+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 10:21:40 on 03-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 00SRC001 in P2(1)/n CELL 0.71073 12.7323 13.1306 13.0397 90.000 96.876 90.000 ZERR 4.00 0.0025 0.0026 0.0026 0.000 0.030 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H O S UNIT 84 80 20 12 V = 2164.33 F(000) = 936.0 Mu = 0.37 mm-1 Cell Wt = 1794.20 Rho = 1.377 L.S. 4 BOND FMAP 2 PLAN 10 WGHT 0.0784 0.0000 FVAR 0.30718 S1 4 1.043962 0.145037 0.479278 11.00000 0.03740 0.10259 = 0.11161 -0.01124 0.01394 -0.00628 S2 4 0.861889 0.140213 0.601744 11.00000 0.04409 0.07277 = 0.05831 -0.00338 0.00007 0.00078 S3 4 0.824860 0.108886 0.381114 11.00000 0.03877 0.06527 = 0.05691 -0.00052 0.01182 0.00195 O1 3 0.664485 0.149218 0.706818 11.00000 0.06865 0.12087 = 0.05758 -0.01545 0.01567 -0.00245 O2 3 0.618354 -0.097391 0.356757 11.00000 0.07258 0.04340 = 0.05207 0.00462 0.01436 0.00577 O3 3 0.645076 -0.087656 -0.002078 11.00000 0.07380 0.09439 = 0.04968 -0.01027 0.01107 0.00529 O4 3 0.389738 0.133360 0.365483 11.00000 0.03268 0.04777 = 0.08203 0.00209 0.00509 -0.00433 O5 3 0.403633 0.494115 0.356045 11.00000 0.05750 0.04422 = 0.10583 -0.00236 0.00780 0.01006 C1 1 0.917369 0.132927 0.488174 11.00000 0.03561 0.05603 = 0.06899 0.00039 0.00570 0.00308 C2 1 0.730853 0.124403 0.547870 11.00000 0.04033 0.04884 = 0.05217 -0.00025 0.00700 0.00015 C3 1 0.713050 0.111500 0.444072 11.00000 0.03644 0.03841 = 0.05218 0.00252 0.01027 0.00141 C4 1 0.647780 0.130274 0.615732 11.00000 0.05121 0.06774 = 0.05512 -0.00656 0.01048 0.00134 AFIX 43 H4 2 0.578279 0.118805 0.587263 11.00000 -1.20000 AFIX 0 C5 1 0.605268 0.108178 0.379796 11.00000 0.03157 0.04171 = 0.05558 -0.00017 0.00794 -0.00038 AFIX 13 H5 2 0.560053 0.063609 0.415897 11.00000 -1.20000 AFIX 0 C6 1 0.613262 0.060584 0.274033 11.00000 0.03387 0.04628 = 0.05089 -0.00011 0.00482 0.00046 C7 1 0.620801 -0.045073 0.266139 11.00000 0.03794 0.04696 = 0.05159 0.00092 0.00690 0.00200 C8 1 0.630222 -0.091002 0.172699 11.00000 0.04622 0.04989 = 0.05716 -0.00555 0.01007 0.00347 AFIX 43 H8 2 0.633579 -0.161601 0.168383 11.00000 -1.20000 AFIX 0 C9 1 0.634705 -0.032116 0.085098 11.00000 0.03854 0.07360 = 0.05133 -0.00334 0.00694 0.00386 C10 1 0.626953 0.072757 0.090678 11.00000 0.05367 0.07352 = 0.05035 0.01198 0.00683 0.00006 AFIX 43 H10 2 0.629805 0.112612 0.032119 11.00000 -1.20000 AFIX 0 C11 1 0.614951 0.117333 0.184165 11.00000 0.05078 0.05065 = 0.06098 0.00622 0.00552 -0.00165 AFIX 43 H11 2 0.607737 0.187706 0.187318 11.00000 -1.20000 AFIX 0 C12 1 0.632105 -0.203675 0.354287 11.00000 0.14751 0.04856 = 0.07937 0.01059 0.03427 0.01573 AFIX 137 H12A 2 0.582014 -0.232474 0.301302 11.00000 -1.50000 H12B 2 0.621068 -0.232108 0.419973 11.00000 -1.50000 H12C 2 0.702612 -0.218941 0.339901 11.00000 -1.50000 AFIX 0 C13 1 0.650576 -0.032237 -0.095525 11.00000 0.07604 0.13314 = 0.05755 -0.00803 0.02260 -0.01536 AFIX 137 H13A 2 0.591729 0.013779 -0.106720 11.00000 -1.50000 