+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 08:59:05 on 11-Feb-2003 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 03SRC0102 in P2(1) CELL 0.71073 5.4663 17.8280 8.1473 90.000 90.423 90.000 ZERR 2.00 0.0002 0.0012 0.0005 0.000 0.003 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H O S UNIT 30 40 10 2 V = 793.96 F(000) = 332.0 Mu = 0.22 mm-1 Cell Wt = 624.74 Rho = 1.307 SHEL 7 0.84 TEMP -153 SIZE 0.3 0.15 0.1 ACTA FMAP 2 PLAN 20 BOND L.S. 4 WGHT 0.129800 0.076400 EXTI 0.023771 FVAR 0.61299 MOLE 1 S1 4 0.667044 0.772275 0.997308 11.00000 0.03323 0.06720 = 0.03382 -0.01752 0.00941 -0.01075 O3 3 0.462385 0.740588 0.880088 11.00000 0.03854 0.04602 = 0.02974 -0.00714 0.00290 -0.00747 O2 3 0.387719 0.631031 0.637617 11.00000 0.03430 0.04582 = 0.03066 -0.01048 0.00324 -0.00328 C14 1 0.600860 0.778715 1.325217 11.00000 0.03653 0.04400 = 0.03544 0.00365 0.00084 0.00285 AFIX 43 H14 2 0.742020 0.747819 1.333416 11.00000 -1.20000 AFIX 0 C9 1 0.509998 0.799825 1.173658 11.00000 0.02660 0.03522 = 0.02917 -0.00756 0.00500 -0.00546 C11 1 0.190440 0.867680 1.301268 11.00000 0.03890 0.03652 = 0.04425 -0.00020 0.00469 0.00898 AFIX 43 H11 2 0.048322 0.898158 1.293019 11.00000 -1.20000 AFIX 0 C12 1 0.277436 0.847740 1.454205 11.00000 0.04540 0.02816 = 0.03107 -0.00059 0.01084 -0.00676 O4 3 0.831349 0.713020 1.039352 11.00000 0.02913 0.10137 = 0.05993 -0.03783 -0.00275 0.01565 O1 3 0.113906 0.537059 0.622719 11.00000 0.06205 0.04196 = 0.04056 -0.00738 0.01114 -0.01626 C8 1 0.357039 0.667520 0.915377 11.00000 0.03442 0.04066 = 0.03188 -0.00026 0.00317 0.00013 AFIX 23 H8A 2 0.246246 0.670443 1.010740 11.00000 -1.20000 H8B 2 0.487085 0.630381 0.939440 11.00000 -1.20000 AFIX 0 C15 1 0.150426 0.873973 1.606708 11.00000 0.06438 0.05035 = 0.04244 -0.00232 0.01901 0.00109 AFIX 137 H15A 2 0.072403 0.922552 1.585629 11.00000 -1.50000 H15B 2 0.270274 0.879227 1.696020 11.00000 -1.50000 H15C 2 0.025755 0.837250 1.637951 11.00000 -1.50000 AFIX 0 C13 1 0.484049 0.803066 1.463986 11.00000 0.04547 0.04334 = 0.02946 0.00606 0.00060 0.00166 AFIX 43 H13 2 0.546252 0.788976 1.568717 11.00000 -1.20000 AFIX 0 C7 1 0.218994 0.646387 0.764178 11.00000 0.02916 0.03569 = 0.02840 0.00047 0.00421 0.00241 AFIX 13 H7 2 0.111319 0.689072 0.730149 11.00000 -1.20000 AFIX 0 C10 1 0.305456 0.844307 1.159048 11.00000 0.03868 0.05165 = 0.02990 0.00134 0.00175 0.00267 AFIX 43 H10 2 0.244509 0.858657 1.054160 11.00000 -1.20000 AFIX 0 C3 1 0.064089 0.573574 0.774086 11.00000 0.03483 0.03957 = 0.03225 0.00018 0.00373 -0.00254 AFIX 13 H3 2 -0.113591 0.586589 0.779802 11.00000 -1.20000 AFIX 0 O5 3 0.756712 0.835743 0.913074 11.00000 0.07271 0.09805 = 0.04233 -0.01434 0.02483 -0.04779 C4 1 0.262324 0.583422 0.524125 11.00000 0.03561 0.04023 = 0.03460 -0.00774 0.00340 -0.00586 C6 1 0.100244 0.628636 0.409319 11.00000 0.07205 0.05192 = 0.03763 -0.00208 -0.01487 -0.00344 AFIX 137 H6A 2 0.022609 0.595003 0.329316 11.00000 -1.50000 H6B 2 0.199534 0.665856 0.351521 11.00000 -1.50000 H6C 2 -0.026207 0.654283 0.472891 11.00000 -1.50000 AFIX 0 C1 1 -0.014952 0.505130 1.032321 11.00000 0.09939 0.05479 = 0.04646 0.00130 0.00571 -0.01584 AFIX 93 H1A 2 -0.172962 0.527142 1.037683 11.00000 -1.20000 H1B 2 0.037744 0.471355 1.115553 11.00000 -1.20000 AFIX 0 C2 1 0.129821 0.521300 0.910534 11.00000 0.06470 0.04288 = 0.04757 0.00276 -0.00492 -0.00952 AFIX 43 H2 2 0.286660 0.498373 0.908678 11.00000 -1.20000 AFIX 0 C5 1 0.447317 0.536618 0.436601 11.00000 0.05051 0.07687 = 0.06135 -0.03602 0.00370 0.00593 AFIX 137 H5A 2 0.555254 0.512313 0.517109 11.00000 -1.50000 H5B 2 0.544587 0.568639 0.364281 11.00000 -1.50000 H5C 2 0.363296 0.498242 0.371077 11.00000 -1.50000 HKLF 4 Covalent radii and connectivity table for 03SRC0102 in P2(1) C 0.770 H 0.320 O 0.660 S 1.030 S1 - O5 O4 O3 C9 O3 - C8 S1 O2 - C7 C4 C14 - C13 C9 C9 - C10 C14 S1 C11 - C12 C10 C12 - C11 C13 C15 O4 - S1 O1 - C4 C3 C8 - O3 C7 C15 - C12 C13 - C14 C12 C7 - O2 C8 C3 C10 - C9 C11 C3 - O1 C2 C7 O5 - S1 C4 - O1 O2 C5 C6 C6 - C4 C1 - C2 C2 - C1 C3 C5 - C4 Floating origin restraints generated 8944 Reflections read, of which 1200 rejected -6 =< h =< 5, -21 =< k =< 21, -9 =< l =< 9, Max. 2-theta = 50.04 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 5 -1 0 44.06 0.90 4 8.11 5 1 0 34.40 0.97 3 10.62 5 3 0 24.48 0.72 4 4.35 5 5 0 58.13 1.08 2 45.65 4 Inconsistent equivalents 2685 Unique reflections, of which 0 suppressed R(int) = 0.0593 R(sigma) = 0.0522 Friedel opposites not merged Maximum memory for data reduction = 1952 / 26883 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 = 2518 / 240566 wR2 = 0.1301 before cycle 1 for 2685 data and 194 / 194 parameters GooF = S = 0.761; Restrained GooF = 0.760 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1298 * P )^2 + 0.08 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.61299 0.00216 0.001 OSF 2 0.02377 0.00660 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.009 for U12 S1 Max. shift = 0.000 A for H15C Max. dU = 0.000 for C2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2518 / 240566 wR2 = 0.1301 before cycle 2 for 2685 data and 194 / 194 parameters GooF = S = 0.761; Restrained GooF = 0.760 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1298 * P )^2 + 0.08 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.61299 0.00216 0.000 OSF 2 0.02377 0.00660 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.003 