+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + dw9810 started at 14:21:37 on 30-Jul-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL dw9710 in P-1 CELL 0.71069 9.725 14.576 8.545 93.58 90.85 103.34 ZERR 2 0.003 0.004 0.004 0.03 0.04 0.02 LATT 1 SFAC C H N S AS UNIT 42 36 8 8 4 V = 1175.75 F(000) = 604.0 Mu = 3.21 mm-1 Cell Wt = 1208.95 Rho = 1.707 L.S. 3 TEMP -93 SHEL 5.8 0 SIZE 0.30 0.20 0.15 LIST 4 CONF BOND $H FMAP 2 PLAN -10 WGHT 0.029100 FVAR 0.25081 AS1 5 0.50437 0.39380 0.12009 11.00000 0.02168 0.02139 = 0.02306 0.00185 -0.00030 0.00335 AS2 5 0.63543 0.20450 0.17159 11.00000 0.02002 0.02210 = 0.02698 0.00372 0.00091 0.00269 S1 4 0.29829 0.28356 0.14255 11.00000 0.02320 0.02852 = 0.03275 -0.00086 0.00073 0.00011 S2 4 0.51495 0.31911 -0.11872 11.00000 0.03162 0.03090 = 0.02276 -0.00039 -0.00186 0.00096 S3 4 0.75291 0.17236 0.38661 11.00000 0.01921 0.03561 = 0.03204 0.01084 0.00026 0.00450 S4 4 0.84111 0.24830 0.04508 11.00000 0.02600 0.02548 = 0.03434 0.00376 0.00711 0.00069 N1 3 0.36638 0.38680 0.41048 11.00000 0.02369 0.02970 = 0.03269 0.00058 0.00415 0.00374 N2 3 0.73725 0.46160 -0.05909 11.00000 0.02732 0.02558 = 0.02344 0.00494 -0.00014 0.00530 N3 3 0.48468 0.16142 0.45067 11.00000 0.02566 0.03354 = 0.03304 0.01115 0.00047 0.00562 N4 3 0.76130 0.06027 -0.00491 11.00000 0.02900 0.02921 = 0.02940 0.00467 -0.00053 0.00453 C1 1 0.26273 0.32293 0.33287 11.00000 0.02221 0.02677 = 0.02928 0.00345 0.00167 0.00656 C2 1 0.13232 0.28755 0.39822 11.00000 0.01865 0.03092 = 0.04074 0.00874 0.00130 0.00339 AFIX 43 H2 2 0.05999 0.24347 0.33918 11.00000 -1.20000 AFIX 0 C3 1 0.11015 0.31723 0.54835 11.00000 0.02647 0.04439 = 0.03947 0.01685 0.01421 0.01111 AFIX 43 H3 2 0.02198 0.29419 0.59521 11.00000 -1.20000 AFIX 0 C4 1 0.21795 0.38147 0.63179 11.00000 0.04052 0.05321 = 0.02745 0.00621 0.00302 0.01170 AFIX 43 H4 2 0.20610 0.40200 0.73740 11.00000 -1.20000 AFIX 0 C5 1 0.34259 0.41469 0.55747 11.00000 0.03660 0.03818 = 0.03400 -0.00197 0.00331 0.00969 AFIX 43 H5 2 0.41552 0.45985 0.61374 11.00000 -1.20000 AFIX 0 C6 1 0.67389 0.39602 -0.16875 11.00000 0.02848 0.02827 = 0.02721 0.00829 0.00044 0.01030 C7 1 0.72725 0.38493 -0.31695 11.00000 0.04610 0.03696 = 0.02371 0.00072 0.00349 0.01192 AFIX 43 H7 2 0.67894 0.33695 -0.39179 11.00000 -1.20000 AFIX 0 C8 1 0.85096 0.44496 -0.35175 11.00000 0.03957 0.04966 = 0.03588 0.01756 0.01465 0.01993 AFIX 43 H8 2 0.88996 0.43933 -0.45220 11.00000 -1.20000 AFIX 0 C9 1 0.91962 0.51405 -0.24065 11.00000 0.02208 0.03986 = 0.04379 0.01471 0.00797 0.00610 AFIX 43 H9 2 1.00664 0.55587 -0.26227 11.00000 -1.20000 AFIX 0 C10 1 0.85771 0.52024 -0.09762 11.00000 0.03004 0.03488 = 0.03306 0.00743 0.00298 0.00919 AFIX 43 H10 2 0.90295 0.56880 -0.02205 11.00000 -1.20000 AFIX 0 C11 1 0.60403 0.13914 0.50156 11.00000 0.02084 0.01935 = 0.02726 0.00206 -0.00250 -0.00189 C12 1 0.61092 0.09205 0.63766 11.00000 0.03089 0.03096 = 0.03128 0.00583 -0.00501 0.00841 AFIX 43 H12 2 0.69647 0.07675 0.66953 11.00000 -1.20000 AFIX 0 C13 1 0.49308 0.06841 0.72392 11.00000 0.03453 0.03601 = 0.02845 0.01007 -0.00096 0.00242 AFIX 43 H13 2 0.49529 0.03637 0.81706 11.00000 -1.20000 AFIX 0 C14 1 0.36926 0.09166 0.67428 11.00000 0.02940 0.04212 = 0.03778 0.00909 0.00858 0.00674 AFIX 43 H14 2 0.28561 0.07618 0.73261 11.00000 -1.20000 AFIX 0 C15 1 0.37143 0.13737 0.53937 11.00000 0.01944 0.03963 = 0.04205 0.00929 -0.00111 0.00673 AFIX 43 H15 2 0.28665 0.15319 0.50615 11.00000 -1.20000 AFIX 0 C16 1 0.85527 0.13749 -0.04047 11.00000 0.02340 0.02968 = 0.02289 0.00483 -0.00395 0.00813 C17 1 0.96382 0.13506 -0.14486 11.00000 0.02280 0.04183 = 0.03605 0.00515 0.00446 0.00639 AFIX 43 H17 2 1.03070 0.19124 -0.16601 11.00000 -1.20000 AFIX 0 C18 1 0.97126 0.04912 -0.21620 11.00000 0.02779 0.05967 = 0.04382 -0.00772 0.00665 0.01679 AFIX 43 H18 2 1.04304 0.04527 -0.28885 11.00000 -1.20000 AFIX 0 C19 1 0.87359 -0.03151 -0.18139 11.00000 0.04362 0.03722 = 0.04226 -0.01055 -0.00481 0.01599 AFIX 43 H19 2 0.87712 -0.09161 -0.22878 11.00000 -1.20000 AFIX 0 C20 1 0.77107 -0.02236 -0.07620 11.00000 0.04147 0.02785 = 0.03470 0.00076 -0.00361 0.01037 AFIX 43 H20 2 0.70347 -0.07772 -0.05284 11.00000 -1.20000 AFIX 0 C21 1 0.63394 0.33628 0.23942 11.00000 0.02424 0.02337 = 