+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - MSDOS 32-BIT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-1 + + s92 started at 12:00:58 on 09-Sep-1999 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P-1 CELL 0.71073 9.643 11.069 11.162 93.35 102.12 98.20 ZERR 4.00 0.002 0.002 0.002 0.03 0.03 0.03 LATT 1 SFAC C H N O S CL UNIT 44 36 8 8 4 4 V = 1148.13 F(000) = 552.0 Mu = 0.50 mm-1 Cell Wt = 1074.85 Rho = 1.555 ACTA FMAP 2 PLAN 10 L.S. 4 BOND WGHT 0.048400 0.273000 FVAR 0.37779 S1 5 -0.00353 0.69594 0.02569 11.00000 0.02312 0.01915 = 0.02625 0.00392 0.00598 -0.00001 CL1 6 0.60256 1.15994 0.17130 11.00000 0.02412 0.04090 = 0.04558 0.00339 0.00433 -0.00642 O1 4 -0.15557 0.67660 0.01661 11.00000 0.02411 0.02633 = 0.03565 0.00383 0.01129 -0.00074 O2 4 0.08785 0.63835 0.11473 11.00000 0.03266 0.02387 = 0.02906 0.00789 0.00323 0.00284 N1 3 0.04330 0.84421 0.05353 11.00000 0.02239 0.01790 = 0.03332 0.00149 0.00275 0.00308 N2 3 0.18850 1.02850 0.06011 11.00000 0.02110 0.02052 = 0.03489 0.00467 0.00445 0.00063 C1 1 0.07406 0.58965 -0.34790 11.00000 0.03527 0.03645 = 0.03032 -0.00329 0.01218 -0.00145 C2 1 -0.05210 0.63244 -0.33902 11.00000 0.03071 0.04352 = 0.02872 0.00265 0.00265 0.00353 C3 1 -0.07602 0.66643 -0.22482 11.00000 0.02125 0.03097 = 0.03266 0.00300 0.00439 0.00573 C4 1 0.02735 0.65578 -0.12043 11.00000 0.02046 0.01714 = 0.02736 0.00366 0.00543 -0.00220 C5 1 0.15307 0.61187 -0.12864 11.00000 0.02206 0.02501 = 0.03195 0.00397 0.00358 0.00160 C6 1 0.17549 0.57912 -0.24409 11.00000 0.02350 0.03131 = 0.04284 0.00114 0.01035 0.00337 C7 1 0.18319 0.91133 0.08309 11.00000 0.02608 0.02213 = 0.02215 0.00161 0.00646 0.00160 C8 1 0.30496 0.86318 0.13570 11.00000 0.03085 0.02177 = 0.03729 0.00492 0.00234 0.00384 C9 1 0.43529 0.93949 0.16326 11.00000 0.02386 0.03467 = 0.03703 0.00372 -0.00024 0.00609 C10 1 0.44146 1.06031 0.13934 11.00000 0.02066 0.02929 = 0.02746 0.00095 0.00491 -0.00047 C11 1 0.31585 1.10180 0.08828 11.00000 0.02989 0.02034 = 0.04165 0.00442 0.00702 -0.00040 H1 2 0.08960 0.56594 -0.42266 11.00000 0.03232 H1A 2 -0.02054 0.88062 0.02020 11.00000 0.03179 H2 2 -0.12415 0.64145 -0.41295 11.00000 0.04823 H3 2 -0.15476 0.69489 -0.21690 11.00000 0.03032 H5 2 0.22109 0.60430 -0.05515 11.00000 0.02975 H6 2 0.26087 0.55184 -0.24652 11.00000 0.04501 H8 2 0.30013 0.78190 0.15404 11.00000 0.03226 H9 2 0.52301 0.91578 0.20201 11.00000 0.03868 H11 2 0.31798 1.18622 0.07494 11.00000 0.03526 S21 5 -0.48465 0.30396 0.47900 11.00000 0.02234 0.02570 = 0.02490 0.00530 0.00316 0.00356 CL21 6 0.09712 0.00155 0.71300 11.00000 0.02353 0.04029 = 0.04910 0.00412 -0.00305 0.00720 N21 3 -0.43545 0.16845 0.48187 11.00000 0.01932 0.02469 = 0.03016 0.00163 0.00103 0.00225 N22 3 -0.30680 0.01955 0.55500 11.00000 0.02264 0.02745 = 0.02823 -0.00090 0.00179 0.00524 O21 4 -0.62259 0.28385 0.39665 11.00000 0.02647 0.03223 = 0.02902 0.00524 -0.00200 0.00624 O22 4 -0.37060 0.39114 0.45619 11.00000 0.02893 0.03181 = 0.03449 0.01033 0.00887 0.00171 C21 1 -0.53870 0.38832 0.86499 11.00000 