for U12 S1 Max. shift = 0.000 A for H15C Max. dU = 0.000 for C2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2518 / 240566 wR2 = 0.1301 before cycle 3 for 2685 data and 194 / 194 parameters GooF = S = 0.761; Restrained GooF = 0.761 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1298 * P )^2 + 0.08 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.61299 0.00216 0.000 OSF 2 0.02377 0.00660 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for tors H15A Max. shift = 0.000 A for H15B Max. dU = 0.000 for O5 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2518 / 240566 wR2 = 0.1301 before cycle 4 for 2685 data and 194 / 194 parameters GooF = S = 0.761; Restrained GooF = 0.761 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1298 * P )^2 + 0.08 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.61299 0.00216 0.000 OSF 2 0.02377 0.00660 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y C9 Max. shift = 0.000 A for H15C Max. dU = 0.000 for C6 Largest correlation matrix elements 0.510 U33 S1 / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H14 0.7420 0.7478 1.3334 43 0.950 0.000 C14 C13 C9 H11 0.0483 0.8982 1.2930 43 0.950 0.000 C11 C12 C10 H8A 0.2462 0.6704 1.0107 23 0.990 0.000 C8 O3 C7 H8B 0.4871 0.6304 0.9394 23 0.990 0.000 C8 O3 C7 H15A 0.0724 0.9226 1.5856 137 0.980 0.000 C15 C12 H15A H15B 0.2703 0.8792 1.6960 137 0.980 0.000 C15 C12 H15A H15C 0.0257 0.8373 1.6379 137 0.980 0.000 C15 C12 H15A H13 0.5463 0.7890 1.5687 43 0.950 0.000 C13 C14 C12 H7 0.1113 0.6891 0.7301 13 1.000 0.000 C7 O2 C8 C3 H10 0.2445 0.8587 1.0542 43 0.950 0.000 C10 C9 C11 H3 -0.1136 0.5866 0.7798 13 1.000 0.000 C3 O1 C2 C7 H6A 0.0226 0.5950 0.3293 137 0.980 0.000 C6 C4 H6A H6B 0.1995 0.6659 0.3515 137 0.980 0.000 C6 C4 H6A H6C -0.0262 0.6543 0.4729 137 0.980 0.000 C6 C4 H6A H1A -0.1730 0.5271 1.0377 93 0.950 0.000 C1 C2 C3 H1B 0.0377 0.4714 1.1156 93 0.950 0.000 C1 C2 C3 H2 0.2867 0.4984 0.9087 43 0.950 0.000 C2 C1 C3 H5A 0.5553 0.5123 0.5171 137 0.980 0.000 C5 C4 H5A H5B 0.5446 0.5686 0.3643 137 0.980 0.000 C5 C4 H5A H5C 0.3633 0.4982 0.3711 137 0.980 0.000 C5 C4 H5A 03SRC0102 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S1 0.66704 0.77227 0.99731 1.00000 0.03323 0.06720 0.03382 -0.01752 0.00941 -0.01075 0.04471 0.00127 0.00013 0.00005 0.00009 0.00000 0.00041 0.00057 0.00040 0.00038 0.00028 0.00039 0.00028 O3 0.46239 0.74059 0.88009 1.00000 0.03854 0.04602 0.02974 -0.00714 0.00290 -0.00747 0.03808 0.00338 0.00036 0.00012 0.00024 0.00000 0.00110 0.00122 0.00105 0.00094 0.00089 0.00094 0.00053 O2 0.38772 0.63103 0.63762 1.00000 0.03430 0.04582 0.03066 -0.01048 0.00324 -0.00328 0.03691 0.00348 0.00037 