0.02354 0.00557 -0.00036 0.00436 AFIX 23 H21A 2 0.60859 0.33846 0.35114 11.00000 -1.20000 H21B 2 0.73107 0.37558 0.23249 11.00000 -1.20000 HKLF 4 Covalent radii and connectivity table for dw9710 in P-1 C 0.770 H 0.320 N 0.700 S 1.030 AS 1.210 As1 - C21 S2 S1 As2 - C21 S4 S3 S1 - C1 As1 S2 - C6 As1 S3 - C11 As2 S4 - C16 As2 N1 - C5 C1 N2 - C6 C10 N3 - C15 C11 N4 - C16 C20 C1 - N1 C2 S1 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 C5 - N1 C4 C6 - N2 C7 S2 C7 - C8 C6 C8 - C7 C9 C9 - C10 C8 C10 - N2 C9 C11 - N3 C12 S3 C12 - C13 C11 C13 - C12 C14 C14 - C15 C13 C15 - N3 C14 C16 - N4 C17 S4 C17 - C18 C16 C18 - C17 C19 C19 - C20 C18 C20 - N4 C19 C21 - As1 As2 5669 Reflections read, of which 12 rejected 0 =< h =< 12, -18 =< k =< 18, -11 =< l =< 10, Max. 2-theta = 55.09 0 Systematic absence violations 0 Inconsistent equivalents 5345 Unique reflections, of which 0 suppressed R(int) = 0.0453 R(sigma) = 0.0800 Friedel opposites merged Maximum memory for data reduction = 2852 / 53423 Default effective X-H distances for T = -93.0 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 = 3612 / 350077 wR2 = 0.1027 before cycle 1 for 5345 data and 280 / 280 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0291 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25081 0.00034 0.001 OSF Mean shift/esd = 0.004 Maximum = 0.097 for y As1 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C11 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3612 / 350077 wR2 = 0.1027 before cycle 2 for 5345 data and 280 / 280 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0291 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25081 0.00034 0.001 OSF Mean shift/esd = 0.001 Maximum = 0.033 for y As1 Max. shift = 0.000 A for C21 Max. dU = 0.000 for C11 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3612 / 350077 wR2 = 0.1027 before cycle 3 for 5345 data and 280 / 280 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0291 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25081 0.00034 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for y As1 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C9 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 4 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.0600 0.2435 0.3392 43 0.950 0.000 C2 C3 C1 H3 0.0220 0.2942 0.5952 43 0.950 0.000 C3 C2 C4 H4 0.2061 0.4020 0.7374 43 0.950 0.000 C4 C5 C3 H5 0.4155 0.4598 0.6137 43 0.950 0.000 C5 N1 C4 H7 0.6789 0.3369 -0.3918 43 0.950 0.000 C7 C8 C6 H8 0.8900 0.4393 -0.4522 43 0.950 0.000 C8 C7 C9 H9 1.0066 0.5559 -0.2623 43 0.950 0.000 C9 C10 C8 H10 0.9029 0.5688 -0.0221 43 0.950 0.000 C10 N2 C9 H12 0.6965 0.0768 0.6695 43 0.950 0.000 C12 C13 C11 H13 0.4953 0.0364 0.8171 43 0.950 0.000 C13 C12 C14 H14 0.2856 0.0762 0.7326 43 0.950 0.000 C14 C15 C13 H15 0.2867 0.1532 0.5062 43 0.950 0.000 C15 N3 C14 H17 1.0307 0.1912 -0.1660 43 0.950 0.000 C17 C18 C16 H18 1.0430 0.0453 -0.2889 43 0.950 0.000 C18 C17 C19 H19 0.8771 -0.0916 -0.2288 43 0.950 0.000 C19 C20 C18 H20 0.7035 -0.0777 -0.0528 43 0.950 0.000 C20 N4 C19 H21A 0.6086 0.3385 0.3511 23 0.990 0.000 C21 As1 As2 H21B 0.7311 0.3756 0.2325 23 0.990 0.000 C21 As1 As2 dw9710 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq As1 0.50437 0.39380 0.12009 1.00000 0.02168 0.02139 0.02306 0.00185 -0.00030 0.00335 0.02231 0.00084 0.00005 0.00003 0.00005 0.00000 0.00024 0.00022 0.00023 0.00017 0.00017 0.00018 0.00012 As2 0.63543 0.20450 0.17159 1.00000 0.02002 0.02210 0.02698 0.00372 0.00091 0.00269 0.02330 0.00085 0.00005 0.00003 0.00005 0.00000 0.00024 0.00022 0.00024 0.00018 0.00018 0.00018 0.00012 S1 0.29829 0.28356 0.14255 1.00000 0.02320 0.02852 0.03275 -0.00086 0.00073 0.00011 0.02924 0.00220 0.00012 0.00008 0.00014 0.00000 0.00058 0.00058 0.00061 0.00047 0.00047 0.00047 0.00026 S2 0.51495 0.31911 -0.11872 1.00000 0.03162 0.03090 0.02276 -0.00039 -0.00186 0.00096 0.02957 0.00220 0.00013 0.00008 0.00013 0.00000 0.00064 0.00058 0.00054 0.00045 0.00046 0.00050 0.00026 S3 0.75291 0.17236 0.38661 1.00000 0.01921 0.03561 0.03204 0.01084 0.00026 0.00450 0.02890 0.00230 0.00012 0.00008 0.00013 0.00000 0.00055 0.00061 0.00061 0.00049 0.00046 0.00048 0.00026 S4 0.84111 0.24830 0.04508 1.00000 0.02600 0.02548 0.03434 0.00376 