0.03466 0.03251 = 0.03032 -0.00441 0.00829 0.00628 C22 1 -0.64080 0.30353 0.78447 11.00000 0.02611 0.03061 = 0.03811 0.00046 0.01197 0.00194 C23 1 -0.62572 0.27920 0.66524 11.00000 0.02226 0.02617 = 0.03336 -0.00091 0.00340 0.00134 C24 1 -0.50740 0.34051 0.62878 11.00000 0.02032 0.02036 = 0.02692 0.00330 0.00324 0.00631 C25 1 -0.40571 0.42620 0.70864 11.00000 0.02148 0.02237 = 0.03525 0.00381 0.00250 0.00065 C26 1 -0.42214 0.44967 0.82813 11.00000 0.02959 0.02698 = 0.03328 -0.00436 -0.00069 0.00284 C27 1 -0.30299 0.13911 0.54242 11.00000 0.02140 0.02864 = 0.02173 0.00163 0.00676 0.00415 C28 1 -0.17970 0.22384 0.58518 11.00000 0.02585 0.02559 = 0.03818 0.00375 0.00418 0.00183 C29 1 -0.05493 0.18366 0.63815 11.00000 0.02227 0.03701 = 0.03550 0.00407 0.00367 -0.00198 C210 1 -0.05685 0.05953 0.64784 11.00000 0.02318 0.03298 = 0.02636 0.00240 0.00409 0.00536 C211 1 -0.18418 -0.01938 0.60708 11.00000 0.02625 0.02743 = 0.03160 0.00032 0.00169 0.00524 H21 2 -0.54848 0.40076 0.94086 11.00000 0.03477 H21A 2 -0.50158 0.11556 0.47390 11.00000 0.02587 H22 2 -0.71966 0.25942 0.80841 11.00000 0.04205 H23 2 -0.69479 0.22151 0.60747 11.00000 0.03188 H25 2 -0.32816 0.46744 0.68339 11.00000 0.02232 H26 2 -0.34942 0.51050 0.88156 11.00000 0.03695 H28 2 -0.18084 0.30241 0.58484 11.00000 0.03974 H29 2 0.03066 0.23909 0.66778 11.00000 0.02687 H211 2 -0.19023 -0.10382 0.61837 11.00000 0.03017 HKLF 4 Covalent radii and connectivity table for s92 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 CL 0.990 S1 - O2 O1 N1 C4 Cl1 - C10 O1 - S1 O2 - S1 N1 - C7 S1 N2 - C7 C11 C1 - C6 C2 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 S1 C5 - C6 C4 C6 - C1 C5 C7 - N2 C8 N1 C8 - C9 C7 C9 - C10 C8 C10 - C9 C11 Cl1 C11 - N2 C10 S21 - O21 O22 N21 C24 Cl21 - C210 N21 - C27 S21 N22 - C27 C211 O21 - S21 O22 - S21 C21 - C26 C22 C22 - C23 C21 C23 - C22 C24 C24 - C25 C23 S21 C25 - C24 C26 C26 - C21 C25 C27 - N22 C28 N21 C28 - C29 C27 C29 - C28 C210 C210 - C211 C29 Cl21 C211 - N22 C210 14032 Reflections read, of which 0 rejected -11 =< h =< 11, -13 =< k =< 12, -13 =< l =< 13, Max. 2-theta = 49.94 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -1 -9 10 2.86 0.87 3 6.08 1 Inconsistent equivalents 4016 Unique reflections, of which 0 suppressed R(int) = 0.0421 R(sigma) = 0.0430 Friedel opposites merged Maximum memory for data reduction = 2511 / 40534 Least-squares cycle 1 Maximum vector length = 511 Memory required = 3406 / 485145 wR2 = 0.0933 before cycle 1 for 4016 data and 379 / 379 parameters GooF = S = 1.054; Restrained GooF = 1.054 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0484 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.37779 0.00066 0.001 OSF Mean shift/esd = 0.006 Maximum = -0.070 for y S1 Max. shift = 0.000 A for H211 Max. dU = 0.000 for H21 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3406 / 485145 wR2 = 0.0933 before cycle 2 for 4016 data and 379 / 379 parameters GooF = S = 1.054; Restrained GooF = 1.054 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0484 