H13B 2 0.648251 -0.078948 -0.152389 11.00000 -1.50000 H13C 2 0.715446 0.005710 -0.090281 11.00000 -1.50000 AFIX 0 C14 1 0.554636 0.213767 0.374322 11.00000 0.03645 0.04444 = 0.05085 -0.00199 0.00716 0.00040 C15 1 0.444784 0.222931 0.367387 11.00000 0.03774 0.04540 = 0.03972 -0.00180 0.00776 -0.00374 C16 1 0.397505 0.317974 0.363049 11.00000 0.03423 0.05350 = 0.04962 -0.00190 0.00505 0.00362 AFIX 43 H16 2 0.324420 0.323549 0.360474 11.00000 -1.20000 AFIX 0 C17 1 0.459287 0.404856 0.362548 11.00000 0.04471 0.04539 = 0.05625 -0.00464 0.00360 0.00597 C18 1 0.567091 0.397968 0.368842 11.00000 0.04442 0.04342 = 0.09079 -0.00291 0.00405 -0.00527 AFIX 43 H18 2 0.608667 0.456197 0.368777 11.00000 -1.20000 AFIX 0 C19 1 0.612794 0.301967 0.375319 11.00000 0.03487 0.05009 = 0.09971 0.00065 0.00814 -0.00191 AFIX 43 H19 2 0.686110 0.297070 0.380575 11.00000 -1.20000 AFIX 0 C20 1 0.276780 0.139061 0.355032 11.00000 0.03763 0.06734 = 0.12338 0.00488 0.00855 -0.01004 AFIX 137 H20A 2 0.254821 0.171786 0.414763 11.00000 -1.50000 H20B 2 0.247678 0.071583 0.348931 11.00000 -1.50000 H20C 2 0.252025 0.177639 0.294388 11.00000 -1.50000 AFIX 0 C21 1 0.461031 0.585906 0.348623 11.00000 0.08821 0.04447 = 0.10079 0.00372 0.00133 0.00431 AFIX 137 H21A 2 0.516264 0.590229 0.405421 11.00000 -1.50000 H21B 2 0.414123 0.642919 0.350650 11.00000 -1.50000 H21C 2 0.491542 0.586677 0.284775 11.00000 -1.50000 HKLF 4 Covalent radii and connectivity table for 00SRC001 in P2(1)/n C 0.770 H 0.320 O 0.660 S 1.030 S1 - C1 S2 - C1 C2 S3 - C3 C1 O1 - C4 O2 - C7 C12 O3 - C9 C13 O4 - C15 C20 O5 - C17 C21 C1 - S1 S2 S3 C2 - C3 C4 S2 C3 - C2 C5 S3 C4 - O1 C2 C5 - C3 C14 C6 C6 - C11 C7 C5 C7 - O2 C8 C6 C8 - C7 C9 C9 - O3 C10 C8 C10 - C11 C9 C11 - C10 C6 C12 - O2 C13 - O3 C14 - C19 C15 C5 C15 - O4 C16 C14 C16 - C15 C17 C17 - O5 C18 C16 C18 - C17 C19 C19 - C14 C18 C20 - O4 C21 - O5 h k l Fo^2 Sigma Why rejected 0 3 0 0.44 0.11 observed but should be systematically absent 16818 Reflections read, of which 376 rejected -16 =< h =< 16, -15 =< k =< 17, -13 =< l =< 16, Max. 2-theta = 55.07 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 1 0 22.48 0.38 4 8.29 2 4 0 62.18 0.89 4 11.30 -1 0 1 33.83 1.55 2 17.56 0 1 1 74.73 0.31 5 63.60 -3 8 1 32.04 0.22 5 8.46 2 8 1 10.13 0.63 4 3.19 8 10 4 0.62 0.15 4 1.37 5 12 6 7.80 1.63 2 29.59 6 10 7 1.12 0.42 3 3.85 -12 7 8 6.05 1.44 3 7.83 9 0 9 1.00 1.18 2 6.59 8 4 11 4.40 1.24 3 6.58 -5 9 11 2.43 1.00 4 5.44 13 Inconsistent equivalents 4938 Unique reflections, of which 0 suppressed R(int) = 0.0533 R(sigma) = 0.0606 Friedel opposites merged Maximum memory for data reduction = 2328 / 48662 Default effective X-H distances for T = 20.