+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 14:48:21 on 04-Dec-2000 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P-1 CELL 0.71073 8.8031 9.6811 10.8622 83.989 71.839 78.348 ZERR 2.00 0.0018 0.0019 0.0022 0.030 0.030 0.030 LATT 1 SFAC C H N O S UNIT 32 40 6 8 2 V = 860.61 F(000) = 370.0 Mu = 0.21 mm-1 Cell Wt = 700.82 Rho = 1.352 MERG 2 FMAP 2 ACTA PLAN 25 L.S. 1 WGHT 0.080500 0.301300 FVAR 0.91543 S11 5 0.266712 0.258087 0.690964 11.00000 0.02382 0.02767 = 0.03007 0.00107 -0.00672 -0.00193 O11 4 0.210442 0.328679 0.586453 11.00000 0.02884 0.03292 = 0.03766 0.00398 -0.01418 -0.00056 O12 4 0.155896 0.259411 0.819277 11.00000 0.02682 0.03906 = 0.03328 -0.00095 -0.00183 -0.00305 O32 4 0.177708 0.545446 0.009287 11.00000 0.02781 0.04570 = 0.03615 -0.00449 -0.01170 -0.00371 N12 3 0.331051 0.093916 0.646875 11.00000 0.03233 0.02707 = 0.02546 0.00209 -0.00903 -0.00525 O31 4 0.035561 0.617240 -0.133045 11.00000 0.04194 0.04091 = 0.05229 0.01531 -0.02511 -0.01529 N11 3 0.850713 0.460509 0.701747 11.00000 0.03014 0.04048 = 0.03939 0.00195 -0.01388 -0.00598 C35 1 0.065593 0.544891 -0.030570 11.00000 0.03022 0.02902 = 0.03254 -0.00544 -0.01236 0.00050 C12 1 0.696032 0.384047 0.582388 11.00000 0.02958 0.03447 = 0.02754 0.00273 -0.00335 -0.00708 C17 1 0.413202 -0.010449 0.716179 11.00000 0.03386 0.02395 = 0.03035 0.00286 -0.01353 -0.00829 C16 1 0.591817 0.394143 0.814789 11.00000 0.03357 0.03091 = 0.03016 -0.00294 -0.01252 -0.00118 C13 1 0.558515 0.339314 0.579342 11.00000 0.03491 0.03267 = 0.02607 0.00102 -0.00765 -0.00666 C14 1 0.437384 0.320437 0.694604 11.00000 0.02637 0.02184 = 0.03043 0.00092 -0.00838 -0.00118 C15 1 0.455131 0.347323 0.812054 11.00000 0.02822 0.02751 = 0.02819 -0.00117 -0.00564 0.00152 C11 1 0.715153 0.412117 0.700071 11.00000 0.02714 0.02070 = 0.03730 0.00275 -0.01271 0.00085 C34 1 0.157852 0.702491 -0.208721 11.00000 0.04171 0.04494 = 0.06146 0.01476 -0.01562 -0.01359 C32 1 -0.045271 0.928724 -0.202743 11.00000 0.05657 0.03716 = 0.07262 -0.00363 -0.00078 -0.00718 C33 1 0.075309 0.815283 -0.284452 11.00000 0.04527 0.04023 = 0.04677 0.00557 -0.01182 -0.00738 C31 1 -0.121798 1.040949 -0.286552 11.00000 0.05791 0.04488 = 0.16362 0.03483 -0.01923 -0.00009 N13 3 0.527719 -0.104595 0.640836 11.00000 0.03770 0.02628 = 0.02992 0.00224 -0.01455 -0.00380 C18 1 0.606888 -0.211384 0.700526 11.00000 0.04845 0.02822 = 0.03573 0.00197 -0.01802 -0.00063 C19 1 0.578174 -0.225162 0.832360 11.00000 0.05991 0.02824 = 0.03950 0.00559 -0.02624 -0.00456 C21 1 0.374765 -0.017247 0.850139 11.00000 0.04657 0.03090 = 0.02924 0.00145 -0.01075 -0.00571 C20 1 0.460113 -0.126748 0.908242 11.00000 0.06263 0.03281 = 0.02933 0.00573 -0.01845 -0.01011 H12 2 0.777531 0.396177 