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.37779 0.00066 0.000 OSF Mean shift/esd = 0.002 Maximum = -0.023 for z S21 Max. shift = 0.000 A for H11 Max. dU = 0.000 for H26 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3406 / 485145 wR2 = 0.0933 before cycle 3 for 4016 data and 379 / 379 parameters GooF = S = 1.054; Restrained GooF = 1.054 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0484 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.37779 0.00066 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H22 Max. dU = 0.000 for H26 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3406 / 485145 wR2 = 0.0933 before cycle 4 for 4016 data and 379 / 379 parameters GooF = S = 1.054; Restrained GooF = 1.054 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0484 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.37779 0.00066 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H21A Max. dU = 0.000 for H22 Largest correlation matrix elements 0.503 U11 H21A / U12 N21 s92 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S1 -0.00353 0.69594 0.02569 1.00000 0.02312 0.01915 0.02625 0.00392 0.00598 -0.00001 0.02302 0.00102 0.00005 0.00005 0.00004 0.00000 0.00028 0.00031 0.00028 0.00021 0.00022 0.00022 0.00015 Cl1 0.60256 1.15994 0.17130 1.00000 0.02412 0.04091 0.04558 0.00339 0.00433 -0.00642 0.03855 0.00113 0.00006 0.00006 0.00005 0.00000 0.00030 0.00039 0.00035 0.00027 0.00025 0.00026 0.00018 O1 -0.15557 0.67660 0.01661 1.00000 0.02411 0.02633 0.03565 0.00383 0.01129 -0.00074 0.02843 0.00297 0.00015 0.00014 0.00013 0.00000 0.00076 0.00090 0.00082 0.00065 0.00065 0.00065 0.00035 O2 0.08785 0.63835 0.11473 1.00000 0.03266 0.02387 0.02906 0.00789 0.00323 0.00284 0.02901 0.00299 0.00016 0.00014 0.00013 0.00000 0.00084 0.00088 0.00078 0.00063 0.00065 0.00068 0.00036 N1 0.04330 0.84421 0.05353 1.00000 0.02239 0.01790 0.03332 0.00149 0.00275 0.00308 0.02509 0.00355 0.00019 0.00017 0.00016 0.00000 0.00096 0.00102 0.00101 0.00077 0.00081 0.00081 0.00042 N2 0.18850 1.02850 0.06011 1.00000 0.02110 0.02052 0.03489 0.00467 0.00445 0.00063 0.02594 0.00350 0.00018 0.00016 0.00016 0.00000 0.00092 0.00105 0.00099 0.00077 0.00077 0.00077 0.00041 C1 0.07406 0.58965 -0.34790 1.00000 0.03527 0.03645 0.03032 -0.00329 0.01218 -0.00145 0.03425 0.00478 0.00025 0.00023 0.00022 0.00000 0.00134 0.00150 0.00126 0.00104 0.00109 0.00110 0.00056 C2 -0.05210 0.63244 -0.33902 1.00000 0.03071 0.04352 0.02872 0.00265 0.00265 0.00353 0.03516 0.00488 0.00025 0.00024 0.00021 0.00000 0.00128 0.00161 0.00121 0.00104 0.00103 0.00112 0.00058 C3 -0.07602 0.66643 -0.22482 1.00000 0.02125 0.03097 0.03266 0.00300 0.00439 0.00573 0.02836 0.00448 0.00024 0.00022 0.00020 0.00000 0.00113 0.00137 0.00121 0.00096 0.00096 0.00100 0.00051 C4 0.02735 0.65578 -0.12043 1.00000 0.02047 0.01714 0.02736 0.00366 0.00543 -0.00220 0.02209 0.00401 0.00021 0.00019 0.00018 0.00000 0.00103 0.00113 0.00106 0.00083 0.00086 0.00085 0.00045 C5 0.15307 0.61187 -0.12864 1.00000 0.02206 0.02501 0.03195 0.00397 0.00358 0.00160 0.02685 