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 0.98 0.97 0.96 0.93 0.86 0.89 1.10 0.82 0.93 0.86 0.93 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 = 3062 / 330890 wR2 = 0.1433 before cycle 1 for 4938 data and 266 / 266 parameters GooF = S = 0.990; Restrained GooF = 0.990 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0784 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.30746 0.00069 0.406 OSF Mean shift/esd = 0.115 Maximum = 0.406 for OSF Max. shift = 0.008 A for H20C Max. dU = 0.000 for C19 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3062 / 330890 wR2 = 0.1432 before cycle 2 for 4938 data and 266 / 266 parameters GooF = S = 0.991; Restrained GooF = 0.991 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0784 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.30741 0.00069 -0.066 OSF Mean shift/esd = 0.038 Maximum = -0.199 for tors H20A Max. shift = 0.004 A for H20C Max. dU = 0.000 for C13 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3062 / 330890 wR2 = 0.1432 before cycle 3 for 4938 data and 266 / 266 parameters GooF = S = 0.991; Restrained GooF = 0.991 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0784 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.30741 0.00069 -0.002 OSF Mean shift/esd = 0.004 Maximum = -0.038 for tors H20A Max. shift = 0.001 A for H20B Max. dU = 0.000 for C13 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3062 / 330890 wR2 = 0.1432 before cycle 4 for 4938 data and 266 / 266 parameters GooF = S = 0.991; Restrained GooF = 0.991 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0784 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.30742 0.00069 0.006 OSF Mean shift/esd = 0.002 Maximum = 0.008 for U22 S2 Max. shift = 0.000 A for H20B Max. dU = 0.000 for C13 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H4 0.5784 0.1187 0.5872 43 0.930 0.000 C4 O1 C2 H5 0.5601 0.0635 0.4158 13 0.980 0.000 C5 C3 C14 C6 H8 0.6337 -0.1616 0.1684 43 0.930 0.000 C8 C7 C9 H10 0.6299 0.1126 0.0321 43 0.930 0.000 C10 C11 C9 H11 0.6078 0.1876 0.1874 43 0.930 0.000 C11 C10 C6 H12A 0.5820 -0.2324 0.3013 137 0.960 0.000 C12 O2 H12A H12B 0.6212 -0.2321 0.4200 137 0.960 0.000 C12 O2 H12A H12C 0.7026 -0.2188 0.3398 137 0.960 0.000 C12 O2 H12A H13A 0.5914 0.0134 -0.1070 137 0.960 0.000 C13 O3 H13A H13B 0.6489 -0.0790 -0.1523 137 0.960 0.000 C13 O3 H13A H13C 0.7152 0.0062 -0.0900 137 0.960 0.000 C13 O3 H13A H16 0.3244 0.3235 0.3603 43 0.930 0.000 C16 C15 C17 H18 0.6086 0.4562 0.3686 43 0.930 0.000 C18 C17 C19 H19 0.6861 0.2971 0.3807 43 0.930 0.000 C19 C14 C18 H20A 0.2549 0.1710 0.4153 137 0.960 0.000 C20 O4 H20A H20B 0.2476 0.0717 0.3480 137 0.960 0.000 C20 O4 H20A H20C 0.2521 0.1785 0.2950 137 0.960 0.000 C20 O4 H20A H21A 0.5158 0.5906 0.4058 137 0.960 0.000 C21 O5 H21A H21B 0.4140 0.6429 0.3499 137 0.960 0.000 C21 O5 H21A H21C 0.4922 0.5863 0.2851 137 0.960 0.000 C21 O5 H21A 00SRC001 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S1 1.04396 0.14506 0.47927 1.00000 0.03748 0.10262 0.11165 -0.01135 0.01383 -0.00641 0.08352 0.00144 0.00006 0.00006 0.00007 0.00000 0.00041 0.00061 0.00072 0.00044 0.00041 0.00035 0.00029 S2 0.86190 0.14022 0.60175 1.00000 0.04417 0.07265 0.05827 -0.00334 0.00000 0.00077 0.05886 0.00116 0.00005 