0.00013 0.00025 0.00000 0.00109 0.00127 0.00108 0.00092 0.00088 0.00094 0.00052 C14 0.60086 0.77872 1.32522 1.00000 0.03653 0.04400 0.03544 0.00365 0.00084 0.00285 0.03865 0.00529 0.00051 0.00019 0.00036 0.00000 0.00149 0.00189 0.00148 0.00147 0.00114 0.00149 0.00070 H14 0.74202 0.74782 1.33342 1.00000 0.04638 0.00000 0.00000 C9 0.51000 0.79983 1.17366 1.00000 0.02660 0.03522 0.02917 -0.00756 0.00500 -0.00546 0.03031 0.00462 0.00048 0.00017 0.00034 0.00000 0.00131 0.00153 0.00142 0.00114 0.00107 0.00110 0.00063 C11 0.19044 0.86768 1.30127 1.00000 0.03890 0.03652 0.04425 -0.00020 0.00468 0.00898 0.03987 0.00584 0.00058 0.00018 0.00041 0.00000 0.00170 0.00176 0.00183 0.00141 0.00140 0.00135 0.00075 H11 0.04832 0.89816 1.29302 1.00000 0.04784 0.00000 0.00000 C12 0.27744 0.84774 1.45420 1.00000 0.04540 0.02816 0.03107 -0.00059 0.01084 -0.00676 0.03482 0.00540 0.00057 0.00017 0.00038 0.00000 0.00167 0.00154 0.00149 0.00120 0.00125 0.00127 0.00067 O4 0.83135 0.71302 1.03935 1.00000 0.02913 0.10137 0.05993 -0.03783 -0.00275 0.01565 0.06349 0.00436 0.00041 0.00018 0.00033 0.00000 0.00117 0.00235 0.00157 0.00157 0.00107 0.00129 0.00086 O1 0.11391 0.53706 0.62272 1.00000 0.06205 0.04196 0.04056 -0.00738 0.01114 -0.01626 0.04814 0.00397 0.00044 0.00013 0.00029 0.00000 0.00148 0.00139 0.00129 0.00103 0.00111 0.00114 0.00062 C8 0.35704 0.66752 0.91538 1.00000 0.03442 0.04066 0.03188 -0.00026 0.00317 0.00013 0.03564 0.00532 0.00056 0.00018 0.00035 0.00000 0.00161 0.00171 0.00156 0.00134 0.00125 0.00124 0.00069 H8A 0.24625 0.67044 1.01074 1.00000 0.04277 0.00000 0.00000 H8B 0.48709 0.63038 0.93944 1.00000 0.04277 0.00000 0.00000 C15 0.15043 0.87397 1.60671 1.00000 0.06438 0.05035 0.04244 -0.00232 0.01901 0.00109 0.05230 0.00734 0.00075 0.00022 0.00046 0.00000 0.00228 0.00211 0.00190 0.00162 0.00162 0.00177 0.00090 H15A 0.07243 0.92256 1.58563 1.00000 0.07844 0.00000 0.00000 H15B 0.27027 0.87922 1.69603 1.00000 0.07844 0.00000 0.00000 H15C 0.02573 0.83726 1.63794 1.00000 0.07844 0.00000 0.00000 C13 0.48405 0.80307 1.46399 1.00000 0.04547 0.04334 0.02947 0.00606 0.00060 0.00166 0.03942 0.00558 0.00059 0.00019 0.00037 0.00000 0.00163 0.00168 0.00157 0.00133 0.00130 0.00143 0.00072 H13 0.54625 0.78898 1.56872 1.00000 0.04731 0.00000 0.00000 C7 0.21899 0.64639 0.76418 1.00000 0.02916 0.03569 0.02840 0.00047 0.00421 0.00241 0.03106 0.00515 0.00053 0.00017 0.00035 0.00000 0.00145 0.00165 0.00144 0.00116 0.00114 0.00116 0.00064 H7 0.11132 0.68907 0.73015 1.00000 0.03728 0.00000 0.00000 C10 0.30546 0.84431 1.15905 1.00000 0.03868 0.05165 0.02990 0.00134 0.00175 0.00267 0.04007 0.00579 0.00057 0.00020 0.00039 0.00000 0.00164 0.00202 0.00155 0.00144 0.00126 