0.505234 11.00000 0.03879 H13 2 0.548795 0.319467 0.496662 11.00000 0.03278 H18 2 0.691513 -0.275711 0.645469 11.00000 0.04755 H17 2 0.373665 0.090866 0.564763 11.00000 0.03023 H16 2 0.606540 0.411627 0.894017 11.00000 0.03248 H10 2 0.858292 0.463495 0.779560 11.00000 0.04381 H33A 2 0.012918 0.779093 -0.339706 11.00000 0.06329 H20 2 0.431024 -0.132673 0.999562 11.00000 0.04078 H15 2 0.372452 0.335802 0.891141 11.00000 0.03585 H21 2 0.286554 0.053129 0.898484 11.00000 0.03877 H19 2 0.637777 -0.304177 0.866422 11.00000 0.04886 H32B 2 0.010667 0.961757 -0.143115 11.00000 0.05431 H11 2 0.935221 0.442236 0.636543 11.00000 0.04962 H34A 2 0.167764 0.756262 -0.131135 11.00000 0.06358 H34B 2 0.262240 0.637811 -0.268879 11.00000 0.07057 H33B 2 0.166516 0.865050 -0.353854 11.00000 0.05546 H32A 2 -0.125253 0.883709 -0.137439 11.00000 0.06909 H31C 2 -0.034631 1.081442 -0.353546 11.00000 0.08336 H31B 2 -0.183828 1.005533 -0.325480 11.00000 0.14145 H31A 2 -0.197905 1.105810 -0.240210 11.00000 0.17054 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 S11 - O12 O11 N12 C14 O11 - S11 O12 - S11 O32 - C35 N12 - C17 S11 O31 - C35 C34 N11 - C11 C35 - O32 O31 C35_$1 C12 - C13 C11 C17 - N13 C21 N12 C16 - C15 C11 C13 - C12 C14 C14 - C15 C13 S11 C15 - C16 C14 C11 - N11 C16 C12 C34 - O31 C33 C32 - C33 C31 C33 - C34 C32 C31 - C32 N13 - C17 C18 C18 - N13 C19 C19 - C18 C20 C21 - C17 C20 C20 - C19 C21 Operators for generating equivalent atoms: $1 -x, -y+1, -z 12927 Reflections read, of which 0 rejected -11 =< h =< 11, -12 =< k =< 12, -14 =< l =< 14, Max. 2-theta = 54.83 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 2 0 0 37.38 0.24 6 6.19 3 0 0 166.89 0.26 6 77.17 3 -2 1 6.47 0.27 4 1.37 -3 1 1 26.95 0.26 4 8.04 1 2 1 4.18 0.49 3 2.54 -5 1 2 131.75 3.15 3 40.43 6 0 3 82.17 0.50 6 14.08 6 -3 4 208.97 1.19 4 89.11 6 -2 4 268.11 4.68 2 186.31 7 -3 5 156.49 3.49 4 37.51 10 Inconsistent equivalents 3860 Unique reflections, of which 0 suppressed R(int) = 0.0571 R(sigma) = 0.0490 Friedel opposites merged Maximum memory for data reduction = 2103 / 38903 Least-squares cycle 1 Maximum vector length = 511 Memory required = 2808 / 372398 wR2 = 0.1335 before cycle 1 for 3860 data and 297 / 297 parameters GooF = S = 0.958; Restrained GooF = 0.958 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0805 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.91543 0.00232 0.001 OSF Mean shift/esd = 0.002 Maximum = -0.019 for U13 S11 Max. shift = 0.000 A for H31B Max. dU = 0.000 for H32A Largest correlation matrix elements 0.526 U33 S11 / OSF 0.515 U11 S11 / OSF s92 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S11 0.26671 0.25809 0.69096 1.00000 0.02382 0.02767 0.03007 0.00107 -0.00672 -0.00193 0.02807 