+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 10:40:05 on 19-Apr-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P2(1)2(1)2(1) CELL 0.71069 5.7880 17.4990 19.4630 90.000 90.000 90.000 ZERR 4.00 0.0050 0.0050 0.0050 0.005 0.005 0.005 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O P UNIT 92 92 12 4 V = 1971.29 F(000) = 800.0 Mu = 0.16 mm-1 Cell Wt = 1513.54 Rho = 1.275 SHEL 7 0.84 ACTA TEMP -153 SIZE 0.15 0.04 0.03 FMAP 2 PLAN 25 L.S. 4 WGHT 0.0307 0.0000 EXTI 0.003377 FVAR 0.84747 P1 4 0.990205 0.118357 0.216253 11.00000 0.03098 0.04075 = 0.03218 0.00096 0.00038 -0.00127 O1 3 1.244005 0.111044 0.207735 11.00000 0.02779 0.05111 = 0.03834 0.00255 0.00038 0.00057 O2 3 0.502459 -0.033895 0.091919 11.00000 0.04743 0.04371 = 0.05786 -0.00178 -0.01409 0.00011 O3 3 0.737011 -0.133871 0.108131 11.00000 0.07275 0.03947 = 0.06068 -0.00714 -0.01543 0.00755 C1 1 0.897652 0.216856 0.215764 11.00000 0.03758 0.04243 = 0.02388 0.00410 -0.00322 -0.00932 C2 1 0.683264 0.240324 0.240581 11.00000 0.04052 0.03739 = 0.05097 0.00281 -0.00142 -0.00414 AFIX 43 H2 2 0.575101 0.203512 0.256467 11.00000 -1.20000 AFIX 0 C3 1 0.627908 0.317166 0.242092 11.00000 0.03278 0.04729 = 0.05287 -0.00578 0.00083 0.00308 AFIX 43 H3 2 0.482092 0.332957 0.259428 11.00000 -1.20000 AFIX 0 C4 1 0.782450 0.370933 0.218675 11.00000 0.04613 0.03711 = 0.04792 -0.00036 -0.01415 0.00296 AFIX 43 H4 2 0.744138 0.423674 0.220700 11.00000 -1.20000 AFIX 0 C5 1 0.993399 0.348381 0.192199 11.00000 0.04871 0.04488 = 0.04049 0.00421 -0.00411 -0.01349 AFIX 43 H5 2 1.098716 0.385272 0.174836 11.00000 -1.20000 AFIX 0 C6 1 1.049898 0.270972 0.191250 11.00000 0.03854 0.04512 = 0.04094 0.00113 0.00060 -0.00650 AFIX 43 H6 2 1.195224 0.255286 0.173479 11.00000 -1.20000 AFIX 0 C7 1 0.893634 0.079307 0.297472 11.00000 0.03247 0.03334 = 0.03869 0.00083 0.00304 -0.00011 C8 1 1.058290 0.078286 0.350087 11.00000 0.02954 0.04174 = 0.04310 -0.00068 -0.00168 -0.00216 AFIX 43 H8 2 1.208681 0.098015 0.341867 11.00000 -1.20000 AFIX 0 C9 1 1.003452 0.048603 0.414341 11.00000 0.03883 0.04035 = 0.03449 0.00424 -0.00730 -0.00223 AFIX 43 H9 2 1.115045 0.048945 0.450133 11.00000 -1.20000 AFIX 0 C10 1 0.787256 0.018777 0.425865 11.00000 0.04392 0.03794 = 0.03332 0.00192 0.00449 0.00594 AFIX 43 H10 2 0.749659 -0.001925 0.469580 11.00000 -1.20000 AFIX 0 C11 1 0.623420 0.018872 0.373574 11.00000 0.03132 0.03801 = 0.04696 0.00378 -0.00127 0.00000 AFIX 43 H11 2 0.474784 -0.002338 0.381635 11.00000 -1.20000 AFIX 0 C12 1 0.675341 0.049682 0.309775 11.00000 0.03750 0.03622 = 0.03449 0.00390 -0.00131 0.00018 AFIX 43 H12 2 0.561629 0.050489 0.274584 11.00000 -1.20000 AFIX 0 C13 1 0.820647 0.070620 0.150562 11.00000 0.03181 0.04301 = 0.03070 -0.00018 -0.00020 0.00181 AFIX 13 H13 2 0.653852 0.080108 0.160891 11.00000 -1.20000 AFIX 0 C14 1 0.871897 0.104654 0.080171 11.00000 0.03679 0.03353 = 0.03188 -0.00522 -0.00179 -0.00496 C15 1 0.709556 0.149910 0.048048 11.00000 0.03435 0.03394 = 0.03846 -0.00074 -0.00308 0.00277 AFIX 43 H15 2 0.567274 0.160488 0.070446 11.00000 -1.20000 AFIX 0 C16 1 0.751714 0.180145 -0.016585 11.00000 0.03306 0.03808 = 0.04024 0.00006 -0.00336 -0.00010 AFIX 43 H16 2 0.637445 0.210524 -0.038532 11.00000 -1.20000 AFIX 0 C17 1 0.958389 0.166263 -0.048957 11.00000 0.04724 0.03490 = 0.02629 0.00225 -0.00303 -0.00622 AFIX 43 H17 2 0.987141 0.186972 -0.093259 11.00000 -1.20000 AFIX 0 C18 1 1.124540 0.122042 -0.016867 11.00000 0.03312 0.04121 = 0.04118 -0.00293 0.00310 -0.00378 AFIX 43 H18 2 1.268030 0.112660 -0.039012 11.00000 -1.20000 AFIX 0 C19 1 1.081542 0.091200 0.048018 11.00000 0.03001 0.04014 = 0.03917 -0.00783 -0.00241 -0.00104 AFIX 43 H19 2 1.195933 0.061007 0.070116 11.00000 -1.20000 AFIX 0 C20 1 0.860776 -0.016565 0.152692 11.00000 0.04475 0.04358 = 0.03753 0.00311 -0.00218 0.00486 AFIX 23 H20A 2 1.013939 -0.028354 0.132684 11.00000 -1.20000 H20B 2 0.861169 -0.033980 0.201088 11.00000 -1.20000 AFIX 0 C21 1 0.677315 -0.059169 0.113623 11.00000 0.05130 0.03747 = 0.03609 -0.00011 0.00267 0.00121 C22 1 0.565946 -0.181942 0.074366 11.00000 0.11093 0.03725 = 0.07320 -0.00645 -0.02074 -0.01075 AFIX 23 H22A 2 0.555498 -0.168904 0.024967 11.00000 -1.20000 H22B 2 0.412083 -0.174370 0.095516 11.00000 -1.20000 AFIX 0 C23 1 0.642017 -0.262325 0.083007 11.00000 0.13926 0.04502 = 0.08414 -0.00624 0.00913 -0.00051 AFIX 137 H23A 2 0.795380 -0.268862 0.062497 11.00000 -1.50000 H23B 2 0.531886 -0.296451 0.060176 11.00000 -1.50000 H23C 2 0.649036 -0.274763 0.132057 11.00000 -1.50000 HKLF 4 Covalent radii and connectivity table for s92 in P2(1)2(1)2(1) C 0.770 H 0.320 O 0.660 P 1.100 P1 - O1 C1 C7 C13 O1 - P1 O2 - C21 O3 - C21 C22 C1 - C6 C2 P1 C2 - C3 C1 C3 - C4 C2 C4 - C3 C5 C5 - C4 C6 C6 - C1 C5 C7 - C12 C8 P1 C8 - C9 C7 C9 - C10 C8 C10 - C9 C11 C11 - C12 C10 C12 - C7 C11 C13 - C14 C20 P1 C14 - C15 C19 C13 C15 - C14 C16 C16 - C17 C15 C17 - C16 C18 C18 - C17 C19 C19 - C14 C18 C20 - C21 C13 C21 - O2 O3 C20 C22 - O3 C23 C23 - C22 11889 Reflections read, of which 1544 rejected -6 =< h =< 6, -19 =< k =< 20, -22 =< l =< 23, Max. 2-theta = 50.00 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 6 2 0 109.70 24.24 2 182.60 4 2 6 404.74 24.88 3 138.45 -3 12 14 114.08 22.52 2 159.12 3 Inconsistent equivalents 3383 Unique reflections, of which 0 suppressed R(int) = 0.0956 R(sigma) = 0.1135 Friedel opposites not merged Maximum memory for data reduction = 2353 / 33376 Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 3061 / 305280 wR2 = 0.1102 before cycle 1 for 3383 data and 246 / 246 parameters GooF = S = 0.981; Restrained GooF = 0.981 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0307 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84759 0.00191 0.061 OSF 2 0.00342 0.00092 0.047 EXTI Mean shift/esd = 0.016 Maximum = 0.063 for z C23 Max. shift = 0.002 A for H23A Max. dU = 0.000 for C22 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3061 / 305280 wR2 = 0.1101 before cycle 2 for 3383 data and 246 / 246 parameters GooF = S = 0.981; Restrained GooF = 0.981 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0307 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84761 0.00191 0.014 OSF 2 0.00344 0.00092 0.016 EXTI Mean shift/esd = 0.005 Maximum = 0.025 for tors H23A Max. shift = 0.001 A for H23A Max. dU = 