0.00142 0.00075 H10 0.24451 0.85866 1.05416 1.00000 0.04808 0.00000 0.00000 C3 0.06409 0.57357 0.77409 1.00000 0.03483 0.03957 0.03225 0.00017 0.00373 -0.00254 0.03553 0.00528 0.00055 0.00017 0.00038 0.00000 0.00158 0.00180 0.00154 0.00128 0.00119 0.00128 0.00069 H3 -0.11359 0.58659 0.77980 1.00000 0.04264 0.00000 0.00000 O5 0.75671 0.83574 0.91307 1.00000 0.07271 0.09805 0.04233 -0.01434 0.02483 -0.04779 0.07091 0.00449 0.00052 0.00019 0.00031 0.00000 0.00180 0.00224 0.00144 0.00145 0.00131 0.00171 0.00093 C4 0.26232 0.58342 0.52412 1.00000 0.03561 0.04023 0.03460 -0.00774 0.00340 -0.00586 0.03680 0.00530 0.00056 0.00019 0.00038 0.00000 0.00155 0.00171 0.00159 0.00135 0.00122 0.00134 0.00068 C6 0.10024 0.62864 0.40932 1.00000 0.07205 0.05192 0.03763 -0.00208 -0.01487 -0.00344 0.05394 0.00651 0.00080 0.00022 0.00047 0.00000 0.00243 0.00208 0.00175 0.00167 0.00170 0.00187 0.00092 H6A 0.02259 0.59500 0.32933 1.00000 0.08091 0.00000 0.00000 H6B 0.19954 0.66585 0.35151 1.00000 0.08091 0.00000 0.00000 H6C -0.02619 0.65429 0.47289 1.00000 0.08091 0.00000 0.00000 C1 -0.01495 0.50513 1.03232 1.00000 0.09939 0.05479 0.04647 0.00129 0.00571 -0.01584 0.06686 0.00794 0.00104 0.00025 0.00051 0.00000 0.00316 0.00250 0.00249 0.00181 0.00233 0.00234 0.00118 H1A -0.17296 0.52714 1.03768 1.00000 0.08023 0.00000 0.00000 H1B 0.03774 0.47135 1.11555 1.00000 0.08023 0.00000 0.00000 C2 0.12982 0.52130 0.91053 1.00000 0.06470 0.04287 0.04757 0.00276 -0.00492 -0.00952 0.05174 0.00651 0.00080 0.00021 0.00048 0.00000 0.00219 0.00195 0.00207 0.00163 0.00167 0.00168 0.00087 H2 0.28666 0.49837 0.90868 1.00000 0.06209 0.00000 0.00000 C5 0.44732 0.53662 0.43660 1.00000 0.05051 0.07687 0.06135 -0.03602 0.00370 0.00593 0.06290 0.00694 0.00071 0.00025 0.00054 0.00000 0.00213 0.00294 0.00239 0.00218 0.00176 0.00192 0.00115 H5A 0.55526 0.51231 0.51711 1.00000 0.09434 0.00000 0.00000 H5B 0.54458 0.56864 0.36428 1.00000 0.09434 0.00000 0.00000 H5C 0.36330 0.49824 0.37108 1.00000 0.09434 0.00000 0.00000 Final Structure Factor Calculation for 03SRC0102 in P2(1) Total number of l.s. parameters = 194 Maximum vector length = 511 Memory required = 2326 / 25046 wR2 = 0.1301 before cycle 5 for 2685 data and 2 / 194 parameters GooF = S = 0.761; Restrained GooF = 0.761 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1298 * P )^2 + 0.08 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0418 for 2315 Fo > 4sig(Fo) and 0.0538 for all 2685 data wR2 = 0.1301, GooF = S = 0.761, Restrained GooF = 0.761 for all data Flack x parameter = 0.1269 with esd 0.0984 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 Occupancy sum of asymmetric unit = 21.00 for non-hydrogen and 20.00 for