0.00711 0.00069 0.02933 0.00228 0.00012 0.00008 0.00014 0.00000 0.00060 0.00055 0.00062 0.00046 0.00049 0.00047 0.00026 N1 0.36638 0.38680 0.41048 1.00000 0.02369 0.02970 0.03269 0.00058 0.00415 0.00374 0.02912 0.00734 0.00040 0.00026 0.00044 0.00000 0.00205 0.00200 0.00211 0.00164 0.00165 0.00167 0.00085 N2 0.73725 0.46160 -0.05909 1.00000 0.02732 0.02558 0.02344 0.00494 -0.00014 0.00530 0.02545 0.00702 0.00040 0.00024 0.00040 0.00000 0.00207 0.00186 0.00187 0.00149 0.00156 0.00163 0.00080 N3 0.48468 0.16142 0.45067 1.00000 0.02566 0.03354 0.03304 0.01115 0.00047 0.00562 0.03057 0.00768 0.00041 0.00027 0.00045 0.00000 0.00213 0.00207 0.00213 0.00168 0.00168 0.00172 0.00088 N4 0.76130 0.06027 -0.00491 1.00000 0.02900 0.02921 0.02940 0.00467 -0.00053 0.00453 0.02946 0.00738 0.00041 0.00026 0.00043 0.00000 0.00215 0.00198 0.00203 0.00160 0.00165 0.00171 0.00085 C1 0.26273 0.32293 0.33287 1.00000 0.02221 0.02677 0.02928 0.00345 0.00167 0.00656 0.02587 0.00867 0.00047 0.00030 0.00051 0.00000 0.00227 0.00222 0.00236 0.00184 0.00184 0.00188 0.00094 C2 0.13232 0.28755 0.39822 1.00000 0.01865 0.03092 0.04074 0.00874 0.00130 0.00339 0.03021 0.00939 0.00047 0.00032 0.00055 0.00000 0.00224 0.00241 0.00272 0.00205 0.00197 0.00192 0.00103 H2 0.05999 0.24347 0.33918 1.00000 0.03626 0.00000 0.00000 C3 0.11015 0.31723 0.54835 1.00000 0.02647 0.04439 0.03947 0.01685 0.01421 0.01111 0.03557 0.01023 0.00052 0.00035 0.00057 0.00000 0.00256 0.00292 0.00280 0.00232 0.00214 0.00226 0.00116 H3 0.02198 0.29419 0.59521 1.00000 0.04268 0.00000 0.00000 C4 0.21795 0.38147 0.63179 1.00000 0.04052 0.05321 0.02745 0.00621 0.00302 0.01170 0.04009 0.01048 0.00056 0.00038 0.00058 0.00000 0.00312 0.00323 0.00254 0.00229 0.00223 0.00263 0.00123 H4 0.20610 0.40200 0.73740 1.00000 0.04811 0.00000 0.00000 C5 0.34259 0.41469 0.55747 1.00000 0.03660 0.03818 0.03400 -0.00197 0.00331 0.00969 0.03626 0.01020 0.00055 0.00035 0.00057 0.00000 0.00289 0.00271 0.00263 0.00214 0.00219 0.00234 0.00113 H5 0.41552 0.45985 0.61374 1.00000 0.04351 0.00000 0.00000 C6 0.67389 0.39602 -0.16875 1.00000 0.02848 0.02827 0.02721 0.00829 0.00044 0.01030 0.02711 0.00897 0.00049 0.00031 0.00051 0.00000 0.00247 0.00229 0.00230 0.00184 0.00189 0.00197 0.00097 C7 0.72725 0.38493 -0.31695 1.00000 0.04610 0.03696 0.02371 0.00072 0.00349 0.01192 0.03525 0.01012 0.00056 0.00035 0.00053 0.00000 0.00315 0.00264 0.00234 0.00198 0.00214 0.00238 0.00113 H7 0.67894 0.33695 -0.39179 1.00000 0.04230 0.00000 0.00000 C8 0.85096 0.44496 -0.35175 1.00000 0.03957 0.04966 0.03588 0.01756 0.01465 0.01993 0.03938 0.01126 0.00056 0.00037 0.00060 0.00000 0.00304 0.00310 0.00277 0.00242 0.00233 0.00258 0.00124 H8 0.88996 0.43933 -0.45220 1.00000 0.04725 0.00000 0.00000 C9 0.91962 0.51405 -0.24065 1.00000 0.02208 0.03986 0.04379 0.01471 0.00797 0.00610 0.03484 0.01003 0.00050 0.00035 0.00057 0.00000 0.00245 0.00275 0.00292 0.00231 0.00213 0.00215 0.00114 H9 1.00664 0.55587 -0.26227 1.00000 0.04180 0.00000 0.00000 C10 0.85771 0.52024 -0.09762 1.00000 0.03004 0.03488 0.03306 0.00743 0.00298 0.00919 0.03215 0.00976 0.00050 0.00033 0.00055 0.00000 0.00265 0.00257 0.00254 0.00205 0.00205 0.00216 0.00107 H10 0.90295 0.56880 -0.02205 1.00000 0.03858 0.00000 0.00000 C11 0.60403 0.13914 0.50156 1.00000 0.02084 0.01935 0.02726 0.00206 -0.00251 -0.00189 0.02356 0.00787 0.00045 0.00028 0.00049 0.00000 0.00220 0.00198 0.00225 0.00169 0.00177 0.00172 0.00090 C12 0.61092 0.09205 0.63766 1.00000 0.03089 0.03096 0.03128 0.00583 -0.00501 0.00841 0.03074 0.00895 0.00051 0.00032 0.00053 0.00000 0.00263 0.00242 0.00244 0.00194 0.00201 0.00209 0.00104 H12 0.69647 0.07675 0.66953 1.00000 0.03689 0.00000 0.00000 C13 0.49308 0.06841 0.72392 1.00000 0.03453 0.03601 0.02845 0.01007 -0.00096 0.00242 0.03361 0.00927 0.00052 0.00034 0.00054 0.00000 0.00277 0.00258 0.00247 0.00203 0.00208 0.00220 0.00110 H13 0.49529 0.03637 0.81706 1.00000 0.04034 0.00000 0.00000 C14 0.36926 0.09166 0.67428 1.00000 0.02940 0.04212 0.03778 0.00909 0.00858 0.00674 0.03634 0.00987 0.00053 0.00035 0.00057 0.00000 0.00269 0.00284 0.00278 0.00226 0.00218 0.00228 0.00115 H14 0.28561 0.07618 0.73261 1.00000 0.04360 0.00000 0.00000 C15 0.37143 0.13737 0.53937 1.00000 0.01944 0.03963 0.04205 0.00929 -0.00111 0.00673 0.03347 0.00940 0.00049 0.00034 0.00056 0.00000 0.00234 0.00267 0.00278 0.00222 0.00204 0.00207 0.00109 H15 0.28665 0.15319 0.50615 1.00000 0.04016 0.00000 0.00000 C16 0.85527 0.13749 -0.04047 1.00000 0.02340 0.02968 0.02289 0.00483 -0.00394 0.00813 0.02492 0.00847 0.00047 0.00031 0.00049 0.00000 0.00228 0.00225 0.00216 0.00176 0.00175 0.00188 0.00092 C17 0.96382 0.13506 -0.14486 1.00000 0.02280 0.04183 0.03605 0.00515 0.00446 0.00639 0.03360 0.00966 0.00050 0.00036 0.00055 0.00000 0.00244 0.00275 0.00264 0.00217 0.00202 0.00215 0.00108 H17 1.03070 0.19124 -0.16601 1.00000 0.04032 0.00000 0.00000 C18 0.97126 0.04912 -0.21620 1.00000 0.02779 0.05967 0.04382 -0.00772 0.00665 0.01679 0.04310 0.01047 0.00055 0.00040 0.00062 0.00000 0.00277 0.00353 0.00306 0.00261 0.00232 0.00262 0.00130 H18 1.04304 0.04527 -0.28885 1.00000 0.05173 0.00000 0.00000 C19 0.87359 -0.03151 -0.18139 1.00000 0.04362 0.03722 0.04226 -0.01055 -0.00481 0.01599 0.04059 0.01000 0.00057 0.00037 0.00060 0.00000 0.00321 0.00278 0.00299 0.00229 0.00245 0.00251 0.00124 H19 0.87712 -0.09161 -0.22878 1.00000 0.04871 0.00000 0.00000 C20 0.77107 -0.02236 -0.07620 1.00000 0.04147 0.02785 0.03470 0.00076 -0.00361 0.01037 0.03440 0.00946 0.00055 0.00033 0.00055 0.00000 0.00301 0.00239 0.00267 0.00201 0.00224 0.00222 0.00111 H20 0.70347 -0.07772 -0.05284 1.00000 0.04128 0.00000 0.00000 C21 0.63394 0.33628 0.23942 1.00000 0.02424 0.02337 0.02354 0.00557 -0.00036 0.00436 0.02375 0.00826 0.00046 0.00028 0.00049 0.00000 0.00227 0.00211 0.00213 0.00170 0.00176 0.00180 0.00090 H21A 0.60859 0.33846 0.35114 1.00000 0.02850 0.00000 0.00000 H21B 0.73107 0.37558 0.23249 1.00000 0.02850 0.00000 0.00000 Final Structure Factor Calculation for dw9710 in P-1 Total number of l.s. parameters = 280 Maximum vector length = 511 Memory required = 3332 / 24017 wR2 = 0.1027 before cycle 4 for 5345 data and 0 / 280 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0291 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0458 for 3888 Fo > 4sig(Fo) and 0.0752 for all 5345 data wR2 = 0.1027, GooF = S = 1.016, Restrained GooF = 1.016 for all data Occupancy sum of asymmetric unit = 31.00 for non-hydrogen and 18.00 for hydrogen atoms Principal mean square atomic displacements U 0.0245 0.0223 0.0202 As1 0.0278 0.0233 0.0188 As2 0.0364 0.0309 0.0204 S1 0.0395 0.0280 0.0212 S2 0.0430 0.0245 0.0192 S3 0.0383 0.0305 0.0192 S4 0.0356 0.0294 0.0223 N1 0.0293 0.0264 0.0207 N2 0.0424 0.0257 0.0237 N3 0.0341 0.0279 0.0264 N4 0.0300 0.0259 0.0217 C1 0.0438 0.0284 0.0185 C2 0.0567 0.0325 0.0175 C3 0.0535 0.0402 0.0266 C4 0.0416 0.0375 0.0298 C5 0.0341 0.0285 0.0187 C6 0.0464 0.0362 0.0231 C7 0.0633 0.0317 0.0231 C8 0.0531 0.0320 0.0194 C9 0.0390 0.0290 0.0284 C10 0.0310 0.0250 0.0146 C11 0.0383 0.0318 0.0221 C12 0.0462 0.0317 0.0229 C13 0.0463 0.0385 0.0242 C14 0.0478 0.0338 0.0188 C15 0.0308 0.0277 0.0163 C16 0.0429 0.0361 0.0218 C17 0.0663 0.0426 0.0204 C18 0.0576 0.0383 0.0259 C19 0.0441 0.0324 0.0267 C20 0.0285 0.0236 0.0191 C21 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.030 0.044 0.062 0.079 0.099 0.123 0.159 0.219 1.000 Number in group 573. 530. 512. 536. 536. 520. 533. 537. 534. 534. GooF 0.986 1.026 1.009 1.017 1.009 1.028 0.946 0.998 1.034 1.103 K 1.190 1.129 1.010 1.012 0.992 1.008 0.996 1.003 1.010 0.993 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.64 inf Number in group 551. 524. 534. 530. 544. 524. 532. 536. 533. 537. GooF 0.995 0.988 1.038 0.965 0.989 1.007 0.976 1.007 1.013 1.166 K 0.985 0.996 0.995 0.993 0.998 1.014 1.005 1.010 1.001 0.990 R1 0.171 0.156 0.127 0.105 0.086 0.067 0.059 0.051 0.038 0.028 Recommended weighting scheme: WGHT 0.0296 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 1 1 37076.38 43131.11 4.75 0.931 5.32 -1 4 0 34189.06 39500.26 4.46 0.891 3.60 2 -4 1 43173.72 49750.24 4.39 1.000 3.05 -2 7 4 1078.59 1360.50 3.78 0.165 1.43 3 4 3 980.51 1240.60 3.75 0.158 1.65 9 1 3 330.02 136.40 3.65 0.052 0.96 3 16 2 223.51 52.70 3.65 0.033 0.78 0 14 5 101.07 2.57 3.58 0.007 0.84 -1 -14 7 122.72 1.59 3.55 0.006 0.79 -3 -11 4 2980.63 3653.71 3.54 0.271 1.01 -2 6 1 1621.15 1289.81 3.52 0.161 2.23 8 9 1 1503.67 1125.24 3.48 0.150 0.85 -12 3 1 163.26 15.11 3.46 0.017 0.81 -1 