0.000 for C22 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3061 / 305280 wR2 = 0.1102 before cycle 3 for 3383 data and 246 / 246 parameters GooF = S = 0.981; Restrained GooF = 0.981 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0307 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84762 0.00191 0.003 OSF 2 0.00344 0.00093 0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.006 for tors H23A Max. shift = 0.000 A for H23C Max. dU = 0.000 for C22 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3061 / 305280 wR2 = 0.1102 before cycle 4 for 3383 data and 246 / 246 parameters GooF = S = 0.981; Restrained GooF = 0.981 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0307 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84762 0.00191 0.000 OSF 2 0.00344 0.00093 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for tors H23A Max. shift = 0.000 A for H23C Max. dU = 0.000 for O3 Largest correlation matrix elements 0.532 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.5751 0.2035 0.2564 43 0.950 0.000 C2 C3 C1 H3 0.4821 0.3330 0.2595 43 0.950 0.000 C3 C4 C2 H4 0.7441 0.4237 0.2207 43 0.950 0.000 C4 C3 C5 H5 1.0987 0.3853 0.1748 43 0.950 0.000 C5 C4 C6 H6 1.1953 0.2553 0.1735 43 0.950 0.000 C6 C1 C5 H8 1.2087 0.0980 0.3419 43 0.950 0.000 C8 C9 C7 H9 1.1150 0.0489 0.4501 43 0.950 0.000 C9 C10 C8 H10 0.7497 -0.0019 0.4696 43 0.950 0.000 C10 C9 C11 H11 0.4748 -0.0024 0.3816 43 0.950 0.000 C11 C12 C10 H12 0.5616 0.0505 0.2746 43 0.950 0.000 C12 C7 C11 H13 0.6538 0.0801 0.1609 13 1.000 0.000 C13 C14 C20 P1 H15 0.5673 0.1605 0.0704 43 0.950 0.000 C15 C14 C16 H16 0.6375 0.2105 -0.0385 43 0.950 0.000 C16 C17 C15 H17 0.9871 0.1869 -0.0933 43 0.950 0.000 C17 C16 C18 H18 1.2680 0.1127 -0.0390 43 0.950 0.000 C18 C17 C19 H19 1.1959 0.0610 0.0701 43 0.950 0.000 C19 C14 C18 H20A 1.0140 -0.0283 0.1327 23 0.990 0.000 C20 C21 C13 H20B 0.8612 -0.0340 0.2011 23 0.990 0.000 C20 C21 C13 H22A 0.5557 -0.1689 0.0250 23 0.990 0.000 C22 O3 C23 H22B 0.4121 -0.1744 0.0955 23 0.990 0.000 C22 O3 C23 H23A 0.7957 -0.2688 0.0627 137 0.980 0.000 C23 C22 H23A H23B 0.5322 -0.2965 0.0601 137 0.980 0.000 C23 C22 H23A H23C 0.6485 -0.2748 0.1321 137 0.980 0.000 C23 C22 H23A s92 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq P1 0.99020 0.11836 0.21625 1.00000 0.03101 0.04078 0.03220 0.00095 0.00039 -0.00127 0.03467 0.00189 0.00020 0.00006 0.00005 0.00000 0.00053 0.00059 0.00053 0.00053 0.00052 0.00060 0.00027 O1 1.24402 0.11104 0.20773 1.00000 0.02775 0.05111 0.03835 0.00260 0.00039 0.00058 0.03907 0.00465 0.00041 0.00016 0.00013 0.00000 0.00142 0.00172 0.00159 0.00150 0.00126 0.00138 0.00067 O2 0.50245 -0.03389 0.09192 1.00000 0.04742 0.04373 0.05787 -0.00177 -0.01411 0.00011 0.04967 0.00507 0.00064 0.00015 0.00014 0.00000 0.00201 0.00171 0.00201 0.00145 0.00184 0.00189 0.00079 O3 0.73701 -0.13387 0.10814 1.00000 0.07284 0.03943 0.06071 -0.00714 -0.01550 0.00751 0.05766 0.00553 0.00061 0.00017 0.00017 0.00000 0.00257 0.00202 0.00209 0.00164 0.00182 0.00174 0.00094 C1 0.89763 0.21685 0.21576 1.00000 0.03757 0.04237 0.02383 0.00410 -0.00318 -0.00930 0.03459 0.00679 0.00069 0.00023 