hydrogen atoms Principal mean square atomic displacements U 0.0787 0.0320 0.0234 S1 0.0530 0.0342 0.0270 O3 0.0522 0.0334 0.0251 O2 0.0462 0.0358 0.0340 C14 0.0434 0.0247 0.0229 C9 0.0490 0.0426 0.0280 C11 0.0525 0.0286 0.0233 C12 0.1262 0.0397 0.0246 O4 0.0758 0.0361 0.0325 O1 0.0407 0.0363 0.0299 C8 0.0749 0.0507 0.0313 C15 0.0472 0.0439 0.0272 C13 0.0369 0.0317 0.0246 C7 0.0523 0.0383 0.0296 C10 0.0409 0.0362 0.0295 C3 0.1416 0.0459 0.0252 O5 0.0489 0.0325 0.0290 C4 0.0782 0.0522 0.0315 C6 0.1048 0.0513 0.0445 C1 0.0699 0.0461 0.0392 C2 0.1061 0.0524 0.0302 C5 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.028 0.043 0.055 0.070 0.084 0.103 0.129 0.163 0.221 1.000 Number in group 278. 259. 275. 263. 267. 276. 263. 268. 267. 269. GooF 0.814 0.908 0.914 0.874 0.832 0.734 0.705 0.606 0.577 0.523 K 0.988 0.974 0.984 1.014 0.994 1.030 1.018 1.014 1.021 1.007 Resolution(A) 0.84 0.88 0.91 0.96 1.01 1.07 1.15 1.27 1.45 1.82 inf Number in group 275. 271. 260. 279. 260. 276. 257. 268. 272. 267. GooF 0.872 0.896 0.841 0.792 0.755 0.735 0.648 0.651 0.716 0.641 K 1.051 1.077 1.015 1.006 1.016 1.012 1.011 1.009 1.027 1.002 R1 0.162 0.119 0.110 0.071 0.060 0.044 0.036 0.034 0.037 0.030 Recommended weighting scheme: WGHT 0.0628 0.0345 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) -3 -14 4 3.92 11.28 4.31 0.042 0.93 -1 -19 3 14.48 31.45 4.23 0.071 0.88 -3 15 4 -2.85 6.18 4.18 0.031 0.90 3 6 8 0.00 17.22 4.05 0.052 0.85 -4 -13 4 11.21 22.06 3.98 0.059 0.88 -3 6 2 153.05 234.60 3.90 0.193 1.45 2 14 3 0.00 6.77 3.50 0.033 1.06 4 -3 5 5.36 14.17 3.48 0.047 1.03 -4 -4 4 -1.98 5.45 3.39 0.029 1.10 2 -18 2 2.27 14.51 3.37 0.048 0.91 3 0 7 -0.98 5.68 3.31 0.030 0.98 2 10 6 27.71 12.93 3.30 0.045 1.00 2 -16 2 16.00 28.86 3.29 0.068 1.00 -1 -2 4 18.52 12.27 3.29 0.044 1.87 -6 0 2 149.06 97.34 3.25 0.124 0.89 2 -5 6 27.95 17.34 3.21 0.052 1.15 5 0 1 0.00 4.31 3.20 0.026 1.08 -4 5 3 24.33 42.24 3.10 0.082 1.16 -3 15 5 8.57 2.18 2.95 0.019 0.85 -3 -15 1 2.91 7.26 2.93 0.034 0.99 -4 2 6 17.08 25.98 2.93 0.064 0.96 0 16 5 2.85 15.62 2.93 0.050 0.92 -3 -1 8 25.27 14.75 2.90 0.048 0.89 3 -3 8 -0.73 4.51 2.86 0.027 0.88 4 -13 1 13.64 22.03 2.85 0.059 0.96 1 14 0 0.00 3.52 2.80 0.024 1.24 -4 -8 4 25.08 34.61 2.79 0.074 1.01 4 10 3 1.47 6.03 2.79 0.031 1.01 -2 9 8 40.06 25.60 2.77 0.064 0.86 2 17 0 22.97 37.85 2.77 0.077 0.98 -1 -8 5 21.43 30.34 2.76 0.069 1.28 -4 7 6 75.98 55.63 2.74 0.094 0.90 -3 12 4 68.36 49.41 2.74 0.088 1.00 3 1 8 0.00 5.37 2.74 0.029 0.89 -4 6 4 8.33 2.54 2.74 0.020 1.06 -1 -15 6 25.46 38.88 2.69 0.078 0.88 3 -10 3 8.15 12.67 2.69 0.045 1.15 0 -16 0 25.58 40.33 2.68 0.080 1.11 -1 13 5 11.58 5.44 2.66 0.029 1.03 -3 0 4 3.88 7.72 2.62 