0.00065 0.00005 0.00005 0.00004 0.00000 0.00025 0.00025 0.00027 0.00018 0.00018 0.00017 0.00016 O11 0.21044 0.32868 0.58645 1.00000 0.02884 0.03292 0.03766 0.00398 -0.01418 -0.00056 0.03329 0.00194 0.00015 0.00014 0.00013 0.00000 0.00068 0.00069 0.00075 0.00056 0.00056 0.00053 0.00032 O12 0.15590 0.25941 0.81928 1.00000 0.02682 0.03906 0.03328 -0.00095 -0.00183 -0.00305 0.03519 0.00203 0.00015 0.00014 0.00013 0.00000 0.00069 0.00076 0.00075 0.00057 0.00055 0.00055 0.00033 O32 0.17771 0.54545 0.00929 1.00000 0.02781 0.04570 0.03615 -0.00449 -0.01170 -0.00371 0.03627 0.00195 0.00015 0.00015 0.00013 0.00000 0.00070 0.00081 0.00077 0.00061 0.00057 0.00057 0.00033 N12 0.33105 0.09392 0.64687 1.00000 0.03233 0.02707 0.02546 0.00209 -0.00903 -0.00525 0.02845 0.00225 0.00019 0.00015 0.00016 0.00000 0.00083 0.00078 0.00084 0.00062 0.00064 0.00062 0.00034 O31 0.03556 0.61724 -0.13304 1.00000 0.04194 0.04091 0.05229 0.01531 -0.02511 -0.01529 0.04261 0.00211 0.00017 0.00015 0.00015 0.00000 0.00083 0.00081 0.00090 0.00066 0.00070 0.00064 0.00037 N11 0.85071 0.46051 0.70175 1.00000 0.03014 0.04048 0.03939 0.00195 -0.01388 -0.00598 0.03618 0.00268 0.00021 0.00019 0.00020 0.00000 0.00092 0.00096 0.00105 0.00078 0.00079 0.00072 0.00040 C35 0.06559 0.54489 -0.03057 1.00000 0.03022 0.02902 0.03254 -0.00544 -0.01236 0.00050 0.03044 0.00264 0.00022 0.00019 0.00018 0.00000 0.00096 0.00091 0.00097 0.00075 0.00078 0.00072 0.00041 C12 0.69603 0.38405 0.58239 1.00000 0.02958 0.03447 0.02754 0.00273 -0.00335 -0.00708 0.03185 0.00287 0.00023 0.00020 0.00018 0.00000 0.00097 0.00098 0.00096 0.00076 0.00075 0.00076 0.00041 C17 0.41320 -0.01045 0.71618 1.00000 0.03386 0.02395 0.03035 0.00286 -0.01353 -0.00829 0.02831 0.00253 0.00022 0.00018 0.00018 0.00000 0.00097 0.00085 0.00095 0.00070 0.00076 0.00071 0.00039 C16 0.59182 0.39414 0.81479 1.00000 0.03357 0.03091 0.03016 -0.00294 -0.01252 -0.00118 0.03140 0.00286 0.00023 0.00020 0.00019 0.00000 0.00102 0.00094 0.00100 0.00077 0.00079 0.00075 0.00041 C13 0.55852 0.33931 0.57934 1.00000 0.03491 0.03267 0.02607 0.00102 -0.00765 -0.00666 0.03164 0.00286 0.00023 0.00020 0.00018 0.00000 0.00102 0.00096 0.00096 0.00075 0.00076 0.00077 0.00041 C14 0.43738 0.32044 0.69460 1.00000 0.02637 0.02184 0.03043 0.00092 -0.00838 -0.00118 0.02685 0.00259 0.00021 0.00018 0.00017 0.00000 0.00088 0.00081 0.00095 0.00068 0.00071 0.00065 0.00038 C15 0.45513 0.34732 0.81205 1.00000 0.02822 0.02751 0.02819 -0.00117 -0.00564 0.00152 0.02959 0.00279 0.00022 0.00019 0.00018 0.00000 0.00094 0.00089 0.00095 0.00072 0.00075 0.00070 0.00039 C11 0.71515 0.41212 0.70007 1.00000 0.02714 0.02070 0.03730 0.00275 -0.01271 0.00085 0.02871 0.00268 0.00021 0.00018 0.00018 0.00000 0.00090 