0.00020 0.00000 0.00231 0.00241 0.00205 0.00207 0.00202 0.00195 0.00095 C2 0.68329 0.24031 0.24057 1.00000 0.04053 0.03743 0.05095 0.00281 -0.00136 -0.00422 0.04297 0.00751 0.00078 0.00024 0.00022 0.00000 0.00297 0.00274 0.00298 0.00215 0.00208 0.00211 0.00117 H2 0.57512 0.20349 0.25644 1.00000 0.05156 0.00000 0.00000 C3 0.62787 0.31717 0.24210 1.00000 0.03281 0.04717 0.05286 -0.00573 0.00082 0.00308 0.04428 0.00757 0.00081 0.00025 0.00022 0.00000 0.00262 0.00290 0.00299 0.00230 0.00211 0.00228 0.00115 H3 0.48207 0.33296 0.25945 1.00000 0.05313 0.00000 0.00000 C4 0.78244 0.37092 0.21868 1.00000 0.04619 0.03710 0.04793 -0.00029 -0.01416 0.00297 0.04374 0.00729 0.00075 0.00025 0.00023 0.00000 0.00263 0.00256 0.00269 0.00239 0.00235 0.00219 0.00108 H4 0.74412 0.42366 0.22070 1.00000 0.05249 0.00000 0.00000 C5 0.99343 0.34839 0.19220 1.00000 0.04873 0.04482 0.04047 0.00417 -0.00414 -0.01347 0.04467 0.00727 0.00091 0.00024 0.00020 0.00000 0.00277 0.00255 0.00247 0.00189 0.00250 0.00258 0.00106 H5 1.09873 0.38528 0.17484 1.00000 0.05361 0.00000 0.00000 C6 1.04992 0.27097 0.19126 1.00000 0.03864 0.04528 0.04086 0.00104 0.00063 -0.00644 0.04159 0.00709 0.00074 0.00024 0.00021 0.00000 0.00294 0.00277 0.00258 0.00211 0.00186 0.00205 0.00113 H6 1.19526 0.25528 0.17350 1.00000 0.04991 0.00000 0.00000 C7 0.89363 0.07930 0.29746 1.00000 0.03253 0.03330 0.03855 0.00090 0.00298 -0.00012 0.03479 0.00686 0.00069 0.00022 0.00021 0.00000 0.00226 0.00230 0.00259 0.00194 0.00204 0.00181 0.00100 C8 1.05827 0.07829 0.35008 1.00000 0.02962 0.04163 0.04314 -0.00074 -0.00167 -0.00221 0.03813 0.00684 0.00070 0.00023 0.00021 0.00000 0.00284 0.00252 0.00264 0.00216 0.00190 0.00183 0.00112 H8 1.20866 0.09802 0.34186 1.00000 0.04575 0.00000 0.00000 C9 1.00344 0.04860 0.41434 1.00000 0.03873 0.04036 0.03450 0.00429 -0.00736 -0.00222 0.03787 0.00704 0.00084 0.00020 0.00019 0.00000 0.00246 0.00240 0.00235 0.00187 0.00234 0.00251 0.00097 H9 1.11505 0.04894 0.45012 1.00000 0.04544 0.00000 0.00000 C10 0.78728 0.01878 0.42586 1.00000 0.04400 0.03786 0.03324 0.00198 0.00453 0.00592 0.03837 0.00764 0.00077 0.00023 0.00022 0.00000 0.00287 0.00260 0.00250 0.00208 0.00211 0.00221 0.00109 H10 0.74968 -0.00190 0.46959 1.00000 0.04604 0.00000 0.00000 C11 0.62342 0.01886 0.37357 1.00000 0.03124 0.03803 0.04701 0.00384 -0.00134 0.00003 0.03876 0.00735 0.00078 0.00023 0.00021 0.00000 0.00240 0.00250 0.00288 0.00218 0.00208 0.00200 0.00105 H11 0.47480 -0.00237 0.38162 1.00000 0.04651 0.00000 0.00000 C12 0.67536 0.04969 0.30978 1.00000 0.03749 0.03624 0.03438 0.00385 -0.00142 0.00018 0.03604 0.00719 0.00073 0.00022 0.00021 0.00000 0.00254 0.00246 0.00248 0.00201 0.00180 0.00193 0.00104 H12 0.56164 0.05051 0.27459 1.00000 0.04325 0.00000 0.00000 C13 0.82064 0.07063 0.15057 1.00000 0.03179 0.04300 0.03069 -0.00020 -0.00020 0.00176 0.03516 0.00695 0.00072 0.00023 0.00020 0.00000 0.00256 0.00263 0.00234 0.00203 0.00180 0.00198 0.00105 H13 0.65385 0.08011 0.16090 1.00000 0.04219 0.00000 0.00000 C14 0.87190 0.10465 0.08017 1.00000 0.03674 0.03344 0.03187 -0.00526 -0.00184 -0.00494 0.03402 0.00668 0.00072 0.00023 0.00020 0.00000 0.00243 