0.00442 0.00023 0.00020 0.00020 0.00000 0.00110 0.00127 0.00119 0.00093 0.00096 0.00094 0.00050 C6 0.17549 0.57912 -0.24409 1.00000 0.02350 0.03131 0.04284 0.00114 0.01035 0.00337 0.03229 0.00474 0.00025 0.00023 0.00021 0.00000 0.00116 0.00142 0.00139 0.00105 0.00105 0.00103 0.00055 C7 0.18319 0.91133 0.08309 1.00000 0.02608 0.02213 0.02215 0.00161 0.00646 0.00160 0.02353 0.00412 0.00022 0.00020 0.00018 0.00000 0.00112 0.00124 0.00103 0.00084 0.00088 0.00092 0.00047 C8 0.30496 0.86318 0.13570 1.00000 0.03085 0.02177 0.03729 0.00492 0.00234 0.00384 0.03069 0.00465 0.00024 0.00022 0.00020 0.00000 0.00125 0.00134 0.00128 0.00100 0.00100 0.00103 0.00053 C9 0.43529 0.93949 0.16326 1.00000 0.02386 0.03467 0.03703 0.00372 -0.00024 0.00609 0.03273 0.00468 0.00024 0.00023 0.00021 0.00000 0.00119 0.00147 0.00129 0.00103 0.00101 0.00104 0.00055 C10 0.44146 1.06031 0.13934 1.00000 0.02066 0.02929 0.02746 0.00095 0.00491 -0.00047 0.02638 0.00425 0.00022 0.00021 0.00019 0.00000 0.00107 0.00136 0.00110 0.00092 0.00088 0.00094 0.00050 C11 0.31585 1.10180 0.08828 1.00000 0.02989 0.02034 0.04165 0.00442 0.00702 -0.00040 0.03113 0.00464 0.00024 0.00022 0.00021 0.00000 0.00126 0.00132 0.00133 0.00100 0.00103 0.00102 0.00053 H1 0.08960 0.56594 -0.42266 1.00000 0.03232 0.04684 0.00242 0.00218 0.00209 0.00000 0.00627 H1A -0.02054 0.88062 0.02020 1.00000 0.03179 0.04855 0.00260 0.00225 0.00210 0.00000 0.00669 H2 -0.12415 0.64145 -0.41295 1.00000 0.04823 0.05393 0.00283 0.00245 0.00233 0.00000 0.00732 H3 -0.15476 0.69489 -0.21690 1.00000 0.03032 0.04571 0.00250 0.00215 0.00196 0.00000 0.00625 H5 0.22109 0.60430 -0.05515 1.00000 0.02975 0.04697 0.00241 0.00208 0.00201 0.00000 0.00594 H6 0.26087 0.55184 -0.24652 1.00000 0.04501 0.04989 0.00271 0.00245 0.00208 0.00000 0.00732 H8 0.30013 0.78190 0.15404 1.00000 0.03226 0.04767 0.00245 0.00240 0.00200 0.00000 0.00632 H9 0.52301 0.91578 0.20201 1.00000 0.03868 0.04948 0.00267 0.00228 0.00208 0.00000 0.00660 H11 0.31798 1.18622 0.07494 1.00000 0.03526 0.04898 0.00253 0.00246 0.00202 0.00000 0.00646 S21 -0.48465 0.30396 0.47900 1.00000 0.02234 0.02570 0.02490 0.00530 0.00316 0.00356 0.02452 0.00106 0.00005 0.00005 0.00004 0.00000 0.00028 0.00033 0.00028 0.00022 0.00022 0.00023 0.00015 Cl21 0.09712 0.00155 0.71300 1.00000 0.02353 0.04029 0.04910 0.00412 -0.00305 0.00720 0.03907 0.00119 0.00006 0.00006 0.00006 0.00000 0.00029 0.00038 0.00036 0.00027 0.00025 0.00025 0.00018 N21 -0.43545 0.16845 0.48187 1.00000 0.01932 0.02469 0.03016 0.00163 0.00103 0.00225 0.02554 0.00396 0.00021 0.00019 0.00016 0.00000 0.00096 0.00113 0.00100 0.00079 0.00078 0.00089 0.00042 N22 -0.30680 0.01955 0.55500 1.00000 0.02264 0.02745 0.02823 -0.00090 0.00179 0.00524 0.02669 0.00349 0.00018 0.00017 0.00015 0.00000 0.00093 0.00113 0.00094 0.00077 0.00076 0.00080 0.00042 O21 -0.62259 0.28385 0.39665 1.00000 0.02647 0.03223 0.02902 0.00524 -0.00200 0.00624 0.03019 0.00295 0.00015 0.00014 0.00013 0.00000 0.00080 0.00095 0.00079 0.00066 0.00064 0.00070 0.00037 O22 -0.37060 0.39114 0.45619 