0.00081 0.00101 0.00071 0.00075 0.00066 0.00039 C34 0.15785 0.70249 -0.20872 1.00000 0.04171 0.04494 0.06146 0.01476 -0.01562 -0.01359 0.04975 0.00396 0.00029 0.00026 0.00027 0.00000 0.00128 0.00131 0.00156 0.00115 0.00113 0.00103 0.00059 C32 -0.04527 0.92872 -0.20274 1.00000 0.05657 0.03716 0.07262 -0.00363 -0.00078 -0.00718 0.05987 0.00472 0.00035 0.00027 0.00030 0.00000 0.00158 0.00126 0.00185 0.00121 0.00137 0.00112 0.00071 C33 0.07531 0.81528 -0.28445 1.00000 0.04527 0.04023 0.04677 0.00557 -0.01182 -0.00738 0.04514 0.00368 0.00028 0.00024 0.00023 0.00000 0.00128 0.00116 0.00130 0.00098 0.00104 0.00096 0.00053 C31 -0.12180 1.04095 -0.28655 1.00000 0.05791 0.04488 0.16362 0.03483 -0.01923 -0.00009 0.09635 0.00873 0.00047 0.00038 0.00058 0.00000 0.00197 0.00167 0.00428 0.00215 0.00239 0.00146 0.00151 N13 0.52772 -0.10459 0.64084 1.00000 0.03770 0.02628 0.02992 0.00224 -0.01455 -0.00380 0.03080 0.00222 0.00019 0.00016 0.00015 0.00000 0.00088 0.00077 0.00083 0.00063 0.00068 0.00064 0.00036 C18 0.60689 -0.21138 0.70053 1.00000 0.04845 0.02822 0.03573 0.00197 -0.01802 -0.00063 0.03736 0.00310 0.00027 0.00021 0.00020 0.00000 0.00120 0.00097 0.00108 0.00081 0.00091 0.00085 0.00046 C19 0.57817 -0.22516 0.83236 1.00000 0.05991 0.02824 0.03950 0.00559 -0.02624 -0.00456 0.04090 0.00309 0.00028 0.00021 0.00021 0.00000 0.00139 0.00099 0.00118 0.00084 0.00103 0.00092 0.00050 C21 0.37477 -0.01725 0.85014 1.00000 0.04657 0.03090 0.02924 0.00145 -0.01075 -0.00571 0.03609 0.00300 0.00026 0.00021 0.00019 0.00000 0.00118 0.00099 0.00099 0.00079 0.00085 0.00086 0.00045 C20 0.46011 -0.12675 0.90824 1.00000 0.06263 0.03281 0.02933 0.00573 -0.01845 -0.01011 0.04079 0.00316 0.00029 0.00021 0.00021 0.00000 0.00140 0.00105 0.00108 0.00082 0.00098 0.00094 0.00049 H12 0.77753 0.39618 0.50523 1.00000 0.03879 0.03084 0.00262 0.00225 0.00209 0.00000 0.00573 H13 0.54879 0.31947 0.49666 1.00000 0.03278 0.03173 0.00240 0.00215 0.00207 0.00000 0.00527 H18 0.69151 -0.27571 0.64547 1.00000 0.04755 0.03419 0.00289 0.00254 0.00222 0.00000 0.00646 H17 0.37366 0.09087 0.56476 1.00000 0.03023 0.03031 0.00246 0.00215 0.00214 0.00000 0.00536 H16 0.60654 0.41163 0.89402 1.00000 0.03248 0.03128 0.00239 0.00214 0.00205 0.00000 0.00532 H10 0.85829 0.46349 0.77956 1.00000 0.04381 0.03643 0.00277 0.00245 0.00241 0.00000 0.00652 H33A 0.01292 0.77909 -0.33971 1.00000 0.06329 0.04118 0.00315 0.00282 0.00249 0.00000 0.00768 H20 0.43102 -0.13267 0.99956 1.00000 0.04078 0.03297 0.00265 0.00231 0.00229 0.00000 0.00586 H15 0.37245 0.33580 0.89114 1.00000 0.03585 0.03095 0.00261 0.00222 0.00210 0.00000 0.00547 H21 0.28655 0.05313 0.89848 1.00000 0.03877 0.03166 0.00268 0.00233 0.00211 0.00000 0.00569 H19 0.63778 -0.30418 0.86642 