0.00240 0.00225 0.00191 0.00190 0.00213 0.00098 C15 0.70957 0.14990 0.04804 1.00000 0.03427 0.03394 0.03845 -0.00072 -0.00303 0.00277 0.03555 0.00693 0.00075 0.00022 0.00021 0.00000 0.00257 0.00235 0.00264 0.00198 0.00197 0.00191 0.00104 H15 0.56728 0.16048 0.07044 1.00000 0.04267 0.00000 0.00000 C16 0.75172 0.18015 -0.01658 1.00000 0.03295 0.03816 0.04032 0.00006 -0.00333 -0.00009 0.03714 0.00690 0.00073 0.00023 0.00021 0.00000 0.00259 0.00249 0.00260 0.00209 0.00201 0.00201 0.00103 H16 0.63747 0.21054 -0.03853 1.00000 0.04457 0.00000 0.00000 C17 0.95841 0.16625 -0.04895 1.00000 0.04720 0.03494 0.02633 0.00230 -0.00302 -0.00622 0.03616 0.00674 0.00076 0.00022 0.00020 0.00000 0.00310 0.00235 0.00218 0.00191 0.00200 0.00210 0.00106 H17 0.98715 0.18695 -0.09326 1.00000 0.04339 0.00000 0.00000 C18 1.12455 0.12204 -0.01687 1.00000 0.03313 0.04115 0.04123 -0.00292 0.00311 -0.00374 0.03850 0.00694 0.00072 0.00024 0.00021 0.00000 0.00221 0.00246 0.00257 0.00234 0.00201 0.00223 0.00100 H18 1.26804 0.11266 -0.03901 1.00000 0.04621 0.00000 0.00000 C19 1.08153 0.09120 0.04801 1.00000 0.02998 0.04004 0.03912 -0.00777 -0.00247 -0.00106 0.03638 0.00671 0.00069 0.00023 0.00022 0.00000 0.00243 0.00258 0.00259 0.00203 0.00191 0.00183 0.00109 H19 1.19592 0.06101 0.07011 1.00000 0.04366 0.00000 0.00000 C20 0.86081 -0.01656 0.15270 1.00000 0.04471 0.04368 0.03743 0.00313 -0.00213 0.00488 0.04194 0.00748 0.00081 0.00023 0.00022 0.00000 0.00285 0.00268 0.00249 0.00214 0.00207 0.00219 0.00111 H20A 1.01397 -0.02834 0.13268 1.00000 0.05033 0.00000 0.00000 H20B 0.86124 -0.03398 0.20109 1.00000 0.05033 0.00000 0.00000 C21 0.67729 -0.05917 0.11363 1.00000 0.05135 0.03745 0.03606 -0.00023 0.00263 0.00120 0.04162 0.00801 0.00085 0.00025 0.00023 0.00000 0.00315 0.00278 0.00259 0.00217 0.00225 0.00228 0.00112 C22 0.56601 -0.18194 0.07436 1.00000 0.11118 0.03715 0.07330 -0.00651 -0.02061 -0.01077 0.07388 0.00866 0.00108 0.00026 0.00029 0.00000 0.00609 0.00297 0.00386 0.00264 0.00352 0.00309 0.00197 H22A 0.55566 -0.16891 0.02495 1.00000 0.08865 0.00000 0.00000 H22B 0.41211 -0.17436 0.09548 1.00000 0.08865 0.00000 0.00000 C23 0.64207 -0.26234 0.08303 1.00000 0.13926 0.04499 0.08419 -0.00627 0.00906 -0.00033 0.08948 0.01121 0.00135 0.00028 0.00032 0.00000 0.00641 0.00341 0.00444 0.00314 0.00415 0.00365 0.00213 H23A 0.79569 -0.26884 0.06268 1.00000 0.13422 0.00000 0.00000 H23B 0.53225 -0.29646 0.06006 1.00000 0.13422 0.00000 0.00000 H23C 0.64850 -0.27481 0.13208 1.00000 0.13422 0.00000 0.00000 Final Structure Factor Calculation for s92 in P2(1)2(1)2(1) Total number of l.s. parameters = 246 Maximum vector length = 511 Memory required = 2817 / 25046 wR2 = 0.1102 before cycle 5 for 3383 data and 2 / 246 parameters GooF = S = 0.981; Restrained GooF = 0.981 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0307 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0552 for 2169 Fo > 4sig(Fo) and 0.1106 for all 3383 data wR2 = 0.1102, GooF = S = 0.981, Restrained GooF = 0.981 for all data Flack x parameter = 0.6578 with esd 0.1708 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 27.00 for non-hydrogen and 23.00 for