1.00000 0.02893 0.03181 0.03449 0.01033 0.00887 0.00171 0.03148 0.00311 0.00016 0.00015 0.00013 0.00000 0.00081 0.00095 0.00083 0.00068 0.00067 0.00070 0.00037 C21 -0.53870 0.38832 0.86499 1.00000 0.03466 0.03251 0.03032 -0.00441 0.00829 0.00628 0.03253 0.00475 0.00025 0.00023 0.00022 0.00000 0.00131 0.00144 0.00126 0.00101 0.00105 0.00109 0.00055 C22 -0.64080 0.30353 0.78447 1.00000 0.02611 0.03061 0.03811 0.00046 0.01197 0.00194 0.03125 0.00474 0.00025 0.00023 0.00021 0.00000 0.00119 0.00141 0.00130 0.00102 0.00104 0.00106 0.00053 C23 -0.62572 0.27920 0.66524 1.00000 0.02226 0.02617 0.03336 -0.00091 0.00340 0.00134 0.02807 0.00461 0.00023 0.00022 0.00020 0.00000 0.00109 0.00129 0.00121 0.00097 0.00096 0.00096 0.00050 C24 -0.50740 0.34051 0.62878 1.00000 0.02032 0.02036 0.02692 0.00330 0.00324 0.00631 0.02247 0.00412 0.00021 0.00019 0.00018 0.00000 0.00102 0.00118 0.00106 0.00085 0.00086 0.00088 0.00046 C25 -0.40571 0.42620 0.70864 1.00000 0.02148 0.02237 0.03525 0.00381 0.00250 0.00065 0.02717 0.00437 0.00024 0.00021 0.00020 0.00000 0.00112 0.00126 0.00123 0.00095 0.00097 0.00097 0.00050 C26 -0.42214 0.44967 0.82813 1.00000 0.02959 0.02698 0.03328 -0.00436 -0.00069 0.00284 0.03154 0.00461 0.00025 0.00022 0.00021 0.00000 0.00122 0.00136 0.00123 0.00101 0.00102 0.00106 0.00054 C27 -0.30299 0.13911 0.54242 1.00000 0.02140 0.02864 0.02173 0.00163 0.00676 0.00415 0.02364 0.00416 0.00021 0.00020 0.00018 0.00000 0.00106 0.00134 0.00102 0.00087 0.00085 0.00093 0.00047 C28 -0.17970 0.22384 0.58518 1.00000 0.02585 0.02559 0.03818 0.00375 0.00418 0.00183 0.03050 0.00466 0.00024 0.00023 0.00021 0.00000 0.00118 0.00144 0.00130 0.00103 0.00098 0.00102 0.00053 C29 -0.05493 0.18366 0.63815 1.00000 0.02227 0.03701 0.03550 0.00407 0.00367 -0.00198 0.03263 0.00486 0.00024 0.00024 0.00021 0.00000 0.00118 0.00153 0.00127 0.00105 0.00100 0.00108 0.00055 C210 -0.05685 0.05953 0.64784 1.00000 0.02318 0.03298 0.02636 0.00240 0.00409 0.00536 0.02764 0.00437 0.00023 0.00021 0.00019 0.00000 0.00111 0.00143 0.00111 0.00094 0.00090 0.00099 0.00051 C211 -0.18418 -0.01938 0.60708 1.00000 0.02625 0.02743 0.03160 0.00032 0.00169 0.00524 0.02912 0.00450 0.00023 0.00023 0.00020 0.00000 0.00118 0.00141 0.00119 0.00098 0.00095 0.00103 0.00052 H21 -0.54848 0.40076 0.94086 1.00000 0.03477 0.04928 0.00255 0.00227 0.00222 0.00000 0.00657 H21A -0.50158 0.11556 0.47390 1.00000 0.02587 0.05020 0.00263 0.00230 0.00207 0.00000 0.00688 H22 -0.71966 0.25942 0.80841 1.00000 0.04205 0.05270 0.00282 0.00250 0.00215 0.00000 0.00712 H23 -0.69479 0.22151 0.60747 1.00000 0.03188 0.04920 0.00249 0.00224 0.00201 0.00000 0.00609 H25 -0.32816 0.46745 0.68339 1.00000 0.02232 0.04439 0.00239 0.00209 0.00183 0.00000 0.00567 H26 -0.34942 0.51050 0.88156 1.00000 0.03695 0.05238 0.00262 0.00237 0.00208 0.00000 0.00652 H28 -0.18084 0.30241 0.58484 1.00000 0.03974 0.05191 0.00268 0.00256 0.00214 0.00000 0.00726 H29 0.03066 0.23909 0.66778 1.00000 0.02687 0.04851 0.00253 0.00218 0.00190 0.00000 0.00583 H211 -0.19023 -0.10382 0.61837 1.00000 0.03017 