1.00000 0.04886 0.03454 0.00286 0.00256 0.00228 0.00000 0.00641 H32B 0.01067 0.96176 -0.14312 1.00000 0.05431 0.04042 0.00307 0.00277 0.00244 0.00000 0.00705 H11 0.93522 0.44224 0.63654 1.00000 0.04962 0.03566 0.00312 0.00256 0.00249 0.00000 0.00707 H34A 0.16776 0.75626 -0.13113 1.00000 0.06359 0.04225 0.00312 0.00288 0.00265 0.00000 0.00776 H34B 0.26224 0.63781 -0.26888 1.00000 0.07057 0.04129 0.00361 0.00303 0.00276 0.00000 0.00817 H33B 0.16652 0.86505 -0.35385 1.00000 0.05546 0.03582 0.00305 0.00262 0.00236 0.00000 0.00693 H32A -0.12525 0.88371 -0.13744 1.00000 0.06910 0.04224 0.00352 0.00305 0.00279 0.00000 0.00822 H31C -0.03463 1.08144 -0.35355 1.00000 0.08336 0.04687 0.00392 0.00349 0.00309 0.00000 0.00966 H31B -0.18384 1.00554 -0.32547 1.00000 0.14145 0.07576 0.00597 0.00521 0.00464 0.00000 0.01924 H31A -0.19790 1.10581 -0.24021 1.00000 0.17054 0.08068 0.00671 0.00588 0.00513 0.00000 0.02186 Final Structure Factor Calculation for s92 in P-1 Total number of l.s. parameters = 297 Maximum vector length = 511 Memory required = 2511 / 24017 wR2 = 0.1335 before cycle 2 for 3860 data and 0 / 297 parameters GooF = S = 0.958; Restrained GooF = 0.958 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0805 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0476 for 3055 Fo > 4sig(Fo) and 0.0644 for all 3860 data wR2 = 0.1335, GooF = S = 0.958, Restrained GooF = 0.958 for all data Occupancy sum of asymmetric unit = 24.00 for non-hydrogen and 20.00 for hydrogen atoms Principal mean square atomic displacements U 0.0345 0.0270 0.0228 S11 0.0423 0.0358 0.0217 O11 0.0448 0.0370 0.0238 O12 0.0472 0.0354 0.0263 O32 0.0326 0.0298 0.0229 N12 0.0672 0.0322 0.0284 O31 0.0440 0.0372 0.0274 N11 0.0387 0.0280 0.0247 C35 0.0391 0.0336 0.0229 C12 0.0365 0.0265 0.0220 C17 0.0384 0.0289 0.0269 C16 0.0360 0.0335 0.0254 C13 0.0323 0.0281 0.0201 C14 0.0385 0.0280 0.0222 C15 0.0385 0.0310 0.0166 C11 0.0739 0.0422 0.0331 C34 0.0936 0.0490 0.0371 C32 0.0549 0.0449 0.0356 C33 0.1949 0.0620 0.0321 C31 0.0390 0.0307 0.0227 N13 0.0517 0.0361 0.0243 C18 0.0628 0.0375 0.0224 C19 0.0480 0.0331 0.0271 C21 0.0627 0.0366 0.0231 C20 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.024 0.037 0.049 0.064 0.081 0.103 0.136 0.195 1.000 Number in group 397. 383. 395. 376. 402. 370. 385. 386. 378. 388. GooF 0.809 1.006 1.005 0.937 1.043 1.062 0.966 0.882 0.950 0.900 K 1.929 1.091 1.009 0.969 0.997 0.984 1.000 1.017 1.026 1.006 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.16 1.32 1.65 inf Number in group 402. 375. 384. 385. 385. 384. 386. 384. 389. 