0.00005 0.00005 0.00000 0.00039 0.00043 0.00043 0.00029 0.00030 0.00029 0.00021 S3 0.82485 0.10889 0.38112 1.00000 0.03878 0.06527 0.05689 -0.00053 0.01171 0.00190 0.05316 0.00111 0.00005 0.00004 0.00005 0.00000 0.00035 0.00038 0.00041 0.00027 0.00029 0.00026 0.00020 O1 0.66452 0.14926 0.70684 1.00000 0.06889 0.12110 0.05704 -0.01542 0.01541 -0.00270 0.08170 0.00368 0.00016 0.00015 0.00016 0.00000 0.00140 0.00158 0.00136 0.00107 0.00105 0.00112 0.00059 O2 0.61835 -0.09741 0.35677 1.00000 0.07243 0.04331 0.05186 0.00447 0.01429 0.00582 0.05531 0.00302 0.00014 0.00010 0.00012 0.00000 0.00121 0.00082 0.00100 0.00067 0.00085 0.00072 0.00044 O3 0.64505 -0.08764 -0.00208 1.00000 0.07372 0.09432 0.04958 -0.01011 0.01104 0.00509 0.07224 0.00329 0.00015 0.00014 0.00013 0.00000 0.00137 0.00128 0.00112 0.00093 0.00096 0.00099 0.00052 O4 0.38972 0.13335 0.36548 1.00000 0.03254 0.04762 0.08189 0.00204 0.00493 -0.00464 0.05417 0.00283 0.00012 0.00010 0.00014 0.00000 0.00086 0.00084 0.00125 0.00074 0.00081 0.00065 0.00043 O5 0.40366 0.49413 0.35609 1.00000 0.05717 0.04400 0.10599 -0.00220 0.00753 0.01003 0.06924 0.00321 0.00013 0.00011 0.00015 0.00000 0.00109 0.00091 0.00148 0.00083 0.00100 0.00078 0.00051 C1 0.91741 0.13293 0.48822 1.00000 0.03567 0.05541 0.06920 0.00032 0.00550 0.00312 0.05349 0.00437 0.00019 0.00016 0.00020 0.00000 0.00130 0.00130 0.00172 0.00110 0.00119 0.00101 0.00061 C2 0.73085 0.12437 0.54783 1.00000 0.03978 0.04869 0.05210 -0.00016 0.00694 -0.00003 0.04674 0.00397 0.00018 0.00015 0.00018 0.00000 0.00133 0.00119 0.00152 0.00096 0.00110 0.00094 0.00055 C3 0.71304 0.11149 0.44408 1.00000 0.03629 0.03817 0.05234 0.00266 0.01024 0.00151 0.04187 0.00388 0.00017 0.00014 0.00017 0.00000 0.00122 0.00106 0.00146 0.00088 0.00103 0.00084 0.00052 C4 0.64786 0.13023 0.61570 1.00000 0.05095 0.06720 0.05523 -0.00628 0.01016 0.00122 0.05749 0.00476 0.00021 0.00017 0.00021 0.00000 0.00159 0.00149 0.00174 0.00116 0.00131 0.00116 0.00064 H4 0.57837 0.11868 0.58725 1.00000 0.06898 0.00000 0.00000 C5 0.60530 0.10811 0.37976 1.00000 0.03141 0.04143 0.05548 -0.00024 0.00796 -0.00034 0.04255 0.00378 0.00017 0.00014 0.00017 0.00000 0.00116 0.00113 0.00143 0.00090 0.00101 0.00086 0.00052 H5 0.56008 0.06353 0.41585 1.00000 0.05106 0.00000 0.00000 C6 0.61327 0.06058 0.27404 1.00000 0.03353 0.04637 0.05042 -0.00031 0.00463 0.00031 0.04347 0.00373 0.00016 0.00015 0.00017 0.00000 0.00119 0.00113 0.00137 0.00094 0.00098 0.00091 0.00051 C7 0.62081 -0.04504 0.26612 1.00000 0.03788 0.04685 0.05091 0.00106 0.00700 0.00192 0.04507 0.00388 0.00017 0.00015 0.00017 0.00000 0.00126 0.00116 0.00143 0.00097 0.00102 0.00092 0.00053 C8 0.63028 -0.09097 0.17271 1.00000 0.04618 0.04986 0.05683 -0.00535 0.00995 0.00369 0.05065 0.00408 0.00018 0.00016 0.00018 0.00000 0.00141 0.00124 0.00155 0.00106 0.00115 0.00101 0.00058 H8 0.63370 -0.16156 0.16841 1.00000 0.06078 0.00000 0.00000 C9 0.63471 -0.03214 0.08518 1.00000 0.03841 0.07343 0.05103 -0.00359 