hydrogen atoms Principal mean square atomic displacements U 0.0410 0.0323 0.0307 P1 0.0516 0.0378 0.0277 O1 0.0678 0.0438 0.0375 O2 0.0857 0.0503 0.0370 O3 0.0506 0.0304 0.0228 C1 0.0520 0.0426 0.0343 C2 0.0564 0.0444 0.0320 C3 0.0615 0.0377 0.0321 C4 0.0620 0.0389 0.0331 C5 0.0492 0.0410 0.0345 C6 0.0399 0.0333 0.0312 C7 0.0435 0.0419 0.0290 C8 0.0472 0.0379 0.0285 C9 0.0491 0.0344 0.0316 C10 0.0485 0.0367 0.0311 C11 0.0396 0.0374 0.0311 C12 0.0433 0.0316 0.0307 C13 0.0407 0.0360 0.0254 C14 0.0406 0.0351 0.0310 C15 0.0416 0.0382 0.0317 C16 0.0504 0.0325 0.0256 C17 0.0459 0.0383 0.0313 C18 0.0474 0.0335 0.0282 C19 0.0491 0.0422 0.0345 C20 0.0519 0.0375 0.0355 C21 0.1209 0.0676 0.0331 C22 0.1407 0.0837 0.0440 C23 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.019 0.028 0.037 0.046 0.057 0.068 0.085 0.107 0.150 1.000 Number in group 357. 323. 336. 358. 335. 321. 353. 330. 329. 341. GooF 0.873 0.879 0.975 0.938 0.969 1.078 1.021 0.978 1.054 1.030 K 1.641 0.939 1.073 1.009 1.034 0.992 1.001 0.997 0.999 1.012 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.25 1.42 1.77 inf Number in group 356. 338. 324. 340. 342. 330. 346. 335. 333. 339. GooF 0.892 0.965 0.905 0.983 1.031 0.989 0.941 0.995 0.983 1.107 K 1.094 1.074 1.061 1.014 1.003 0.998 1.002 0.990 1.008 1.008 R1 0.292 0.268 0.194 0.193 0.133 0.088 0.075 0.067 0.055 0.031 Recommended weighting scheme: WGHT 0.0301 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) -1 5 21 158.25 52.70 3.93 0.041 0.89 -5 11 9 147.82 46.35 3.85 0.039 0.86 2 9 15 55.85 131.11 3.39 0.065 1.01 -5 1 13 86.42 26.81 3.36 0.029 0.91 4 10 0 73.91 155.00 3.25 0.070 1.12 4 6 2 298.74 423.21 3.12 0.116 1.28 -2 4 6 1186.48 1007.36 3.03 0.180 1.94 2 3 17 216.09 296.33 3.02 0.097 1.05 6 9 0 0.00 88.97 3.01 0.053 0.86 -2 12 16 288.11 164.12 2.91 0.072 0.89 1 3 1 593.18 509.63 2.90 0.128 4.02 1 3 9 1165.66 1011.11 2.88 0.180 1.91 -1 16 2 42.28 104.56 2.86 0.058 1.07 -1 7 10 481.79 400.84 2.85 0.113 1.48 1 16 12 84.87 8.68 2.84 0.017 0.90 -2 3 9 201.55 263.88 2.83 0.092 1.66 -1 11 10 229.10 303.53 2.82 0.099 1.20 3 12 15 187.09 69.90 2.81 0.047 0.87 -3 8 16 -4.69 57.35 2.77 0.043 0.93 1 1 2 4394.07 4865.32 2.76 0.395 4.79 -2 6 2 540.36 468.38 2.74 0.122 2.01 -2 17 1 61.15 2.76 2.73 0.009 0.97 3 4 1 322.60 442.75 2.69 0.119 1.76 -1 3 19 55.10 121.66 2.69 0.062 0.99 3 1 15 148.61 242.25 2.68 0.088 1.07 5 3 5 220.55 165.01 2.68 0.073 1.09 0 19 7 281.56 123.06 2.67 0.063 0.87 2 6 16 40.14 95.33 2.67 0.055 1.05 -3 2 12 274.44 341.12 2.66 0.104 1.23 4 2 8 39.30 88.16 2.62 0.053 1.23 -4 4 16 214.87 149.43 2.59 0.069 0.91 -2 3 3 679.95 604.39 2.58 0.139 2.41 5 9 6 33.56 80.12 2.53 0.051 0.95 -1 3 14 124.27 173.78 2.52 0.075 1.32 1 1 9 387.42 451.34 2.52 0.120 2.01 -6 4 9 154.33 80.38 2.52 0.051 0.86 5 6 10 66.66 20.77 2.52 0.026 0.94 0 12 7 79.71 25.11 2.51 0.028 1.29 2 2 17 455.10 351.33 2.51 0.106 1.06 -2 11 7 204.93 151.47 2.49 0.070 1.25 -1 18 2 33.65 89.08 2.46 0.053 0.95 -2 6 17 256.73 163.77 2.45 0.072 1.00 2 4 2 760.44 854.31 2.43 0.165 2.34 0 2 9 1283.69 1146.47 2.43 0.192 2.10 1 14 9 71.92 124.44 2.42 0.063 1.06 4 7 13 146.19 94.23 2.42 0.055 0.96 3 2 