386. GooF 0.927 0.918 0.857 0.813 0.814 0.898 0.842 0.867 1.020 1.453 K 1.033 1.050 1.027 1.006 1.022 1.011 1.031 1.026 1.033 0.984 R1 0.161 0.137 0.108 0.079 0.061 0.054 0.041 0.037 0.042 0.048 Recommended weighting scheme: WGHT 0.0722 0.2045 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 -4 2 73.13 40.81 5.85 0.071 2.03 -3 1 2 269.70 176.11 5.30 0.147 2.06 -2 1 3 21.77 10.48 4.76 0.036 2.22 2 0 2 148.54 227.85 4.71 0.167 3.82 2 3 1 38.59 22.26 4.34 0.052 2.84 -3 6 8 7.25 21.21 3.98 0.051 0.86 2 2 5 356.44 257.94 3.90 0.178 2.04 0 1 6 25.73 41.97 3.79 0.072 1.70 -1 1 0 19.89 11.43 3.79 0.037 5.73 3 0 4 106.60 151.85 3.77 0.136 2.24 -1 1 4 126.87 90.83 3.75 0.106 2.21 3 0 6 12.32 5.35 3.69 0.026 1.70 -2 1 0 5.13 11.90 3.63 0.038 3.55 4 -2 2 5.21 1.39 3.57 0.013 1.82 1 4 4 31.46 47.86 3.46 0.077 1.88 4 1 0 33.38 21.74 3.45 0.052 2.09 0 -5 2 9.97 4.69 3.44 0.024 1.75 -2 -3 4 297.52 226.97 3.33 0.167 1.69 -3 -2 2 15.17 25.04 3.32 0.055 2.07 -1 0 2 48.33 33.77 3.31 0.064 3.88 6 5 13 6.24 22.34 3.27 0.052 0.78 -4 3 1 1.14 4.29 3.19 0.023 1.53 2 -3 2 271.10 209.49 3.14 0.160 2.23 -1 -2 1 200.19 262.94 3.13 0.180 3.82 2 0 0 44.61 20.86 3.11 0.051 4.11 2 2 3 1444.95 1857.09 3.11 0.477 2.86 -1 6 7 20.18 32.08 3.11 0.063 1.05 2 -4 4 5.66 1.99 3.03 0.016 1.62 -4 8 6 -2.43 5.79 3.02 0.027 0.80 -4 4 4 50.89 36.49 2.98 0.067 1.17 -2 10 5 108.04 70.08 2.97 0.093 0.81 1 6 2 12.46 21.08 2.97 0.051 1.58 -9 1 4 27.98 10.58 2.97 0.036 0.78 -2 2 5 50.05 68.35 2.88 0.092 1.55 -4 4 9 54.78 35.90 2.87 0.066 0.82 3 -1 6 71.64 53.78 2.87 0.081 1.63 -4 9 3 9.51 0.36 2.86 0.007 0.83 -5 6 2 -0.29 3.10 2.85 0.020 1.00 6 -8 4 5.92 0.10 2.85 0.004 0.82 1 -1 4 3.27 0.70 2.78 0.009 2.53 4 7 10 18.47 5.50 2.75 0.026 0.89 -2 -4 2 211.90 168.35 2.74 0.144 1.91 11 0 6 -5.20 11.49 2.73 0.038 0.78 -5 -1 2 32.03 44.28 2.71 0.074 1.46 3 -7 10 6.96 18.11 2.71 0.047 0.80 2 1 2 658.42 819.87 2.71 0.317 3.82 4 -4 1 28.38 40.85 2.70 0.071 1.45 -3 2 1 15.41 9.75 2.69 0.035 2.07 -1 2 6 14.73 8.40 2.69 0.032 1.51 1 0 2 121.25 95.62 2.68 0.108 5.11 Bond lengths and angles S11 - Distance Angles O12 1.4302 (0.0014) O11 1.4326 (0.0014) 119.15 (0.08) N12 1.6441 (0.0016) 109.03 (0.09) 103.70 (0.08) C14 1.7412 (0.0018) 108.47 (0.09) 109.59 (0.08) 106.12 (0.08) S11 - O12 O11 N12 O11 - Distance Angles S11 1.4326 (0.0014) O11 - O12 - Distance Angles S11 1.4302 (0.0014) O12 - O32 - Distance Angles C35 1.1961 (0.0022) O32 - N12 - Distance Angles C17 1.4126 (0.0023) S11 1.6441 (0.0016) 122.78 (0.13) N12 - C17 O31 - Distance Angles C35 1.3209 (0.0023) C34 1.4768 (0.0026) 115.98 (0.16) O31 - C35 N11 - Distance Angles C11 1.3730 (0.0025) N11 - C35 - Distance Angles O32 1.1961 (0.0022) O31 1.3209 (0.0023) 126.81 (0.18) C35_$1 1.5286 (0.0038) 123.99 (0.22) 109.19 (0.19) C35 - O32 O31 C12 - Distance Angles C13 1.3762 (0.0027) C11 1.4006 (0.0028) 120.83 (0.18) C12 - C13 C17 - Distance