0.035 1.36 -1 -16 5 23.36 34.71 2.60 0.074 0.91 -2 15 1 90.58 68.12 2.60 0.104 1.08 -2 -18 2 31.16 44.38 2.59 0.084 0.91 5 7 4 37.02 23.94 2.57 0.062 0.90 -5 -1 6 82.53 54.99 2.57 0.093 0.85 3 -9 5 14.52 9.23 2.56 0.038 1.03 2 19 2 -2.77 7.70 2.55 0.035 0.87 -3 12 5 37.10 24.12 2.54 0.062 0.94 3 5 0 92.88 71.62 2.52 0.106 1.62 -5 -5 3 61.35 45.90 2.48 0.085 0.98 Bond lengths and angles S1 - Distance Angles O5 1.4130 (0.0031) O4 1.4267 (0.0029) 119.31 (0.19) O3 1.5707 (0.0021) 103.93 (0.15) 108.90 (0.13) C9 1.7495 (0.0027) 110.37 (0.16) 108.82 (0.15) 104.40 (0.12) S1 - O5 O4 O3 O3 - Distance Angles C8 1.4538 (0.0037) S1 1.5707 (0.0020) 118.91 (0.19) O3 - C8 O2 - Distance Angles C7 1.4152 (0.0034) C4 1.4268 (0.0038) 105.94 (0.21) O2 - C7 C14 - Distance Angles C13 1.3730 (0.0043) C9 1.3799 (0.0041) 118.96 (0.28) C14 - C13 C9 - Distance Angles C10 1.3752 (0.0045) C14 1.3799 (0.0041) 121.45 (0.28) S1 1.7495 (0.0027) 119.63 (0.23) 118.87 (0.22) C9 - C10 C14 C11 - Distance Angles C12 1.3771 (0.0047) C10 1.3865 (0.0044) 121.53 (0.29) C11 - C12 C12 - Distance Angles C11 1.3771 (0.0047) C13 1.3838 (0.0046) 118.48 (0.27) C15 1.5024 (0.0044) 120.62 (0.30) 120.90 (0.30) C12 - C11 C13 O4 - Distance Angles S1 1.4267 (0.0029) O4 - O1 - Distance Angles C4 1.4129 (0.0038) C3 1.4226 (0.0039) 109.85 (0.22) O1 - C4 C8 - Distance Angles O3 1.4538 (0.0037) C7 1.4883 (0.0041) 105.21 (0.24) C8 - O3 C15 - Distance Angles C12 1.5024 (0.0044) C15 - C13 - Distance Angles C14 1.3730 (0.0043) C12 1.3838 (0.0046) 121.26 (0.27) C13 - C14 C7 - Distance Angles O2 1.4152 (0.0034) C8 1.4883 (0.0041) 108.84 (0.23) C3 1.5523 (0.0041) 103.58 (0.23) 116.24 (0.25) C7 - O2 C8 C10 - Distance Angles C9 1.3752 (0.0045) C11 1.3865 (0.0044) 118.32 (0.29) C10 - C9 C3 - Distance Angles O1 1.4226 (0.0039) C2 1.4925 (0.0049) 108.26 (0.27) C7 1.5523 (0.0041) 103.27 (0.23) 115.63 (0.29) C3 - O1 C2 O5 - Distance Angles S1 1.4130 (0.0031) O5 - C4 - Distance Angles O1 1.4129 (0.0038) O2 1.4268 (0.0038) 104.75 (0.23) C5 1.4960 (0.0046) 109.74 (0.29) 108.51 (0.27) C6 1.5157 (0.0052) 109.06 (0.27) 111.06 (0.29) 113.36 (0.31) C4 - O1 O2 C5 C6 - Distance Angles C4 1.5157 (0.0052) C6 - C1 - Distance Angles C2 1.3060 (0.0065) C1 - C2 - Distance Angles C1 1.3060 (0.0065) C3 1.4925 (0.0049) 124.05 (0.43) C2 - C1 C5 - Distance Angles C4 1.4960 (0.0046) C5 - FMAP and GRID set by program FMAP 2 1 14 GRID -4.545 -2 -2 4.545 2 2 R1 = 0.0433 for 1453 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.21 at 0.2635 0.6180 0.3833 [ 0.94 A from C6 ] Deepest hole -0.23 at 0.3924 0.2247 -0.0020 [ 0.91 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 2395 / 17566 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2635 