10 227.83 278.25 2.42 0.094 1.35 3 11 0 52.16 0.58 2.42 0.004 1.23 3 1 3 723.19 619.03 2.41 0.141 1.84 -2 16 8 -11.11 32.78 2.41 0.032 0.94 Bond lengths and angles P1 - Distance Angles O1 1.4839 (0.0028) C1 1.8049 (0.0042) 112.06 (0.17) C7 1.8105 (0.0041) 111.75 (0.17) 105.87 (0.18) C13 1.8152 (0.0041) 114.64 (0.18) 105.97 (0.19) 105.92 (0.19) P1 - O1 C1 C7 O1 - Distance Angles P1 1.4839 (0.0028) O1 - O2 - Distance Angles C21 1.1825 (0.0054) O2 - O3 - Distance Angles C21 1.3563 (0.0052) C22 1.4558 (0.0055) 114.78 (0.38) O3 - C21 C1 - Distance Angles C6 1.3788 (0.0054) C2 1.3932 (0.0058) 119.13 (0.39) P1 1.8049 (0.0042) 117.90 (0.33) 122.95 (0.31) C1 - C6 C2 C2 - Distance Angles C3 1.3830 (0.0057) C1 1.3932 (0.0058) 120.04 (0.41) C2 - C3 C3 - Distance Angles C4 1.3759 (0.0061) C2 1.3830 (0.0057) 120.46 (0.44) C3 - C4 C4 - Distance Angles C3 1.3759 (0.0061) C5 1.3829 (0.0064) 120.18 (0.41) C4 - C3 C5 - Distance Angles C4 1.3829 (0.0064) C6 1.3937 (0.0055) 119.29 (0.43) C5 - C4 C6 - Distance Angles C1 1.3788 (0.0054) C5 1.3937 (0.0055) 120.87 (0.42) C6 - C1 C7 - Distance Angles C12 1.3864 (0.0056) C8 1.3990 (0.0054) 119.30 (0.37) P1 1.8105 (0.0041) 124.99 (0.32) 115.69 (0.30) C7 - C12 C8 C8 - Distance Angles C9 1.3908 (0.0052) C7 1.3990 (0.0054) 120.50 (0.39) C8 - C9 C9 - Distance Angles C10 1.3741 (0.0062) C8 1.3908 (0.0052) 119.76 (0.39) C9 - C10 C10 - Distance Angles C9 1.3741 (0.0062) C11 1.3912 (0.0060) 120.06 (0.39) C10 - C9 C11 - Distance Angles C12 1.3867 (0.0055) C10 1.3912 (0.0060) 120.50 (0.42) C11 - C12 C12 - Distance Angles C7 1.3864 (0.0056) C11 1.3867 (0.0055) 119.85 (0.39) C12 - C7 C13 - Distance Angles C14 1.5231 (0.0053) C20 1.5439 (0.0056) 112.40 (0.33) P1 1.8152 (0.0041) 110.39 (0.28) 110.76 (0.28) C13 - C14 C20 C14 - Distance Angles C15 1.3788 (0.0056) C19 1.3854 (0.0056) 119.31 (0.39) C13 1.5231 (0.0053) 119.98 (0.38) 120.71 (0.38) C14 - C15 C19 C15 - Distance Angles C14 1.3788 (0.0056) C16 1.3863 (0.0057) 120.72 (0.42) C15 - C14 C16 - Distance Angles C17 1.3737 (0.0056) C15 1.3863 (0.0057) 120.12 (0.40) C16 - C17 C17 - Distance Angles C16 1.3737 (0.0056) C18 1.3831 (0.0056) 119.83 (0.39) C17 - C16 C18 - Distance Angles C17 1.3831 (0.0056) C19 1.3957 (0.0055) 120.05 (0.39) C18 - C17 C19 - Distance Angles C14 1.3854 (0.0056) C18 1.3957 (0.0055) 119.96 (0.38) C19 - C14 C20 - Distance Angles C21 1.5042 (0.0064) C13 1.5439 (0.0056) 111.71 (0.36) C20 - C21 C21 - Distance Angles O2 1.1825 (0.0054) O3 1.3563 (0.0052) 123.41 (0.43) C20 1.5042 (0.0064) 126.83 (0.40) 109.73 (0.40) C21 - O2 O3 C22 - Distance Angles O3 1.4558 (0.0055) C23 1.4838 (0.0067) 107.14 (0.48) C22 - O3 C23 - Distance Angles C22 1.4838 (0.0067) C23 - FMAP and GRID set by program FMAP 2 1 9 GRID -4.167 -2 -2 4.167 2 2 R1 = 0.0883 for 1996 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.16 at -0.0004 0.8795 0.1440 [ 1.63 A from H20A ] Deepest hole -0.22 at 0.1283 0.6177 0.2770 [ 0.70 A from P1 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 3351 / 22203 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9996 -0.1205 0.1440 1.00000 0.05 0.16 1.63 H20A 1.69 O3 2.00 C20 2.04 H20B Q2 1 1.4970 