7 6 2550.31 3149.19 3.44 0.252 1.14 1 5 7 519.66 349.62 3.34 0.084 1.07 10 5 1 317.62 131.60 3.32 0.051 0.83 2 -3 1 30315.35 33762.78 3.31 0.824 3.52 -4 -11 6 297.11 525.42 3.26 0.103 0.86 0 -10 3 10185.45 11484.23 3.22 0.480 1.30 -8 1 0 144.82 43.58 3.18 0.030 1.20 -2 -1 7 96.18 17.44 3.17 0.019 1.18 -3 -4 7 701.36 522.00 3.09 0.102 1.09 2 4 0 1564.08 1240.45 3.05 0.158 2.56 5 -18 3 666.23 442.66 3.03 0.094 0.78 3 -10 8 1690.46 1347.89 3.03 0.165 0.88 -7 8 0 181.38 79.12 3.01 0.040 1.22 2 -7 1 61.20 7.69 2.98 0.012 2.01 -1 -6 10 130.04 23.14 2.95 0.022 0.81 4 13 4 140.05 9.54 2.92 0.014 0.82 2 12 7 381.68 212.05 2.90 0.065 0.78 -5 12 3 138.78 38.40 2.88 0.028 1.03 -2 13 6 104.12 0.27 2.86 0.002 0.85 3 4 7 2412.17 1978.73 2.84 0.199 1.03 -1 5 1 14217.86 15786.09 2.83 0.563 2.70 -7 -11 2 767.33 1029.20 2.83 0.144 0.83 5 -7 1 1246.78 1478.68 2.81 0.172 1.56 -4 5 5 182.97 90.87 2.81 0.043 1.30 -8 -8 4 142.28 348.22 2.78 0.084 0.84 -6 4 1 58.82 0.39 2.77 0.003 1.56 -5 -2 5 203.32 114.01 2.76 0.048 1.24 -2 3 7 158.81 287.41 2.76 0.076 1.15 -6 15 0 127.01 17.16 2.75 0.019 0.91 1 -3 1 15212.36 16676.40 2.75 0.579 4.19 3 -4 2 492.32 400.99 2.73 0.090 2.30 -1 2 8 -16.53 106.99 2.72 0.046 1.04 -6 9 6 151.97 48.16 2.71 0.031 0.93 4 0 4 3253.74 3818.11 2.71 0.277 1.56 -1 2 4 -22.89 37.98 2.69 0.028 2.00 -5 15 0 82.19 0.28 2.68 0.002 0.94 -6 8 4 1114.36 898.62 2.68 0.134 1.12 Bond lengths and angles As1 - Distance Angles C21 1.9715 (0.0042) S2 2.2673 (0.0016) 99.05 (0.14) S1 2.2802 (0.0014) 99.78 (0.13) 85.19 (0.06) As1 - C21 S2 As2 - Distance Angles C21 1.9747 (0.0042) S4 2.2668 (0.0015) 92.88 (0.13) S3 2.2788 (0.0015) 97.31 (0.13) 91.04 (0.06) As2 - C21 S4 S1 - Distance Angles C1 1.7565 (0.0046) As1 2.2802 (0.0014) 96.10 (0.16) S1 - C1 S2 - Distance Angles C6 1.7631 (0.0047) As1 2.2673 (0.0016) 94.79 (0.16) S2 - C6 S3 - Distance Angles C11 1.7531 (0.0045) As2 2.2788 (0.0015) 96.55 (0.15) S3 - C11 S4 - Distance Angles C16 1.7664 (0.0046) As2 2.2668 (0.0015) 100.12 (0.15) S4 - C16 N1 - Distance Angles C5 1.3359 (0.0059) C1 1.3388 (0.0056) 117.54 (0.40) N1 - C5 N2 - Distance Angles C6 1.3307 (0.0056) C10 1.3400 (0.0056) 116.90 (0.40) N2 - C6 N3 - Distance Angles C15 1.3379 (0.0058) C11 1.3484 (0.0056) 116.49 (0.37) N3 - C15 N4 - Distance Angles C16 1.3306 (0.0054) C20 1.3393 (0.0058) 117.60 (0.42) N4 - C16 C1 - Distance Angles N1 1.3388 (0.0056) C2 1.3934 (0.0060) 122.51 (0.42) S1 1.7565 (0.0046) 116.95 (0.33) 120.53 (0.36) C1 - N1 C2 C2 - Distance Angles C3 1.3643 (0.0066) C1 1.3934 (0.0060) 118.94 (0.45) H2 0.9500 120.53 120.53 C2 - C3 C1 C3 - Distance Angles C2 1.3643 (0.0066) C4 1.3877 (0.0071) 119.21 (0.45) H3 0.9500 120.40 120.40 C3 - C2 C4 C4 - Distance Angles C5 1.3774 (0.0069) C3 1.3877 (0.0071) 118.26 (0.48) H4 0.9500 120.87 120.87 C4 - C5 C3 C5 - Distance Angles N1 1.3359 (0.0059) C4 1.3774 (0.0069) 123.50 (0.49) H5 0.9500 118.25 118.25 C5 - N1 C4 C6 - Distance Angles N2 1.3307 (0.0056) C7 1.3899 (0.0062) 123.60 (0.44) S2 1.7631 (0.0046) 117.01 (0.34) 119.38 (0.37) C6 - N2 C7 C7 - Distance Angles C8 1.3634 (0.0068) C6 1.3899 (0.0062) 118.04 (0.47) H7 0.9500 120.98 120.98 C7 - C8 C6 C8 - Distance Angles C7 1.3634 (0.0068) C9 1.3831 (0.0073) 119.92 (0.46) H8 0.9500 120.04 120.04 C8 - C7 C9 C9 - Distance Angles C10 1.3775 (0.0064) C8 1.3831 (0.0073) 117.82 (0.46) H9 0.9500 121.09 121.09 C9 - C10 C8 C10 - Distance Angles N2 1.3400 (0.0056) C9 1.3775 (0.0064) 123.69 (0.46) H10 0.9500 118.15 118.15 C10 - N2 C9 C11 - Distance Angles N3 1.3484 (0.0056) C12 1.3953 (0.0058) 122.72 (0.42) S3 1.7531 (0.0045) 116.36 (0.31) 120.93 (0.35) C11 - N3 C12 C12 - Distance Angles C13 1.3601 (0.0065) C11 1.3953 (0.0058) 118.88 (0.44) H12 0.9500 120.56 120.56 C12 - C13 C11 C13 - Distance Angles C12 1.3601 (0.0065) C14 1.3913 (0.0068) 119.28 (0.42) H13 0.9500 120.36 120.36 C13 - C12 C14 C14 - Distance Angles C15 1.3651 (0.0064) C13 1.3913 (0.0068) 118.09 (0.45) H14 0.9500 120.95 120.95 C14 - C15 C13 C15 - Distance Angles N3 1.3379 (0.0058) C14 1.3651 (0.0064) 124.53 (0.45) H15 0.9500 117.73 117.73 C15 - N3 C14 C16 - Distance Angles N4 1.3306 (0.0054) C17 1.3973 (0.0062) 122.83 (0.43) S4 1.7664 (0.0046) 118.84 (0.34) 118.32 (0.35) C16 - N4 C17 C17 - Distance Angles C18 1.3761 (0.0071) C16 1.3973 (0.0062) 118.23 (0.46) H17 0.9500 120.88 120.88 C17 - C18 C16 C18 - Distance Angles C17 1.3761 (0.0071) C19 1.3816 (0.0073) 119.52 (0.47) H18 0.9500 120.24 120.24 C18 - C17 C19 C19 - Distance Angles C20 1.3757 (0.0070) C18 1.3816 (0.0073) 118.16 (0.47) H19 0.9500 120.92 120.92 C19 - C20 C18 C20 - Distance Angles N4 1.3393 (0.0058) C19 1.3757 (0.0070) 123.64 (0.47) H20 0.9500 118.18 118.18 C20 - N4 C19 C21 - Distance Angles As1 1.9715 (0.0042) As2 1.9747 (0.0042) 115.92 (0.21) H21A 0.9900 108.30 108.30 H21B 0.9900 108.30 108.30 107.41 C21 - As1 As2 H21A Selected torsion angles 79.92 ( 0.20) C21 - As1 - S1 - C1 178.30 ( 0.15) S2 - As1 - S1 - C1 -81.91 ( 0.19) C21 - As1 - S2 - C6 178.93 ( 0.15) S1 - As1 - S2 - C6 85.58 ( 0.19) C21 - As2 - S3 - C11 178.62 ( 0.15) S4 - As2 - S3 - C11 -175.48 ( 0.18) C21 - As2 - S4 - C16 87.15 ( 0.15) S3 - As2 - S4 - C16 1.78 ( 0.66) C5 - N1 - C1 - C2 -177.56 ( 0.34) C5 - N1 - C1 - S1 -10.64 ( 0.35) As1 - S1 - C1 - N1 170.00 ( 0.34) As1 - S1 - C1 - C2 -1.62 ( 0.68) N1 - C1 - C2 - C3 177.70 ( 0.35) S1 - C1 - C2 - C3 -0.18 ( 0.69) C1 - C2 - C3 - C4 1.65 ( 0.74) C2 - C3 - C4 - C5 -0.18 ( 0.72) C1 - N1 - C5 - C4 -1.53 ( 0.78) C3 - C4 - C5 - N1 1.14 ( 0.65) C10 - N2 - C6 - C7 -179.71 ( 0.31) C10 - N2 - C6 - S2 4.81 ( 0.34) As1 - S2 - C6 - N2 -176.01 ( 0.36) As1 - S2 - C6 - C7 -0.33 ( 0.71) N2 - C6 - C7 - C8 -179.45 ( 0.36) S2 - C6 - C7 - C8 0.23 ( 0.72) C6 - C7 - C8 - C9 -0.96 ( 0.72) C7 - C8 - C9 - C10 -1.95 ( 0.66) C6 - N2 - C10 - C9 1.89 ( 0.72) C8 - C9 - C10 - N2 1.08 ( 0.66) C15 - N3 - C11 - C12 -179.07 ( 0.35) C15 - N3 - C11 - S3 -13.96 ( 0.35) As2 - S3 - C11 - N3 165.89 ( 0.34) As2 - S3 - C11 - C12 -0.75 ( 0.70) N3 - C11 - C12 - C13 179.41 ( 0.36) S3 - C11 - C12 - C13 0.05 ( 0.71) C11 - C12 - C13 - C14 0.25 ( 0.75) C12 - C13 - C14 - C15 -0.78 ( 0.74) C11 - N3 - C15 - C14 0.13 ( 0.81) C13 - C14 - C15 - N3 -1.55 ( 0.65) C20 - N4 - C16 - C17 177.39 ( 0.32) C20 - N4 - C16 - S4 -5.63 ( 0.36) As2 - S4 - C16 - N4 173.36 ( 0.33) As2 - S4 - C16 - C17 1.51 ( 0.71) N4 - C16 - C17 - C18 -177.44 ( 0.37) S4 - C16 - C17 - C18 -0.88 ( 0.75) C16 - C17 - C18 - C19 0.39 ( 0.77) C17 - C18 - C19 - C20 1.03 ( 0.69) C16 - N4 - C20 - C19 -0.47 ( 0.76) C18 - C19 - C20 - N4 -32.63 ( 0.22) S2 - As1 - C21 - As2 54.01 ( 0.22) S1 - As1 - C21 - As2 102.65 ( 0.21) S4 - As2 - C21 - As1 -165.94 ( 0.19) S3 - As2 - C21 - As1 FMAP and GRID set by program FMAP 2 3 22 GRID -2.632 -2 -2 2.632 2 2 R1 = 0.0724 for 5345 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.50 at 0.7364 0.2029 0.3060 [ 0.88 A from S3 ] Deepest hole -0.66 at 0.5764 0.1767 0.2578 [ 0.99 A from AS2 ] Mean = 0.00, Rms deviation from mean = 0.11 e/A^3, Highest memory used = 3349 / 24634 Molecule 1 scale 0.474 inches = 1.204 cm per Angstrom AS2 N4 C13 C14 S1 AS2 S3 C12 C15 C11 N3 C3 C2 C20 S4 C4 S3 C19 N4 8 1 4 C1 C5 AS2 7 S1 N1 C16 C18 AS1 C21 C17 S4 AS1 S2 10 N1 N2 S3 6 C6 N2 C7 5 S2 3 C10 AS1 C8 9 C9 2 S4 Atom Peak x y z Sof Height Distances and Angles AS1 0.00 0.5044 0.3938 0.1201 1.000 2.6 0 S1 2.280 0 S2 2.267 85.2 0 N1 2.835 61.2 145.8 0 N2 2.777 147.5 62.4 150.6 0 C21 1.972 99.8 99.0 81.7 85.1 0 7 2.308 61.2 80.4 77.8 108.8 41.8 0 10 2.335 63.5 73.8 94.9 105.2 161.9 120.2 0 4 2.421 35.5 81.1 67.9 129.0 65.8 25.7 96.4 16 H5 2.984 116.2 158.4 55.8 96.2 80.5 111.1 112.4 117.4 12 N2 3.553 81.2 104.0 78.6 106.5 156.9 141.9 34.1 116.5 78.5 1 AS1 3.836 118.0 83.6 116.6 62.6 142.2 164.0 54.7 150.3 83.9 43.9 6 S2 4.233 118.0 115.8 87.9 80.3 129.2 163.8 68.1 150.5 53.5 38.5 AS2 0.00 0.6354 0.2045 0.1716 1.000 3.5 0 S1 3.728 0 S2 3.414 50.8 0 S3 2.279 129.9 162.9 0 S4 2.267 131.2 82.0 91.0 0 N3 2.845 71.7 122.4 60.9 150.9 0 N4 3.007 135.3 103.5 85.9 59.0 121.2 0 C21 1.975 60.8 67.7 97.3 92.9 83.9 151.8 0 8 1.110 141.6 124.6 67.0 72.3 100.7 21.9 157.5 0 7 1.456 13.5 59.5 118.1 134.0 63.6 148.4 51.3 149.9 0 1 1.505 133.1 151.0 12.7 81.4 69.7 88.1 89.5 72.0 120.0 0 4 2.391 10.4 60.4 122.4 141.5 62.5 134.2 66.4 135.2 15.2 127.8 22 H13 3.455 100.2 118.8 78.3 115.3 69.1 56.7 151.4 44.6 105.6 89.9 24 H20 3.488 49.8 71.7 123.1 133.5 73.6 90.3 110.6 91.8 59.9 135.7 S1 0.00 0.2983 0.2836 0.1425 1.000 2.0 0 AS1 2.280 0 AS2 3.728 62.3 0 C1 1.757 96.1 106.8 0 H2 2.855 140.3 128.5 45.4 