0.6180 0.3833 1.00000 0.05 0.21 0.94 C6 0.96 H6B 1.30 C4 1.44 H6A Q2 1 0.5929 0.7854 1.0908 1.00000 0.05 0.20 0.86 C9 0.90 S1 1.88 O4 1.91 C14 Q3 1 0.9874 0.7210 1.0586 1.00000 0.05 0.16 0.88 O4 1.72 H8A 2.03 S1 2.53 C8 Q4 1 -0.1000 0.6390 0.5080 1.00000 0.05 0.16 0.57 H6C 1.38 C6 1.79 H6A 2.14 H6B Q5 1 -0.0036 0.8784 1.6068 1.00000 0.05 0.14 0.79 H15C 0.85 C15 0.91 H15A 1.66 H15B Q6 1 0.2654 0.8396 1.0176 1.00000 0.05 0.14 0.47 H10 1.17 C10 1.97 C9 2.36 O3 Q7 1 0.2647 0.5805 1.0981 1.00000 0.05 0.14 1.76 H8A 1.99 H8B 1.99 C2 2.10 C1 Q8 1 0.4659 0.5004 0.5235 1.00000 0.05 0.13 0.54 H5A 0.96 C5 1.36 H5C 1.83 H5B Q9 1 0.7406 0.7230 0.7539 1.00000 0.05 0.13 1.87 O3 2.13 H7 2.18 H13 2.21 S1 Q10 1 0.7742 0.7355 0.7785 1.00000 0.05 0.13 1.90 O3 1.99 S1 2.06 H7 2.10 O5 Q11 1 0.2165 0.6254 0.6260 1.00000 0.05 0.13 0.95 O2 1.15 C4 1.19 C7 1.53 H7 Q12 1 0.7767 0.7684 1.3348 1.00000 0.05 0.13 0.41 H14 0.98 C14 2.02 C13 2.03 C9 Q13 1 0.2974 0.5210 0.9436 1.00000 0.05 0.13 0.50 H2 0.95 C2 1.88 C1 2.09 C3 Q14 1 0.8317 0.7640 1.0089 1.00000 0.05 0.13 0.92 S1 0.94 O4 1.55 O5 2.31 O3 Q15 1 1.0037 0.7760 0.9651 1.00000 0.05 0.13 1.59 O4 1.77 O5 1.86 S1 2.10 H10 Q16 1 0.2245 0.5426 0.6528 1.00000 0.05 0.12 0.66 O1 1.29 C4 1.44 C3 1.82 O2 Q17 1 0.6323 0.7975 1.2351 1.00000 0.05 0.12 0.83 C14 0.83 C9 1.33 H14 2.00 S1 Q18 1 0.0446 0.7019 0.8428 1.00000 0.05 0.12 1.02 H7 1.52 C7 1.84 H8A 1.90 C8 Q19 1 0.1399 0.8644 1.7110 1.00000 0.05 0.12 0.77 H15B 0.87 C15 0.99 H15C 1.50 H15A Q20 1 0.1194 0.5822 0.4930 1.00000 0.05 0.12 0.82 C4 1.08 C6 1.33 O1 1.45 H6A Shortest distances between peaks (including symmetry equivalents) 9 10 0.35 14 15 1.03 5 19 1.18 3 14 1.21 2 17 1.21 12 17 1.24 3 15 1.24 1 20 1.36 11 20 1.43 11 16 1.49 2 14 1.52 4 20 1.57 16 20 1.58 7 13 1.66 15 18 1.67 10 18 1.67 3 18 1.82 9 18 1.85 8 16 1.85 6 15 1.87 10 14 1.97 4 11 1.99 1 11 2.00 10 15 2.09 14 18 2.11 2 6 2.12 14 17 2.23 2 12 2.24 9 14 2.25 1 4 2.27 8 20 2.40 1 7 2.42 9 15 2.43 11 18 2.43 13 16 2.43 2 3 2.46 2 15 2.48 3 10 2.57 1 16 2.58 6 19 2.62 3 6 2.63 1 8 2.63 4 9 2.65 3 12 2.67 12 14 2.68 15 19 2.71 6 14 2.73 4 16 2.73 8 11 2.75 6 17 2.77 3 17 2.78 4 12 2.78 3 9 2.82 2 10 2.88 4 10 2.88 3 7 2.94 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 0.06: Analyse other restraints etc. 0.44: 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 1.58: Structure factors and derivatives 1.06: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.09: Apply other restraints 0.05: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.17: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 08:59:08 Total elapsed time: 3.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++