0.0569 -0.0162 1.00000 0.05 0.15 1.70 H18 1.77 H10 2.07 H9 2.14 C10 Q3 1 0.9980 -0.2803 0.1396 1.00000 0.05 0.15 1.91 H23A 2.03 H23C 2.36 C23 2.47 H8 Q4 1 1.3841 0.2383 0.1502 1.00000 0.05 0.15 1.22 H6 1.82 H17 2.17 C6 2.32 H15 Q5 1 0.8746 -0.1075 0.0777 1.00000 0.05 0.15 1.09 O3 1.58 C21 1.93 H20A 2.16 C20 Q6 1 1.0423 -0.1389 0.0444 1.00000 0.05 0.14 2.16 O3 2.33 H23B 2.44 H22B 2.59 H20A Q7 1 0.7620 0.1601 0.2010 1.00000 0.05 0.14 1.30 C1 1.54 P1 1.66 C2 1.71 H2 Q8 1 1.2281 0.0674 0.1431 1.00000 0.05 0.14 1.44 H19 1.48 O1 2.08 C19 2.09 H20A Q9 1 1.1071 0.1200 0.4422 1.00000 0.05 0.14 1.25 H9 1.49 C9 1.96 C8 2.03 H23A Q10 1 0.6705 -0.0349 0.5064 1.00000 0.05 0.14 1.03 H10 1.90 C14 1.94 C19 1.95 C10 Q11 1 0.4435 -0.0006 0.4132 1.00000 0.05 0.14 0.64 H11 1.34 C11 2.03 C10 2.08 H10 Q12 1 1.2170 0.0113 0.4355 1.00000 0.05 0.14 0.93 H9 1.46 C9 1.84 H11 2.23 H18 Q13 1 0.3225 0.3252 0.2028 1.00000 0.05 0.13 1.44 H3 1.54 H6 1.75 H5 1.85 C6 Q14 1 0.6147 -0.0232 0.1376 1.00000 0.05 0.13 0.86 C21 1.12 O2 1.46 C20 1.88 H13 Q15 1 0.9074 0.4748 0.2245 1.00000 0.05 0.13 1.30 H4 1.96 C4 1.98 H20B 2.15 H5 Q16 1 0.9329 -0.3341 0.1019 1.00000 0.05 0.13 1.59 H23A 1.80 C8 1.81 H8 2.03 H23C Q17 1 0.9060 -0.3195 0.0433 1.00000 0.05 0.13 1.15 H23A 1.60 H22A 1.98 C23 2.22 H23B Q18 1 1.4078 0.0391 0.4648 1.00000 0.05 0.13 1.73 H9 1.82 H11 2.11 H10 2.20 C11 Q19 1 0.8778 0.1089 0.1793 1.00000 0.05 0.13 0.93 C13 0.98 P1 1.44 H13 1.93 C14 Q20 1 0.4980 0.1224 0.0403 1.00000 0.05 0.13 0.97 H15 1.32 C15 2.04 H18 2.10 C16 Q21 1 0.4982 0.1215 0.2857 1.00000 0.05 0.13 1.31 H12 1.61 H2 1.69 C12 2.04 H8 Q22 1 0.9166 -0.2584 0.0008 1.00000 0.05 0.13 1.41 H23A 1.59 H22A 1.67 H23B 1.99 C22 Q23 1 1.0005 0.0977 -0.1231 1.00000 0.05 0.13 1.67 H17 1.68 H11 1.89 C17 2.16 C11 Q24 1 1.2468 0.0691 0.3431 1.00000 0.05 0.12 0.55 H8 1.11 C8 1.97 H11 2.01 C9 Q25 1 0.4066 0.3162 0.2386 1.00000 0.05 0.12 0.66 H3 1.28 C3 2.06 H6 2.08 C2 Shortest distances between peaks (including symmetry equivalents) 13 25 0.86 9 17 1.10 16 17 1.18 7 19 1.20 9 16 1.20 11 18 1.24 3 16 1.25 5 6 1.29 12 18 1.33 17 22 1.35 11 12 1.40 1 5 1.50 2 20 1.59 4 13 1.87 11 23 1.87 2 12 1.96 1 6 1.98 9 12 2.01 2 10 2.01 21 24 2.05 3 17 2.06 12 24 2.07 11 24 2.16 10 18 2.16 4 25 2.20 16 24 2.26 8 19 2.27 9 24 2.27 9 18 2.29 15 24 2.29 13 23 2.30 10 11 2.32 7 21 2.35 6 18 2.35 6 22 2.37 16 22 2.37 9 22 2.40 5 14 2.41 3 9 2.44 10 20 2.54 18 24 2.60 8 20 2.71 8 14 2.74 12 23 2.76 23 25 2.76 4 7 2.76 3 22 2.77 1 3 2.80 5 18 2.80 6 17 2.81 1 14 2.81 6 9 2.86 5 10 2.86 14 19 2.88 2 18 2.91 22 22 2.91 10 23 2.92 9 11 2.93 12 16 2.93 6 22 2.95 18 23 2.99 4 23 2.99 Time profile in seconds ----------------------- 0.16: 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. 0.39: 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 2.36: Structure factors and derivatives 1.61: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 0.19: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.11: Merge reflections for Fourier and .fcf 0.11: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 10:40:10 Total elapsed time: 5.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++