0.00686 0.00384 0.05417 0.00431 0.00018 0.00018 0.00019 0.00000 0.00133 0.00160 0.00149 0.00119 0.00111 0.00108 0.00060 C10 0.62699 0.07271 0.09067 1.00000 0.05366 0.07318 0.05026 0.01191 0.00684 0.00003 0.05898 0.00453 0.00019 0.00019 0.00019 0.00000 0.00159 0.00160 0.00154 0.00120 0.00122 0.00125 0.00064 H10 0.62986 0.11256 0.03211 1.00000 0.07078 0.00000 0.00000 C11 0.61497 0.11724 0.18423 1.00000 0.05053 0.05022 0.06110 0.00587 0.00544 -0.00160 0.05405 0.00445 0.00020 0.00017 0.00020 0.00000 0.00150 0.00124 0.00165 0.00108 0.00124 0.00104 0.00061 H11 0.60776 0.18761 0.18739 1.00000 0.06486 0.00000 0.00000 C12 0.63216 -0.20361 0.35426 1.00000 0.14706 0.04833 0.07962 0.01058 0.03374 0.01570 0.09004 0.00601 0.00029 0.00017 0.00024 0.00000 0.00323 0.00148 0.00212 0.00127 0.00206 0.00164 0.00106 H12A 0.58201 -0.23243 0.30133 1.00000 0.13505 0.00000 0.00000 H12B 0.62125 -0.23207 0.41997 1.00000 0.13505 0.00000 0.00000 H12C 0.70264 -0.21883 0.33976 1.00000 0.13505 0.00000 0.00000 C13 0.65059 -0.03225 -0.09549 1.00000 0.07656 0.13407 0.05716 -0.00821 0.02264 -0.01561 0.08808 0.00563 0.00025 0.00025 0.00021 0.00000 0.00219 0.00272 0.00195 0.00169 0.00160 0.00187 0.00095 H13A 0.59142 0.01335 -0.10702 1.00000 0.13212 0.00000 0.00000 H13B 0.64890 -0.07900 -0.15227 1.00000 0.13212 0.00000 0.00000 H13C 0.71518 0.00616 -0.09000 1.00000 0.13212 0.00000 0.00000 C14 0.55462 0.21377 0.37431 1.00000 0.03632 0.04421 0.05091 -0.00199 0.00708 0.00043 0.04366 0.00369 0.00016 0.00015 0.00016 0.00000 0.00125 0.00115 0.00138 0.00091 0.00101 0.00091 0.00052 C15 0.44478 0.22291 0.36743 1.00000 0.03788 0.04555 0.03936 -0.00170 0.00762 -0.00361 0.04069 0.00353 0.00016 0.00015 0.00016 0.00000 0.00122 0.00113 0.00122 0.00086 0.00094 0.00094 0.00049 C16 0.39753 0.31796 0.36301 1.00000 0.03374 0.05316 0.04986 -0.00205 0.00482 0.00366 0.04560 0.00386 0.00017 0.00015 0.00017 0.00000 0.00120 0.00125 0.00139 0.00097 0.00102 0.00098 0.00053 H16 0.32444 0.32355 0.36035 1.00000 0.05472 0.00000 0.00000 C17 0.45930 0.40479 0.36255 1.00000 0.04457 0.04551 0.05578 -0.00463 0.00355 0.00621 0.04882 0.00399 0.00018 0.00015 0.00018 0.00000 0.00143 0.00123 0.00150 0.00096 0.00112 0.00102 0.00057 C18 0.56705 0.39798 0.36880 1.00000 0.04445 0.04316 0.09109 -0.00277 0.00380 -0.00503 0.05992 0.00448 0.00020 0.00016 0.00021 0.00000 0.00149 0.00127 0.00202 0.00113 0.00136 0.00103 0.00069 H18 0.60859 0.45623 0.36865 1.00000 0.07190 0.00000 0.00000 C19 0.61279 0.30197 0.37536 1.00000 0.03478 0.04985 0.09907 0.00035 0.00823 -0.00168 0.06122 0.00441 0.00018 0.00016 0.00021 0.00000 0.00133 0.00140 0.00213 0.00121 0.00132 0.00104 0.00070 H19 0.68611 0.29708 0.38071 1.00000 0.07346 0.00000 0.00000 C20 0.27679 0.13910 0.35509 1.00000 0.03750 0.06739 0.12346 0.00499 0.00817 -0.01028 0.07624 0.00525 0.00020 0.00018 0.00028 0.00000 0.00151 0.00159 0.00273 0.00159 0.00157 0.00122 0.00087 H20A 0.25485 0.17096 0.41528 1.00000 0.11435 0.00000 0.00000 H20B 0.24763 0.07169 0.34801 