0.04672 0.00241 0.00236 0.00195 0.00000 0.00620 Final Structure Factor Calculation for s92 in P-1 Total number of l.s. parameters = 379 Maximum vector length = 511 Memory required = 3027 / 25039 wR2 = 0.0933 before cycle 5 for 4016 data and 0 / 379 parameters GooF = S = 1.054; Restrained GooF = 1.054 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0484 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0366 for 3239 Fo > 4sig(Fo) and 0.0501 for all 4016 data wR2 = 0.0933, GooF = S = 1.054, Restrained GooF = 1.054 for all data Occupancy sum of asymmetric unit = 34.00 for non-hydrogen and 18.00 for hydrogen atoms Principal mean square atomic displacements U 0.0269 0.0254 0.0167 S1 0.0507 0.0452 0.0198 Cl1 0.0367 0.0303 0.0184 O1 0.0383 0.0289 0.0198 O2 0.0353 0.0221 0.0179 N1 0.0362 0.0235 0.0181 N2 0.0476 0.0297 0.0255 C1 0.0444 0.0347 0.0264 C2 0.0334 0.0310 0.0206 C3 0.0281 0.0249 0.0133 C4 0.0338 0.0255 0.0212 C5 0.0436 0.0312 0.0221 C6 0.0276 0.0218 0.0212 C7 0.0420 0.0289 0.0211 C8 0.0420 0.0347 0.0215 C9 0.0322 0.0276 0.0194 C10 0.0423 0.0324 0.0187 C11 0.0293 0.0234 0.0208 S21 0.0564 0.0403 0.0205 Cl21 0.0330 0.0252 0.0185 N21 0.0336 0.0251 0.0213 N22 0.0386 0.0324 0.0196 O21 0.0408 0.0313 0.0223 O22 0.0395 0.0347 0.0233 C21 0.0407 0.0302 0.0228 C22 0.0358 0.0275 0.0210 C23 0.0280 0.0230 0.0164 C24 0.0377 0.0243 0.0195 C25 0.0429 0.0303 0.0215 C26 0.0288 0.0232 0.0189 C27 0.0399 0.0278 0.0238 C28 0.0422 0.0351 0.0206 C29 0.0331 0.0272 0.0226 C210 0.0364 0.0267 0.0243 C211 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 0.050 0.065 0.083 0.105 0.134 0.190 1.000 Number in group 423. 408. 407. 374. 407. 412. 379. 404. 399. 403. GooF 0.877 0.980 1.069 1.079 1.192 1.086 1.073 0.938 1.059 1.160 K 1.391 0.951 0.931 0.949 0.955 0.966 0.985 1.007 1.029 1.008 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.15 1.26 1.44 1.81 inf Number in group 406. 400. 416. 392. 394. 418. 388. 402. 395. 405. GooF 0.933 0.968 0.939 0.984 1.020 0.979 0.947 0.931 1.212 1.494 K 1.001 0.993 0.994 1.015 1.018 1.031 1.044 1.031 1.025 0.973 R1 0.111 0.103 0.077 0.061 0.052 0.039 0.034 0.031 0.035 0.036 Recommended weighting scheme: WGHT 0.0484 0.2730 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 0 2 111.37 160.54 4.81 0.077 4.00 3 3 1 105.94 72.39 4.32 0.052 2.07 -4 1 2 145.77 110.39 3.83 0.064 2.34 2 0 4 965.40 1217.68 3.67 0.213 2.15 3 4 2 143.13 102.54 3.61 0.062 1.69 -4 -1 3 51.53 75.61 3.60 0.053 2.11 -5 2 1 133.92 172.12 3.52 0.080 1.89 2 -3 2 37.23 24.70 3.47 0.030 2.63 0 1 0 548.60 717.01 3.47 0.164 10.91 0 0 1 31.95 59.21 3.43 0.047 10.87 3 -3 1 23.18 36.37 3.42 0.037 2.44 4 -2 2 95.30 124.12 3.41 0.068 1.98 1 -3 5 104.69 135.76 3.41 0.071 1.86 -3 4 1 102.04 74.86 3.36 0.053 2.22 -9 6 7 40.54 1.26 3.33 0.007 0.89 2 1 4 75.64 103.51 3.20 0.062 2.05 3 0 1 1046.77 1249.67 3.18 0.216 2.82 -6 8 1 44.57 64.70 3.16 0.049 1.12 -1 2 3 295.32 242.94 3.14 0.095 3.00 1 2 3 1244.90 1484.64 3.12 0.235 2.58 -4 3 10 70.74 94.94 3.12 0.060 1.03 -3 -1 3 435.06 532.70 3.11 0.141 2.55 -1 -2 3 290.73 229.22 3.07 0.092 3.08 -5 2 9 48.39 72.16 3.04 0.052 1.11 0 5 1 49.47 33.45 2.98 0.035 2.10 -3 -7 2 75.19 108.60 2.96 0.064 1.33 1 0 3 3160.34 3753.49 2.96 0.374 3.15 2 10 0 16.03 43.67 2.95 0.040 1.03 -4 3 0 43.40 31.43 2.92 0.034 2.12 0 -2 4 18.32 28.88 2.91 0.033 2.53 0 2 0 422.36 508.44 2.91 0.138 5.46 1 -1 3 710.70 835.83 2.91 0.177 3.14 -5 4 1 55.34 73.36 2.85 0.052 1.68 -4 -11 2 131.02 217.57 2.84 0.090 0.88 7 -5 8 9.79 51.45 2.79 0.044 0.85 -3 3 9 180.75 219.63 2.79 0.091 1.15 4 -1 2 81.36 60.93 2.78 0.048 2.02 3 -6 2 124.53 99.85 2.77 0.061 1.60 2 0 2 4.92 0.11 2.75 0.002 3.20 -1 -6 9 1686.41 1447.52 2.73 0.232 1.06 -7 11 1 30.30 53.73 2.72 0.045 0.87 -5 3 0 96.67 119.29 2.70 0.067 1.78 2 -1 2 1948.09 2253.63 2.69 0.290 3.22 2 4 1 414.22 489.91 2.68 0.135 2.09 7 -7 1 74.66 97.26 2.68 0.060 1.08 0 9 0 40.84 61.71 2.67 0.048 1.21 5 1 2 240.87 202.17 2.66 0.087 1.59 -1 -5 2 394.41 329.76 2.65 0.111 2.01 -6 4 4 52.56 70.21 2.64 0.051 1.37 -1 1 0 727.85 843.49 2.62 0.177 7.71 Bond lengths and angles S1 - Distance Angles O2 1.4273 (0.0015) O1 1.4322 (0.0015) 120.24 (0.10) N1 1.6323 (0.0019) 108.52 (0.10) 104.09 (0.10) C4 1.7616 (0.0021) 108.26 (0.09) 107.98 (0.09) 107.05 (0.10) S1 - O2 O1 N1 Cl1 - Distance Angles C10 1.7291 (0.0023) Cl1 - O1 - Distance Angles S1 1.4322 (0.0015) O1 - O2 - Distance Angles S1 1.4273 (0.0015) O2 - N1 - Distance Angles C7 1.4068 (0.0028) S1 1.6323 (0.0019) 127.66 (0.15) N1 - C7 N2 - Distance Angles C7 1.3327 (0.0028) C11 1.3376 (0.0029) 118.57 (0.18) N2 - C7 C1 - Distance Angles C6 1.3730 (0.0032) C2 1.3870 (0.0033) 120.71 (0.22) C1 - C6 C2 - Distance Angles C3 1.3827 (0.0032) C1 1.3870 (0.0033) 120.00 (0.22) C2 - C3 C3 - Distance Angles C2 1.3827 (0.0032) C4 1.3882 (0.0029) 118.86 (0.20) C3 - C2 C4 - Distance Angles C5 1.3870 (0.0029) C3 1.3882 (0.0029) 121.41 (0.20) S1 1.7616 (0.0021) 119.31 (0.16) 119.27 (0.16) C4 - C5 C3 C5 - Distance Angles C6 1.3870 (0.0031) C4 1.3870 (0.0029) 118.83 (0.20) C5 - C6 C6 - Distance Angles C1 1.3730 (0.0032) C5 1.3870 (0.0031) 120.18 (0.21) C6 - C1 C7 - Distance Angles N2 1.3327 (0.0028) C8 1.3904 (0.0029) 122.32 (0.20) N1 1.4068 (0.0027) 113.52 (0.18) 124.12 (0.20) C7 - N2 C8 C8 - Distance Angles C9 1.3756 (0.0034) C7 1.3904 (0.0029) 118.41 (0.22) C8 - C9 C9 - Distance Angles C10 1.3744 (0.0034) C8 1.3756 (0.0034) 119.51 (0.21) C9 - C10 C10 - Distance Angles C9 1.3744 (0.0034) C11 1.3792 (0.0031) 118.78 (0.21) Cl1 1.7291 (0.0023) 121.40 (0.17) 119.82 (0.18) C10 - C9 C11 C11 - Distance Angles N2 1.3376 (0.0029) C10 1.3792 (0.0031) 122.41 (0.22) C11 - N2 S21 - Distance Angles O21 1.4290 (0.0015) O22 1.4313 (0.0017) 120.43 (0.09) N21 1.6366 (0.0020) 104.25 (0.10) 109.19 (0.10) C24 1.7628 (0.0021) 108.44 (0.09) 108.38 (0.10) 105.08 (0.10) S21 - O21 O22 N21 Cl21 - Distance Angles C210 1.7374 (0.0021) Cl21 - N21 - Distance Angles C27 1.4055 (0.0026) S21 1.6366 (0.0020) 127.30 (0.17) N21 - C27 N22 - Distance Angles C27 1.3351 (0.0029) C211 1.3445 (0.0027) 118.17 (0.20) N22 - C27 O21 - Distance Angles