 Fo > 4sig(Fo) and 0.0665 for all 4468 data wR2 = 0.1050, GooF = S = 1.033, Restrained GooF = 1.033 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 0.0555 0.0459 0.0235 Br1 0.0441 0.0260 0.0236 S1 0.0606 0.0331 0.0212 O1 0.0512 0.0352 0.0286 O2 0.0593 0.0293 0.0236 N1 0.0534 0.0301 0.0168 N2 0.0432 0.0268 0.0226 N3 0.0367 0.0278 0.0215 C1 0.0346 0.0268 0.0250 C2 0.0412 0.0255 0.0218 C3 0.0336 0.0270 0.0198 C4 0.0303 0.0293 0.0217 C5 0.0380 0.0281 0.0220 C6 0.0359 0.0276 0.0192 C7 0.0448 0.0319 0.0214 C8 0.0455 0.0335 0.0218 C9 0.0422 0.0277 0.0227 C10 0.0384 0.0332 0.0257 C11 0.0536 0.0419 0.0241 Br21 0.0345 0.0318 0.0215 S21 0.0470 0.0366 0.0209 O21 0.0440 0.0350 0.0242 O22 0.0436 0.0367 0.0258 N21 0.0407 0.0262 0.0203 N22 0.0356 0.0273 0.0253 N23 0.0375 0.0350 0.0136 C21 0.0423 0.0240 0.0198 C22 0.0439 0.0251 0.0183 C23 0.0339 0.0287 0.0185 C24 0.0384 0.0261 0.0188 C25 0.0403 0.0249 0.0198 C26 0.0347 0.0281 0.0238 C27 0.0454 0.0294 0.0284 C28 0.0405 0.0334 0.0257 C29 0.0392 0.0342 0.0238 C210 0.0373 0.0321 0.0242 C211 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.019 0.030 0.040 0.052 0.066 0.084 0.109 0.152 1.000 Number in group 501. 418. 453. 424. 460. 439. 449. 438. 439. 447. GooF 0.909 0.910 1.066 1.154 1.100 1.099 0.984 0.982 1.002 1.102 K 1.289 1.004 0.934 0.932 0.976 0.971 0.995 1.014 1.030 0.985 Resolution(A) 0.84 0.87 0.90 0.95 0.99 1.06 1.14 1.26 1.43 1.81 inf Number in group 454. 441. 448. 445. 456. 438. 455. 435. 450. 446. GooF 0.992 0.996 0.995 1.030 1.001 0.979 0.994 0.966 1.012 1.318 K 0.980 0.971 0.979 0.998 1.026 1.040 1.045 1.036 1.019 0.950 R1 0.178 0.141 0.117 0.087 0.069 0.059 0.044 0.036 0.034 0.035 Recommended weighting scheme: WGHT 0.0497 0.0000 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 2 -11 4 78.12 152.22 3.88 0.040 1.04 -1 1 0 221.52 170.89 3.84 0.042 7.78 2 -5 3 705.35 885.84 3.80 0.096 2.12 3 -6 12 30.50 127.18 3.80 0.036 0.95 -2 4 0 176.10 125.18 3.76 0.036 2.46 6 -10 10 48.17 274.75 3.67 0.053 0.85 -6 -5 13 156.24 280.18 3.64 0.054 0.90 -5 -4 5 311.34 210.30 3.50 0.047 1.52 3 -3 2 329.92 246.20 3.49 0.051 2.50 -2 -2 1 123.72 77.55 3.45 0.028 3.52 -10 0 1 88.63 188.81 3.38 0.044 0.98 1 -8 14 145.75 266.74 3.36 0.053 0.86 -2 2 0 50.15 5.15 3.25 0.007 3.89 -4 -10 4 13.58 71.98 3.18 0.027 0.99 3 -9 11 214.13 311.17 3.11 0.057 0.95 4 9 2 134.76 286.26 3.10 0.054 0.87 -1 4 1 61.84 122.63 3.06 0.036 2.32 0 -4 2 252.91 308.30 2.96 0.057 2.87 -1 -9 9 999.98 832.95 2.94 0.093 1.13 0 -4 6 27.95 5.07 2.92 0.007 2.00 3 -3 1 696.98 826.54 2.92 0.093 2.62 1 -3 1 81252.89 96508.48 2.91 1.000 3.68 2 -3 5 88.16 56.28 2.89 0.024 2.07 -1 7 2 127.13 61.11 2.88 0.025 1.30 -11 4 3 96.80 200.48 2.84 0.046 0.87 -1 -9 10 2172.39 1827.02 2.82 0.138 1.08 3 -11 1 530.06 664.35 2.82 0.083 0.97 -7 1 12 -23.54 116.38 2.81 0.035 0.85 3 -7 12 81.65 27.94 2.81 0.017 0.94 -8 3 0 94.56 147.60 2.81 0.039 1.21 -9 -2 9 446.17 330.65 2.80 0.059 0.94 -1 4 6 751.88 571.06 2.80 0.077 1.28 9 -1 3 187.70 269.04 2.80 0.053 0.99 -5 8 1 75.54 147.16 2.79 