0 4 1.441 77.6 17.4 98.0 111.7 24 H20 3.046 117.9 61.0 122.5 95.5 52.6 23 H19 3.062 153.8 92.3 84.8 51.1 76.4 44.5 S2 0.00 0.5149 0.3191 -0.1187 1.000 2.2 0 AS1 2.267 0 AS2 3.414 68.8 0 S4 3.827 86.5 35.9 0 C6 1.763 94.8 100.5 67.7 0 H7 2.837 140.5 115.1 81.4 45.9 1 AS1 4.233 64.2 129.0 121.2 65.7 90.5 S3 0.00 0.7529 0.1724 0.3866 1.000 4.4 0 AS2 2.279 0 N4 3.641 55.5 0 C11 1.753 96.5 120.3 0 H12 2.863 139.8 125.9 45.2 0 H21A 3.094 52.1 106.6 78.6 115.6 0 1 0.876 22.2 61.7 112.6 157.8 47.1 0 8 2.109 29.0 27.5 105.9 134.2 81.1 41.8 14 H2 2.969 107.4 82.9 153.8 112.7 107.8 88.3 100.2 17 H7 3.182 94.7 149.4 64.3 80.2 42.8 88.2 123.6 102.6 15 H3 3.240 132.6 126.5 111.3 82.1 95.7 110.7 141.2 43.8 66.8 S4 0.04 0.8411 0.2483 0.0451 1.000 3.9 0 AS2 2.267 0 S2 3.827 62.1 0 N2 3.640 89.3 41.4 0 C16 1.766 100.1 111.0 140.2 0 H17 2.822 146.2 119.0 113.3 46.5 0 H21B 2.783 57.5 63.3 50.6 157.5 156.1 0 6 2.080 118.0 70.8 31.2 134.1 91.0 66.7 0 8 2.200 28.7 82.1 116.6 73.4 119.7 84.1 146.6 19 H10 3.219 139.3 105.2 64.7 120.1 74.5 82.0 34.4 159.0 14 H2 3.284 98.3 150.2 123.4 93.6 90.0 87.5 104.3 89.5 74.4 18 H9 3.330 100.1 100.7 64.7 147.7 112.0 47.6 51.6 118.5 41.4 58.7 N1 0.00 0.3664 0.3868 0.4105 1.000 2.6 0 AS1 2.835 0 C1 1.339 84.8 0 C5 1.336 156.9 117.5 0 H21A 2.657 53.3 107.7 118.7 16 H5 2.724 64.9 145.6 92.1 67.7 N2 0.00 0.7373 0.4616 -0.0591 1.000 3.0 0 AS1 2.777 0 S4 3.640 83.7 0 C6 1.331 85.6 75.8 0 C10 1.340 157.1 104.8 116.9 0 H21B 2.854 52.0 48.9 108.3 118.3 1 AS1 3.553 73.5 155.3 92.9 99.9 117.8 N3 0.00 0.4847 0.1614 0.4507 1.000 3.5 0 AS2 2.845 0 C11 1.348 84.5 0 C15 1.338 156.9 116.5 0 H21A 2.776 52.1 97.5 128.1 N4 0.00 0.7613 0.0603 -0.0049 1.000 3.8 0 AS2 3.007 0 S3 3.641 38.6 0 C16 1.331 81.8 87.9 0 C20 1.339 159.6 140.5 117.6 20 H12 2.880 105.0 142.9 76.6 75.5 21 H13 2.920 79.8 112.8 111.7 86.5 47.2 C1 0.00 0.2627 0.3229 0.3329 1.000 2.1 0 S1 1.757 0 N1 1.339 117.0 0 C2 1.393 120.5 122.5 C2 0.00 0.1323 0.2876 0.3982 1.000 1.8 0 C1 1.393 0 H2 0.950 120.5 0 C3 1.364 118.9 120.5 H2 0.00 0.0600 0.2435 0.3392 1.000 1.5 0 S1 2.855 0 C2 0.950 73.5 7 S3 2.969 151.7 132.8 9 S4 3.284 91.8 136.8 62.2 C3 0.09 0.1102 0.3172 0.5483 1.000 2.0 0 C2 1.364 0 H3 0.950 120.4 0 C4 1.388 119.2 120.4 H3 0.00 0.0220 0.2942 0.5952 1.000 1.8 0 C3 0.950 7 S3 3.240 120.7 C4 0.00 0.2179 0.3815 0.6318 1.000 2.5 0 C3 1.388 0 H4 0.950 120.9 0 C5 1.377 118.3 120.9 H4 0.00 0.2061 0.4020 0.7374 1.000 2.6 0 C4 0.950 C5 0.00 0.3426 0.4147 0.5575 1.000 2.8 0 N1 1.336 0 C4 1.377 123.5 0 H5 0.950 118.2 118.2 H5 0.00 0.4155 0.4598 0.6137 1.000 3.1 0 C5 0.950 11 N1 2.724 144.9 2 AS1 2.984 147.7 59.3 C6 0.00 0.6739 0.3960 -0.1687 1.000 2.6 0 S2 1.763 0 N2 1.331 117.0 0 C7 1.390 119.4 123.6 C7 0.00 0.7272 0.3849 -0.3169 1.000 2.6 0 C6 1.390 0 H7 0.950 121.0 0 C8 1.363 118.0 121.0 0 9 1.685 102.0 127.9 32.9 0 5 1.816 98.2 58.8 113.1 89.2 H7 0.00 0.6789 0.3369 -0.3918 1.000 2.3 0 S2 2.837 0 C7 0.950 73.8 0 5 1.553 80.8 89.7 8 S3 3.182 127.8 137.3 126.6 C8 0.00 0.8510 0.4450 -0.3517 1.000 2.9 0 C7 1.363 0 H8 0.950 120.0 0 C9 1.383 119.9 120.0 0 9 0.917 93.2 107.8 68.7 H8 0.00 0.8900 0.4393 -0.4522 1.000 2.9 0 C8 0.950 0 9 1.509 35.3 C9 0.00 0.9196 0.5140 -0.2406 1.000 3.3 0 C8 1.383 0 H9 0.950 121.1 0 C10 1.377 117.8 121.1 0 9 1.354 39.1 119.5 105.5 0 3 1.540 92.8 84.1 93.3 131.7 0 2 1.705 144.2 54.5 77.8 107.8 119.6 H9 0.00 1.0066 0.5559 -0.2623 1.000 3.5 0 C9 0.950 0 2 1.389 91.7 10 S4 3.330 125.3 43.8 C10 0.12 0.8577 0.5202 -0.0976 1.000 3.3 0 N2 1.340 0 C9 1.377 123.7 0 H10 0.950 118.2 118.2 0 2 1.952 152.5 58.6 67.1 H10 0.00 0.9029 0.5688 -0.0221 1.000 3.6 0 C10 0.950 10 S4 3.219 132.3 C11 0.00 0.6040 0.1391 0.5016 1.000 4.1 0 S3 1.753 0 N3 1.348 116.4 0 C12 1.395 120.9 122.7 C12 0.00 0.6109 0.0920 0.6377 1.000 4.5 0 C11 1.395 0 H12 0.950 120.6 0 C13 1.360 118.9 120.6 H12 0.23 0.6965 0.0768 0.6695 1.000 4.9 0 S3 2.863 0 C12 0.950 73.3 13 N4 2.880 150.3 121.3 C13 0.00 0.4931 0.0684 0.7239 1.000 4.2 0 C12 1.360 0 H13 0.950 120.4 0 C14 1.391 119.3 120.4 H13 0.00 0.4953 0.0364 0.8171 1.000 4.5 0 C13 0.950 13 N4 2.920 119.8 3 AS2 3.455 122.5 100.3 C14 0.00 0.3693 0.0917 0.6743 1.000 3.6 0 C13 1.391 0 H14 0.950 121.0 0 C15 1.365 118.1 121.0 H14 0.00 0.2856 0.0762 0.7326 1.000 3.4 0 C14 0.950 