Angles N13 1.3370 (0.0024) C21 1.3850 (0.0027) 123.16 (0.17) N12 1.4126 (0.0023) 113.79 (0.16) 123.02 (0.17) C17 - N13 C21 C16 - Distance Angles C15 1.3783 (0.0027) C11 1.3962 (0.0027) 120.41 (0.18) C16 - C15 C13 - Distance Angles C12 1.3762 (0.0027) C14 1.3916 (0.0026) 119.70 (0.18) C13 - C12 C14 - Distance Angles C15 1.3892 (0.0027) C13 1.3916 (0.0026) 120.05 (0.17) S11 1.7412 (0.0018) 120.33 (0.14) 119.60 (0.14) C14 - C15 C13 C15 - Distance Angles C16 1.3783 (0.0027) C14 1.3892 (0.0027) 120.19 (0.17) C15 - C16 C11 - Distance Angles N11 1.3730 (0.0025) C16 1.3962 (0.0027) 120.78 (0.18) C12 1.4006 (0.0028) 120.38 (0.18) 118.81 (0.17) C11 - N11 C16 C34 - Distance Angles O31 1.4768 (0.0026) C33 1.5037 (0.0031) 107.20 (0.18) C34 - O31 C32 - Distance Angles C33 1.5055 (0.0035) C31 1.5305 (0.0048) 111.09 (0.31) C32 - C33 C33 - Distance Angles C34 1.5037 (0.0031) C32 1.5055 (0.0035) 114.07 (0.23) C33 - C34 C31 - Distance Angles C32 1.5305 (0.0048) C31 - N13 - Distance Angles C17 1.3370 (0.0024) C18 1.3510 (0.0024) 117.29 (0.16) N13 - C17 C18 - Distance Angles N13 1.3510 (0.0024) C19 1.3712 (0.0029) 123.41 (0.20) C18 - N13 C19 - Distance Angles C18 1.3712 (0.0029) C20 1.3776 (0.0032) 118.38 (0.19) C19 - C18 C21 - Distance Angles C17 1.3850 (0.0027) C20 1.3858 (0.0028) 118.12 (0.19) C21 - C17 C20 - Distance Angles C19 1.3776 (0.0032) C21 1.3858 (0.0028) 119.62 (0.20) C20 - C19 FMAP and GRID set by program FMAP 2 1 24 GRID -2.381 -2 -2 2.381 2 2 R1 = 0.0641 for 3860 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.43 at 0.0030 0.3109 0.0733 [ 0.94 A from O31 ] Deepest hole -0.47 at 0.2918 0.2034 0.7441 [ 0.79 A from S11 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2500 / 21759 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0030 0.6891 -0.0733 1.00000 0.05 0.43 0.94 O31 1.49 C35 1.67 H34A 1.71 C34 Q2 1 -0.0122 0.8924 -0.3039 1.00000 0.05 0.41 1.02 C33 1.12 C32 1.16 H33A 1.47 H33B Q3 1 0.0733 0.7919 -0.1012 1.00000 0.05 0.32 0.81 H34A 1.44 C34 1.69 H32B 1.87 O31 Q4 1 0.4446 0.3362 0.7405 1.00000 0.05 0.28 0.56 C14 0.83 C15 1.56 H15 1.73 C13 Q5 1 0.0007 0.8989 -0.1328 1.00000 0.05 0.26 0.63 H32B 0.96 C32 1.16 H32A 1.79 C33 Q6 1 0.2381 0.7168 -0.1658 1.00000 0.05 0.25 0.68 H34A 1.00 C34 1.36 H34B 2.11 O31 Q7 1 0.2645 0.2325 0.5963 1.00000 0.05 0.23 0.97 O11 1.09 S11 1.47 N12 1.51 H17 Q8 1 0.1506 0.3157 0.8971 1.00000 0.05 0.21 1.04 O12 1.98 H15 2.23 S11 2.28 C35 Q9 1 0.4863 0.3462 0.6464 1.00000 0.05 0.20 0.63 C14 0.80 C13 1.58 H13 1.73 C15 Q10 1 -0.0257 0.9553 -0.4015 1.00000 0.05 0.19 1.36 H31C 1.40 H31B 1.50 C31 1.77 H33A Q11 1 -0.1531 1.1217 -0.1809 1.00000 0.05 0.19 0.89 H31A 1.38 C31 1.88 H31C 1.92 C32 Q12 1 0.2611 0.2719 0.7985 1.00000 0.05 0.19 0.91 O12 