0.039 1.13 -10 -3 4 146.45 241.32 2.77 0.050 0.94 1 -5 1 1098.83 1288.65 2.76 0.116 2.21 7 -1 4 119.56 61.64 2.75 0.025 1.16 9 -5 5 69.36 125.51 2.73 0.036 0.93 2 -8 6 778.84 645.56 2.72 0.082 1.35 -1 2 1 204.64 152.09 2.72 0.040 4.04 -3 -6 14 184.40 318.50 2.69 0.057 0.90 -4 -3 4 566.81 684.57 2.69 0.084 1.93 5 -12 2 116.87 186.23 2.69 0.044 0.88 1 -5 3 1061.12 1234.21 2.67 0.113 2.26 4 7 2 65.94 141.23 2.66 0.038 1.03 4 -10 2 90.06 137.53 2.66 0.038 1.06 1 -11 13 232.07 425.23 2.65 0.066 0.85 -4 2 0 4591.66 5309.81 2.65 0.235 2.35 -7 8 5 87.25 185.75 2.63 0.044 0.88 1 -1 1 105.70 76.57 2.60 0.028 6.89 Bond lengths and angles Br1 - Distance Angles C10 1.8888 (0.0042) Br1 - S1 - Distance Angles O2 1.4306 (0.0028) O1 1.4469 (0.0030) 117.96 (0.17) N2 1.6229 (0.0042) 111.04 (0.20) 102.85 (0.20) C4 1.7369 (0.0040) 107.66 (0.18) 110.43 (0.18) 106.30 (0.19) S1 - O2 O1 N2 O1 - Distance Angles S1 1.4469 (0.0030) O1 - O2 - Distance Angles S1 1.4306 (0.0028) O2 - N1 - Distance Angles C1 1.3483 (0.0053) N1 - N2 - Distance Angles C7 1.3988 (0.0055) S1 1.6229 (0.0042) 127.42 (0.33) N2 - C7 N3 - Distance Angles C7 1.3232 (0.0053) C11 1.3489 (0.0053) 118.30 (0.35) N3 - C7 C1 - Distance Angles N1 1.3483 (0.0053) C6 1.4020 (0.0053) 121.71 (0.38) C2 1.4135 (0.0056) 120.82 (0.35) 117.44 (0.36) C1 - N1 C6 C2 - Distance Angles C3 1.3694 (0.0058) C1 1.4135 (0.0056) 121.18 (0.36) C2 - C3 C3 - Distance Angles C2 1.3694 (0.0058) C4 1.3956 (0.0054) 120.19 (0.38) C3 - C2 C4 - Distance Angles C5 1.3933 (0.0055) C3 1.3956 (0.0054) 119.63 (0.37) S1 1.7369 (0.0040) 119.68 (0.28) 120.68 (0.31) C4 - C5 C3 C5 - Distance Angles C6 1.3740 (0.0057) C4 1.3933 (0.0055) 119.97 (0.35) C5 - C6 C6 - Distance Angles C5 1.3740 (0.0057) C1 1.4020 (0.0053) 121.51 (0.38) C6 - C5 C7 - Distance Angles N3 1.3232 (0.0053) C8 1.3855 (0.0056) 122.96 (0.39) N2 1.3988 (0.0055) 114.36 (0.36) 122.67 (0.40) C7 - N3 C8 C8 - Distance Angles C9 1.3684 (0.0060) C7 1.3855 (0.0056) 118.62 (0.41) C8 - C9 C9 - Distance Angles C8 1.3684 (0.0060) C10 1.3881 (0.0059) 118.97 (0.39) C9 - C8 C10 - Distance Angles C11 1.3731 (0.0059) C9 1.3881 (0.0059) 118.99 (0.39) Br1 1.8888 (0.0042) 119.21 (0.33) 121.80 (0.31) C10 - C11 C9 C11 - Distance Angles N3 1.3489 (0.0053) C10 1.3731 (0.0059) 122.04 (0.40) C11 - N3 Br21 - Distance Angles C210 1.8978 (0.0041) Br21 - S21 - Distance Angles O22 1.4334 (0.0029) O21 1.4367 (0.0029) 119.33 (0.16) N22 1.6320 (0.0038) 108.41 (0.18) 103.88 (0.19) C24 1.7371 (0.0039) 108.13 (0.19) 109.47 (0.18) 106.95 (0.18) S21 - O22 O21 N22 O21 - Distance Angles S21 1.4367 (0.0029) O21 - O22 - Distance Angles S21 1.4334 (0.0029) O22 - N21 - Distance Angles C21 1.3688 (0.0053) N21 - N22 - Distance Angles C27 1.4078 (0.0052) S21 1.6320 (0.0038) 125.85 (0.32) N22 - C27 N23 - Distance Angles C211 1.3417 (0.0051) C27 1.3424 (0.0050) 118.43 (0.36) N23 - C211 C21 - Distance Angles N21 1.3688 (0.0053) C22 1.3930 (0.0058) 120.85 (0.37) C26 1.4072 (0.0054) 120.15 (0.40) 119.00 (0.36) C21 - N21 C22 C22 - Distance Angles C23 