S21 1.4290 (0.0015) O21 - O22 - Distance Angles S21 1.4313 (0.0017) O22 - C21 - Distance Angles C26 1.3794 (0.0035) C22 1.3871 (0.0034) 121.09 (0.22) C21 - C26 C22 - Distance Angles C23 1.3840 (0.0032) C21 1.3871 (0.0034) 119.75 (0.23) C22 - C23 C23 - Distance Angles C22 1.3840 (0.0032) C24 1.3908 (0.0031) 118.96 (0.21) C23 - C22 C24 - Distance Angles C25 1.3873 (0.0031) C23 1.3908 (0.0031) 121.49 (0.20) S21 1.7628 (0.0021) 119.79 (0.17) 118.68 (0.16) C24 - C25 C23 C25 - Distance Angles C24 1.3873 (0.0031) C26 1.3898 (0.0032) 118.93 (0.22) C25 - C24 C26 - Distance Angles C21 1.3794 (0.0035) C25 1.3898 (0.0032) 119.77 (0.22) C26 - C21 C27 - Distance Angles N22 1.3351 (0.0029) C28 1.3829 (0.0033) 122.46 (0.19) N21 1.4055 (0.0026) 113.22 (0.19) 124.33 (0.21) C27 - N22 C28 C28 - Distance Angles C29 1.3710 (0.0031) C27 1.3829 (0.0033) 119.09 (0.23) C28 - C29 C29 - Distance Angles C28 1.3710 (0.0031) C210 1.3823 (0.0034) 118.79 (0.23) C29 - C28 C210 - Distance Angles C211 1.3749 (0.0033) C29 1.3823 (0.0034) 119.15 (0.20) Cl21 1.7374 (0.0021) 119.36 (0.18) 121.47 (0.18) C210 - C211 C29 C211 - Distance Angles N22 1.3445 (0.0027) C210 1.3749 (0.0033) 122.27 (0.22) C211 - N22 FMAP and GRID set by program FMAP 2 1 23 GRID -2.500 -2 -2 2.500 2 2 R1 = 0.0498 for 4016 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.35 at 0.1048 0.1616 0.6751 [ 1.19 A from H29 ] Deepest hole -0.41 at 0.4668 0.2434 0.4920 [ 0.80 A from S21 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2910 / 21233 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1048 0.1616 0.6751 1.00000 0.05 0.35 1.19 H29 1.57 C29 1.75 C210 1.84 CL21 Q2 1 0.6006 0.9997 0.2141 1.00000 0.05 0.29 1.09 H9 1.61 C9 1.82 C10 1.86 CL1 Q3 1 0.3785 1.0624 0.0832 1.00000 0.05 0.23 0.78 C10 0.80 C11 1.56 H11 1.76 C9 Q4 1 -0.2142 0.5257 0.6321 1.00000 0.05 0.22 1.43 H25 1.61 H2 1.78 C2 2.23 C3 Q5 1 0.7296 1.1243 0.2474 1.00000 0.05 0.20 1.46 CL1 2.31 CL21 2.76 C10 2.77 H9 Q6 1 0.1263 0.7802 -0.2598 1.00000 0.05 0.20 2.19 C2 2.22 C1 2.28 C3 2.35 C6 Q7 1 0.0851 0.5531 -0.2833 1.00000 0.05 0.19 0.84 C1 0.89 C6 1.58 H1 1.66 H6 Q8 1 -0.5021 0.3293 0.5747 1.00000 0.05 0.19 0.62 C24 1.14 S21 1.77 C23 1.79 C25 Q9 1 -0.1494 0.6126 0.0235 1.00000 0.05 0.19 0.73 O1 1.56 S1 2.27 O2 2.32 H26 Q10 1 -0.2963 0.6638 -0.0591 1.00000 0.05 0.19 1.42 O1 1.72 H11 1.75 H26 2.26 H21 Shortest distances between peaks (including symmetry equivalents) 5 6 1.60 2 5 1.69 9 10 1.71 6 7 2.48 2 3 2.54 4 7 2.81 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. 1.16: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.05: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 6.94: Structure factors and derivatives 33.98: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 3.79: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.55: Analysis of variance 0.28: Merge reflections for Fourier and .fcf 0.27: Fourier summations 0.16: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 12:01:46 Total elapsed time: 47.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++