1.17 S11 1.73 C14 1.83 H15 Q13 1 0.7062 0.3995 0.6457 1.00000 0.05 0.18 0.65 C11 0.75 C12 1.46 H12 1.79 N11 Q14 1 0.4944 -0.2016 0.8630 1.00000 0.05 0.18 0.71 C19 0.87 C20 1.45 H19 1.58 H20 Q15 1 -0.0712 0.9824 -0.3837 1.00000 0.05 0.18 0.99 H31B 1.17 C31 1.18 H31C 1.97 H31A Q16 1 0.6140 -0.1897 0.7612 1.00000 0.05 0.18 0.74 C18 0.81 C19 1.48 H18 1.54 H19 Q17 1 0.4088 0.0205 0.7852 1.00000 0.05 0.18 0.76 C21 0.82 C17 1.37 H21 1.86 N12 Q18 1 0.1378 0.5354 -0.3146 1.00000 0.05 0.17 1.82 H34B 2.06 H12 2.06 O31 2.15 C34 Q19 1 0.3386 0.2641 0.4867 1.00000 0.05 0.17 1.39 O11 1.53 H18 1.81 H17 2.03 C18 Q20 1 0.0841 0.5341 -0.2270 1.00000 0.05 0.17 1.28 O31 1.92 C34 1.94 H34B 2.10 C35 Q21 1 -0.0874 0.9609 -0.4540 1.00000 0.05 0.16 1.45 H31B 1.89 H31C 1.96 C31 2.07 H31C Q22 1 0.0801 0.5794 0.0289 1.00000 0.05 0.16 0.81 C35 0.82 O32 1.90 O31 1.92 C35 Q23 1 0.2860 0.4630 0.8191 1.00000 0.05 0.16 1.58 H15 1.66 C15 1.86 H34B 2.01 C14 Q24 1 0.2779 0.5393 -0.1390 1.00000 0.05 0.16 1.58 O32 1.64 H34B 1.87 C35 1.94 C34 Q25 1 0.1863 0.5519 0.0851 1.00000 0.05 0.16 0.86 O32 1.40 H10 1.89 C35 2.01 H16 Shortest distances between peaks (including symmetry equivalents) 10 15 0.43 15 21 0.87 23 24 0.89 10 21 0.89 18 20 0.92 4 9 0.97 3 5 1.18 2 10 1.19 7 19 1.21 22 25 1.24 8 12 1.25 1 3 1.27 14 16 1.28 2 15 1.31 3 6 1.47 1 22 1.69 6 24 1.70 4 23 1.72 4 12 1.76 10 21 1.79 21 21 1.81 2 5 1.90 12 23 1.95 2 21 1.95 1 8 1.95 20 23 1.97 15 21 1.98 8 23 1.99 8 22 2.03 1 5 2.07 22 24 2.10 9 13 2.10 1 6 2.10 10 10 2.17 1 20 2.21 20 24 2.21 18 23 2.21 7 12 2.26 10 15 2.28 14 17 2.30 24 25 2.32 9 12 2.34 9 23 2.34 3 22 2.37 4 13 2.39 5 6 2.40 5 11 2.41 16 17 2.41 6 23 2.42 4 24 2.43 8 20 2.45 15 15 2.47 20 22 2.48 12 17 2.51 22 22 2.53 1 24 2.53 11 15 2.54 6 22 2.55 8 24 2.57 2 3 2.58 18 24 2.58 2 11 2.59 22 23 2.62 7 9 2.64 20 25 2.64 4 8 2.65 6 14 2.65 6 20 2.68 3 24 2.71 9 19 2.73 12 20 2.73 3 8 2.74 16 19 2.74 1 22 2.77 12 24 2.79 1 25 2.81 2 21 2.83 10 11 2.83 20 22 2.85 12 18 2.87 23 25 2.91 4 7 2.91 8 22 2.92 6 18 2.93 8 25 2.94 3 20 2.94 1 18 2.94 6 25 2.96 8 18 2.98 5 15 2.98 5 10 2.98 Time profile in seconds ----------------------- 0.28: 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. 1.97: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.61: Structure factors and derivatives 3.91: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.39: Solve l.s. equations 0.00: Generate HTAB table 0.09: Other dependent quantities, CIF, tables 0.83: Analysis of variance 0.28: Merge reflections for Fourier and .fcf 0.22: Fourier summations 0.27: Peaksearch 0.06: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 14:48:31 Total elapsed time: 10.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++