1.3773 (0.0058) C21 1.3930 (0.0058) 120.27 (0.37) C22 - C23 C23 - Distance Angles C22 1.3773 (0.0058) C24 1.3977 (0.0054) 120.33 (0.41) C23 - C22 C24 - Distance Angles C25 1.3869 (0.0057) C23 1.3977 (0.0054) 119.90 (0.36) S21 1.7371 (0.0039) 120.18 (0.29) 119.89 (0.33) C24 - C25 C23 C25 - Distance Angles C26 1.3782 (0.0056) C24 1.3869 (0.0057) 119.85 (0.36) C25 - C26 C26 - Distance Angles C25 1.3782 (0.0056) C21 1.4072 (0.0054) 120.62 (0.40) C26 - C25 C27 - Distance Angles N23 1.3424 (0.0050) C28 1.4014 (0.0060) 122.40 (0.38) N22 1.4078 (0.0052) 114.18 (0.36) 123.42 (0.39) C27 - N23 C28 C28 - Distance Angles C29 1.3749 (0.0062) C27 1.4014 (0.0060) 118.37 (0.43) C28 - C29 C29 - Distance Angles C28 1.3749 (0.0062) C210 1.3804 (0.0059) 119.10 (0.42) C29 - C28 C210 - Distance Angles C211 1.3797 (0.0060) C29 1.3804 (0.0059) 119.68 (0.40) Br21 1.8978 (0.0041) 119.50 (0.33) 120.81 (0.33) C210 - C211 C29 C211 - Distance Angles N23 1.3417 (0.0051) C210 1.3797 (0.0060) 122.00 (0.41) C211 - N23 FMAP and GRID set by program FMAP 2 3 33 GRID -1.667 -2 -2 1.667 2 2 R1 = 0.0636 for 4468 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.40 at 0.9280 0.2422 0.0812 [ 1.46 A from BR21 ] Deepest hole -0.72 at 0.0052 0.7222 0.0462 [ 0.88 A from BR21 ] Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 3016 / 25227 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9280 0.2422 0.0812 1.00000 0.05 0.40 1.46 BR21 2.05 H3 2.74 H2A 2.88 C3 Q2 1 0.8375 0.1892 -0.1033 1.00000 0.05 0.40 1.37 BR21 1.98 H22 2.52 H23 2.63 C210 Q3 1 1.3243 0.6266 -0.0217 1.00000 0.05 0.35 2.24 N23 2.33 C27 2.51 H22A 2.51 BR1 Q4 1 0.6475 0.3820 0.1942 1.00000 0.05 0.33 1.63 BR1 2.13 H2 2.35 N22 2.60 H22A Q5 1 0.2655 -0.3392 -0.2155 1.00000 0.05 0.32 1.63 H2 1.73 BR1 2.00 C2 2.26 H3 Q6 1 0.8346 0.1932 0.0078 1.00000 0.05 0.32 1.49 BR21 2.82 N3 2.87 BR1 2.88 H3 Q7 1 0.1532 -0.4132 -0.2159 1.00000 0.05 0.32 1.67 H2 1.86 H3 2.18 C2 2.27 C3 Q8 1 1.0731 0.3767 0.0944 1.00000 0.05 0.31 1.58 H211 1.63 BR21 1.87 C210 1.87 C211 Q9 1 0.2577 -0.1156 0.0087 1.00000 0.05 0.31 2.25 N3 2.32 BR1 2.48 C11 2.60 BR21 Q10 1 1.8261 0.3648 -0.1481 1.00000 0.05 0.31 1.72 H23 2.23 H29 2.35 H211 2.41 BR21 Shortest distances between peaks (including symmetry equivalents) 4 5 1.09 1 6 1.09 6 9 1.14 5 7 1.34 2 6 1.40 4 7 1.93 1 8 1.94 1 9 2.03 2 9 2.05 1 2 2.14 3 4 2.22 1 7 2.31 2 10 2.33 3 7 2.56 3 5 2.63 3 6 2.69 6 8 2.72 6 7 2.73 1 5 2.79 8 10 2.79 3 10 2.80 5 6 2.86 2 3 2.87 7 8 2.91 5 9 2.92 2 8 2.95 3 9 2.98 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. 1.21: 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 8.23: Structure factors and derivatives 44.26: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 4.72: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.77: Analysis of variance 0.33: Merge reflections for Fourier and .fcf 0.22: Fourier summations 0.28: Peaksearch 0.05: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 11:09:06 Total elapsed time: 60.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++