1.00000 0.11435 0.00000 0.00000 H20C 0.25208 0.17851 0.29501 1.00000 0.11435 0.00000 0.00000 C21 0.46104 0.58590 0.34861 1.00000 0.08807 0.04468 0.10013 0.00364 0.00144 0.00426 0.07842 0.00524 0.00025 0.00017 0.00024 0.00000 0.00229 0.00139 0.00233 0.00133 0.00182 0.00139 0.00088 H21A 0.51581 0.59059 0.40579 1.00000 0.11763 0.00000 0.00000 H21B 0.41398 0.64288 0.34988 1.00000 0.11763 0.00000 0.00000 H21C 0.49215 0.58631 0.28508 1.00000 0.11763 0.00000 0.00000 Final Structure Factor Calculation for 00SRC001 in P2(1)/n Total number of l.s. parameters = 266 Maximum vector length = 511 Memory required = 2796 / 22995 wR2 = 0.1432 before cycle 5 for 4938 data and 0 / 266 parameters GooF = S = 0.991; Restrained GooF = 0.991 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0784 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0493 for 2899 Fo > 4sig(Fo) and 0.1006 for all 4938 data wR2 = 0.1432, GooF = S = 0.991, Restrained GooF = 0.991 for all data Occupancy sum of asymmetric unit = 29.00 for non-hydrogen and 20.00 for hydrogen atoms Principal mean square atomic displacements U 0.1195 0.0952 0.0359 S1 0.0737 0.0604 0.0425 S2 0.0654 0.0581 0.0360 S3 0.1248 0.0708 0.0496 O1 0.0751 0.0495 0.0413 O2 0.0976 0.0733 0.0459 O3 0.0826 0.0488 0.0312 O4 0.1067 0.0626 0.0384 O5 0.0694 0.0559 0.0351 C1 0.0521 0.0487 0.0394 C2 0.0538 0.0377 0.0341 C3 0.0699 0.0555 0.0470 C4 0.0556 0.0414 0.0307 C5 0.0506 0.0464 0.0335 C6 0.0513 0.0468 0.0371 C7 0.0598 0.0515 0.0407 C8 0.0745 0.0506 0.0374 C9 0.0783 0.0537 0.0450 C10 0.0642 0.0509 0.0471 C11 0.1534 0.0722 0.0445 C12 0.1391 0.0778 0.0473 C13 0.0515 0.0438 0.0357 C14 0.0476 0.0397 0.0347 C15 0.0549 0.0489 0.0330 C16 0.0598 0.0482 0.0385 C17 0.0923 0.0489 0.0386 C18 0.0993 0.0500 0.0343 C19 0.1246 0.0701 0.0340 C20 0.1070 0.0843 0.0440 C21 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.005 0.010 0.016 0.021 0.028 0.036 0.048 0.068 0.114 1.000 Number in group 514. 513. 527. 456. 514. 441. 501. 486. 491. 495. GooF 0.783 0.829 0.958 0.958 1.099 1.041 1.160 1.065 1.012 0.961 K 1.405 0.992 0.980 1.005 0.966 0.988 0.997 0.991 1.029 1.005 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.65 inf Number in group 504. 500. 485. 486. 495. 497. 493. 495. 488. 495. GooF 0.865 0.783 0.836 0.839 0.951 1.000 1.052 0.983 1.064 1.398 K 1.011 1.044 1.037 1.025 1.033 1.016 1.036 1.051 1.040 0.982 R1 0.379 0.315 0.242 0.184 0.133 0.100 0.069 0.048 0.041 0.037 Recommended weighting scheme: WGHT 0.0764 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 2 1 12.86 21.80 5.39 0.021 5.21 6 0 0 176.20 107.31 5.37 0.047 2.11 -4 6 1 10.93 0.88 4.88 0.004 1.80 2 5 0 19.37 6.73 4.72 0.012 2.43 0 2 1 72.57 50.77 4.62 0.032 5.86 -8 2 1 37.17 66.31 4.58 0.037 1.55 -1 5 3 19.61 34.43 4.52 0.026 2.23 2 6 0 28.39 13.69 4.44 0.017 2.07 2 7 0 56.01 87.89 4.33 0.042 1.80 -1 3 3 3.38 10.38 4.12 0.014 3.05 0 1 1 790.77 3558.44 4.08 0.268 9.22 -2 3 6 102.41 147.81 4.03 0.055 1.91 0 6 0 966.25 711.73 