C15 0.00 0.3714 0.1374 0.5394 1.000 3.3 0 N3 1.338 0 C14 1.365 124.5 0 H15 0.950 117.7 117.7 H15 0.00 0.2867 0.1532 0.5062 1.000 2.8 0 C15 0.950 C16 0.00 0.8553 0.1375 -0.0405 1.000 4.0 0 S4 1.766 0 N4 1.331 118.8 0 C17 1.397 118.3 122.8 C17 0.00 0.9638 0.1351 -0.1449 1.000 4.2 0 C16 1.397 0 H17 0.950 120.9 0 C18 1.376 118.2 120.9 H17 0.00 1.0307 0.1912 -0.1660 1.000 4.3 0 S4 2.822 0 C17 0.950 74.3 C18 0.13 0.9713 0.0491 -0.2162 1.000 4.2 0 C17 1.376 0 H18 0.950 120.2 0 C19 1.382 119.5 120.2 H18 0.00 1.0430 0.0453 -0.2889 1.000 4.4 0 C18 0.950 C19 0.00 0.8736 -0.0315 -0.1814 1.000 4.0 0 C18 1.382 0 H19 0.950 120.9 0 C20 1.376 118.2 120.9 H19 0.00 0.8771 -0.0916 -0.2288 1.000 4.0 0 C19 0.950 5 S1 3.062 126.5 C20 0.00 0.7711 -0.0224 -0.0762 1.000 3.8 0 N4 1.339 0 C19 1.376 123.6 0 H20 0.950 118.2 118.2 H20 0.00 0.7035 -0.0777 -0.0528 1.000 3.7 0 C20 0.950 5 S1 3.046 128.8 4 AS2 3.488 139.9 69.2 C21 0.00 0.6339 0.3363 0.2394 1.000 3.4 0 AS1 1.972 0 AS2 1.975 115.9 0 H21A 0.990 108.3 108.3 0 H21B 0.990 108.3 108.3 107.4 0 7 1.558 80.8 46.9 92.9 153.0 H21A 0.00 0.6086 0.3385 0.3511 1.000 3.5 0 S3 3.094 0 N1 2.657 140.5 0 N3 2.776 53.2 87.5 0 C21 0.990 87.1 115.6 112.7 H21B 0.00 0.7311 0.3756 0.2325 1.000 3.7 0 S4 2.783 0 N2 2.854 80.4 0 C21 0.990 97.9 105.8 1 0.50 0.7364 0.2029 0.3060 1.000 4.1 0 AS2 1.505 0 S3 0.876 145.1 0 8 1.569 42.3 116.3 2 0.43 0.9634 0.6327 -0.1924 1.000 3.4 0 C9 1.705 0 H9 1.389 33.8 0 C10 1.952 43.6 73.0 3 0.42 1.0148 0.4515 -0.1823 1.000 3.9 0 C9 1.540 0 6 1.934 101.0 4 0.41 0.4033 0.2331 0.1840 1.000 2.5 0 AS1 2.421 0 AS2 2.391 88.1 0 S1 1.441 66.9 152.2 0 7 1.057 71.2 21.1 138.0 5 0.40 0.5767 0.4002 -0.4322 1.000 1.7 0 C7 1.816 0 H7 1.553 31.5 6 0.40 0.8993 0.3862 -0.0228 1.000 3.8 0 S4 2.080 0 3 1.934 136.5 7 0.39 0.5146 0.2463 0.1964 1.000 3.0 0 AS1 2.308 0 AS2 1.456 123.8 0 C21 1.558 57.5 81.8 0 4 1.057 83.2 143.7 134.2 8 0.38 0.6792 0.1410 0.1516 1.000 3.7 0 AS2 1.110 0 S3 2.109 84.0 0 S4 2.200 79.0 97.6 0 1 1.569 65.8 21.8 82.4 9 0.38 0.8118 0.4966 -0.3486 1.000 2.7 0 C7 1.685 0 C8 0.917 53.9 0 H8 1.509 78.0 36.8 0 C9 1.354 102.4 72.1 90.3 10 0.38 0.3098 0.4128 -0.0269 1.000 1.5 0 AS1 2.335 Code Atom x y z Height Symmetry Transformation 1 AS1 0.4956 0.6062 -0.1201 1.7 1.0000-X 1.0000-Y 0.0000-Z 2 AS1 0.4956 0.6062 0.8799 3.8 1.0000-X 1.0000-Y 1.0000-Z 3 AS2 0.3646 -0.2045 0.8284 4.3 1.0000-X 0.0000-Y 1.0000-Z 4 AS2 0.3646 -0.2045 -0.1716 2.3 1.0000-X 0.0000-Y 0.0000-Z 5 S1 0.7017 -0.2836 -0.1425 3.8 1.0000-X 0.0000-Y 0.0000-Z 6 S2 0.4851 0.6809 0.1187 2.1 1.0000-X 1.0000-Y 0.0000-Z 7 S3 -0.2471 0.1724 0.3866 0.5 -1.0000+X 0.0000+Y 0.0000+Z 8 S3 0.7529 0.1724 -0.6134 2.4 0.0000+X 0.0000+Y -1.0000+Z 9 S4 -0.1589 0.2483 0.0451 0.0 -1.0000+X 0.0000+Y 0.0000+Z 10 S4 1.1589 0.7517 -0.0451 4.3 2.0000-X 1.0000-Y 0.0000-Z 11 N1 0.6336 0.6132 0.5895 3.7 1.0000-X 1.0000-Y 1.0000-Z 12 N2 0.2627 0.5384 0.0591 1.3 1.0000-X 1.0000-Y 0.0000-Z 13 N4 0.7613 0.0603 0.9951 5.8 0.0000+X 0.0000+Y 1.0000+Z 14 H2 1.0600 0.2435 0.3392 5.4 1.0000+X 0.0000+Y 0.0000+Z 15 H3 1.0220 0.2942 0.5952 5.7 1.0000+X 0.0000+Y 0.0000+Z 16 H5 0.5845 0.5402 0.3863 3.2 1.0000-X 1.0000-Y 1.0000-Z 17 H7 0.6789 0.3369 0.6082 4.3 0.0000+X 0.0000+Y 1.0000+Z 18 H9 0.9934 0.4441 0.2623 4.7 2.0000-X 1.0000-Y 0.0000-Z 19 H10 1.0971 0.4312 0.0220 4.7 2.0000-X 1.0000-Y 0.0000-Z 20 H12 0.6965 0.0768 -0.3305 2.9 0.0000+X 0.0000+Y -1.0000+Z 21 H13 0.4953 0.0364 -0.1829 2.4 0.0000+X 0.0000+Y -1.0000+Z 22 H13 0.5047 -0.0364 0.1829 3.3 1.0000-X 0.0000-Y 1.0000-Z 23 H19 0.1229 0.0916 0.2288 1.7 1.0000-X 0.0000-Y 0.0000-Z 24 H20 0.2965 0.0777 0.0528 2.1 1.0000-X 0.0000-Y 0.0000-Z Time profile in seconds ----------------------- 0.20: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.02: 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. 0.80: 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 1.25: Structure factors and derivatives 2.45: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.36: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.13: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.03: Peaksearch 0.05: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + dw9810 finished at 14:21:43 Total CPU time: 5.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++