3.97 0.120 2.19 0 1 7 62.77 37.82 3.93 0.028 1.83 -3 4 2 91.51 128.14 3.90 0.051 2.47 8 10 0 71.56 113.70 3.66 0.048 1.01 5 1 1 136.07 185.64 3.58 0.061 2.39 -4 4 9 -0.54 20.00 3.57 0.020 1.27 -2 1 6 66.57 42.34 3.42 0.029 2.09 2 7 1 641.17 491.40 3.38 0.100 1.77 0 10 7 1.72 13.99 3.36 0.017 1.07 2 6 5 53.34 76.05 3.34 0.039 1.59 -2 7 5 111.75 83.85 3.34 0.041 1.50 -3 5 4 43.75 61.55 3.33 0.035 1.89 -3 0 1 76.88 105.47 3.26 0.046 4.16 3 6 2 185.75 139.07 3.24 0.053 1.83 0 3 6 10.56 20.39 3.23 0.020 1.94 -2 4 5 11.53 3.90 3.23 0.009 1.99 3 1 5 99.58 73.98 3.19 0.039 2.07 -3 10 4 63.79 88.03 3.16 0.042 1.18 -11 9 8 139.26 76.31 3.13 0.039 0.82 4 7 2 386.86 293.70 3.10 0.077 1.54 -7 2 10 11.51 40.61 3.10 0.029 1.10 -1 2 10 20.32 6.84 3.07 0.012 1.28 1 11 8 18.45 34.69 3.07 0.026 0.95 6 0 4 64.47 41.82 3.06 0.029 1.68 1 4 11 133.53 178.99 3.01 0.060 1.09 -15 3 2 84.70 33.59 3.00 0.026 0.83 4 6 3 5.52 12.24 2.99 0.016 1.62 -2 10 6 24.60 37.81 2.97 0.028 1.12 -6 2 13 86.18 36.25 2.92 0.027 0.94 -5 12 4 -1.70 7.74 2.91 0.013 0.97 9 4 5 115.05 155.45 2.91 0.056 1.11 -4 4 7 69.42 92.46 2.89 0.043 1.50 5 2 2 302.58 240.62 2.88 0.070 2.14 -2 6 7 61.63 83.91 2.85 0.041 1.41 6 11 6 1.61 34.62 2.84 0.026 0.91 2 8 8 15.94 3.63 2.84 0.009 1.12 -2 6 10 60.15 82.41 2.82 0.041 1.12 -4 11 5 62.17 84.43 2.82 0.041 1.04 Bond lengths and angles S1 - Distance Angles C1 1.6371 (0.0024) S1 - S2 - Distance Angles C1 1.7178 (0.0027) C2 1.7438 (0.0024) 96.80 (0.12) S2 - C1 S3 - Distance Angles C3 1.7268 (0.0022) C1 1.7449 (0.0026) 97.59 (0.11) S3 - C3 O1 - Distance Angles C4 1.2080 (0.0031) O1 - O2 - Distance Angles C7 1.3711 (0.0025) C12 1.4064 (0.0026) 117.48 (0.18) O2 - C7 O3 - Distance Angles C9 1.3709 (0.0028) C13 1.4277 (0.0031) 117.18 (0.22) O3 - C9 O4 - Distance Angles C15 1.3678 (0.0024) C20 1.4299 (0.0029) 117.62 (0.17) O4 - C15 O5 - Distance Angles C17 1.3677 (0.0024) C21 1.4185 (0.0028) 117.75 (0.20) O5 - C17 C1 - Distance Angles S1 1.6371 (0.0024) S2 1.7178 (0.0027) 124.47 (0.16) S3 1.7449 (0.0026) 122.46 (0.16) 113.06 (0.13) C1 - S1 S2 C2 - Distance Angles C3 1.3552 (0.0032) C4 1.4594 (0.0033) 124.41 (0.22) S2 1.7438 (0.0024) 117.07 (0.18) 118.46 (0.18) C2 - C3 C4 C3 - Distance Angles C2 1.3552 (0.0032) C5 1.5205 (0.0030) 125.90 (0.20) S3 1.7268 (0.0022) 115.35 (0.17) 118.55 (0.16) C3 - C2 C5 C4 - Distance Angles O1 1.2080 (0.0031) C2 1.4594 (0.0033) 123.57 (0.25) C4 - O1 C5 - Distance Angles C3 1.5205 (0.0030) C14 1.5282 (0.0027) 110.32 (0.16) C6 1.5277 (0.0030) 110.90 (0.17) 113.72 (0.17) C5 - C3 C14 C6 - Distance Angles C11 1.3898 (0.0031) C7 1.3948 (0.0028) 117.50 (0.21) C5 1.5277 (0.0030) 123.45 (0.19) 119.05 (0.19) C6 - C11 C7 C7 - Distance Angles O2 1.3711 (0.0025) C8 1.3774 (0.0030) 123.80 (0.19) C6 1.3948 (0.0028) 115.21 (0.19) 120.99 (0.20) C7 - O2 C8 C8 - Distance Angles C7 1.3774 (0.0030) C9 1.3848 (0.0032) 120.07 (0.21) C8 - C7 C9 - Distance Angles O3 1.3709 (0.0028) C10 1.3828 (0.0033) 125.93 (0.22) C8 1.3848 (0.0032) 113.89 (0.21) 120.17 (0.22) C9 - O3 C10 C10 - Distance Angles C11 1.3777 (0.0034) C9 1.3828 (0.0033) 118.98 (0.22) C10 - C11 C11 - Distance Angles C10 1.3777 (0.0034) C6 1.3898 (0.0031) 122.25 (0.21) C11 - C10 C12 - Distance Angles O2 1.4064 (0.0026) C12 - C13 - Distance Angles O3 1.4277 (0.0031) C13 - C14 - Distance Angles C19 1.3739 (0.0029) C15 1.3958 (0.0029) 117.58 (0.19) C5 1.5282 (0.0027) 122.73 (0.19) 119.69 (0.17) C14 - C19 C15 C15 - Distance Angles O4 1.3678 (0.0024) C16 1.3837 (0.0027) 123.74 (0.19) C14 1.3958 (0.0029) 115.76 (0.17) 120.50 (0.18) C15 - O4 C16 C16 - Distance Angles C15 1.3837 (0.0027) C17 1.3855 (0.0029) 119.88 (0.20) C16 - C15 C17 - Distance Angles O5 1.3677 (0.0024) C18 1.3676 (0.0033) 124.62 (0.20) C16 1.3855 (0.0029) 114.58 (0.21) 120.79 (0.20) C17 - O5 C18 C18 - Distance Angles C17 1.3676 (0.0033) C19 1.3870 (0.0031) 118.29 (0.21) C18 - C17 C19 - Distance Angles C14 1.3739 (0.0029) C18 1.3870 (0.0031) 122.94 (0.22) C19 - C14 C20 - Distance Angles O4 1.4299 (0.0029) C20 - C21 - Distance Angles O5 1.4185 (0.0028) C21 - FMAP and GRID set by program FMAP 2 2 18 GRID -1.667 -2 -2 1.667 2 2 R1 = 0.1002 for 4938 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.23 at 0.7170 0.0786 0.9186 [ 0.96 A from H13C ] Deepest hole -0.34 at 0.8347 0.1363 0.5393 [ 0.85 A from S2 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2907 / 24198 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7170 0.0786 -0.0814 1.00000 0.05 0.23 0.96 H13C 1.68 C13 1.81 H13A 2.00 H10 Q2 1 0.5577 0.2148 0.4046 1.00000 0.05 0.19 0.39 C14 1.42 C19 1.47 C15 1.58 C5 Q3 1 0.6356 0.1394 -0.0964 1.00000 0.05 0.18 1.72 H10 1.75 H13A 2.02 H13C 2.26 C13 Q4 1 0.6402 0.0716 0.0629 1.00000 0.05 0.18 0.42 C10 0.67 H10 1.40 C9 1.76 C11 Q5 1 0.7595 -0.1058 -0.1516 1.00000 0.05 0.17 1.45 H13B 1.80 H13C 1.91 C13 2.02 H21B Q6 1 0.6718 0.5393 0.4641 1.00000 0.05 0.17 1.77 H18 2.10 H13C 2.15 H21A 2.52 C18 Q7 1 0.6340 0.3047 0.3945 1.00000 0.05 0.17 0.35 C19 0.72 H19 1.51 C18 1.57 C14 Q8 1 0.6277 0.4756 0.4187 1.00000 0.05 0.17 0.71 H18 1.39 C18 2.07 H21A 2.35 C19 Q9 1 0.7821 0.0968 -0.0177 1.00000 0.05 0.16 1.68 H13C 2.03 H16 2.13 H10 2.51 C13 Q10 1 0.6387 0.6124 0.2805 1.00000 0.05 0.16 1.90 H21C 2.19 H12A 2.21 S3 2.40 H18 Shortest distances between peaks (including symmetry equivalents) 1 9 1.13 6 8 1.13 6 9 1.14 1 3 1.30 2 7 1.54 1 6 2.02 3 9 2.09 4 9 2.22 1 4 2.22 3 4 2.25 7 8 2.27 8 9 2.27 4 6 2.50 8 10 2.56 6 10 2.57 1 5 2.67 Time profile in seconds ----------------------- 0.22: 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 0.02: Analyse other restraints etc. 2.38: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.06: Structure factors and derivatives 2.92: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.42: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.06: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 10:21:49 Total CPU time: 8.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++