+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 13:25:52 on 16-Jul-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02SOT082 in Pna2(1) CELL 0.71073 9.3133 15.4441 9.8424 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0004 0.0003 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SFAC C H O UNIT 56 88 24 V = 1415.69 F(000) = 616.0 Mu = 0.10 mm-1 Cell Wt = 1145.26 Rho = 1.343 MERG 2 OMIT -3.00 55.00 EXTI 0.00940 FMAP 2 PLAN 10 SIZE 0.10 0.22 0.26 ACTA BOND $H WGHT 0.04170 0.15480 L.S. 4 TEMP -153.00 FVAR 0.50703 MOLE 1 C1 1 0.373800 -0.066053 0.241552 11.00000 0.01684 0.02060 = 0.01901 0.00069 0.00309 0.00102 C2 1 0.502865 -0.096431 0.319626 11.00000 0.01956 0.02434 = 0.02463 -0.00059 0.00010 0.00285 AFIX 23 H2A 2 0.587908 -0.101054 0.259718 11.00000 -1.20000 H2B 2 0.484698 -0.153433 0.362304 11.00000 -1.20000 AFIX 0 C3 1 0.524504 -0.026699 0.426784 11.00000 0.01847 0.02431 = 0.01944 -0.00082 -0.00142 0.00381 AFIX 23 H3A 2 0.627729 -0.017972 0.446517 11.00000 -1.20000 H3B 2 0.473910 -0.041557 0.512118 11.00000 -1.20000 AFIX 0 C4 1 0.458546 0.054114 0.359843 11.00000 0.01540 0.02200 = 0.01713 -0.00107 -0.00272 -0.00084 C5 1 0.568915 0.105350 0.278731 11.00000 0.02106 0.02743 = 0.02229 -0.00111 0.00216 -0.00218 AFIX 137 H5A 2 0.621968 0.066014 0.218864 11.00000 -1.50000 H5B 2 0.635967 0.133724 0.341230 11.00000 -1.50000 H5C 2 0.519821 0.149276 0.223913 11.00000 -1.50000 AFIX 0 C6 1 0.378279 0.113400 0.457061 11.00000 0.01451 0.01990 = 0.01763 -0.00089 0.00011 -0.00316 AFIX 13 H6 2 0.450352 0.143612 0.515578 11.00000 -1.20000 AFIX 0 C7 1 0.283429 0.182026 0.389829 11.00000 0.01825 0.01878 = 0.02526 0.00316 0.00049 -0.00158 AFIX 23 H7A 2 0.336971 0.236559 0.374709 11.00000 -1.20000 H7B 2 0.244596 0.161227 0.302068 11.00000 -1.20000 AFIX 0 C8 1 0.164419 0.194130 0.494428 11.00000 0.01999 0.01692 = 0.03018 -0.00152 0.00064 0.00034 AFIX 23 H8A 2 0.193906 0.235207 0.566431 11.00000 -1.20000 H8B 2 0.075250 0.215517 0.451163 11.00000 -1.20000 AFIX 0 C9 1 0.143762 0.103142 0.551736 11.00000 0.01509 0.01957 = 0.02181 -0.00051 0.00057 0.00185 C10 1 0.096285 0.101433 0.699661 11.00000 0.01909 0.03567 = 0.02488 -0.00695 0.00246 -0.00169 AFIX 137 H10A 2 0.105653 0.042469 0.735368 11.00000 -1.50000 H10B 2 -0.004132 0.119959 0.706022 11.00000 -1.50000 H10C 2 0.156761 0.140771 0.752851 11.00000 -1.50000 AFIX 0 C11 1 0.039978 0.050489 0.460202 11.00000 0.01553 0.02035 = 0.02161 -0.00013 -0.00087 0.00077 AFIX 13 H11 2 0.084600 0.044768 0.368227 11.00000 -1.20000 AFIX 0 C12 1 0.013245 -0.039934 0.515869 11.00000 0.01773 0.02114 = 0.02358 -0.00219 -0.00132 -0.00105 C13 1 0.103862 -0.180031 0.551490 11.00000 0.02626 0.01861 = 0.04772 0.00635 0.00475 -0.00087 AFIX 23 H13A 2 0.012788 -0.205207 0.517872 11.00000 -1.20000 H13B 2 0.100272 -0.177891 0.651962 11.00000 -1.20000 AFIX 0 C14 1 0.227961 -0.233361 0.505745 11.00000 0.02639 0.02247 = 0.04739 -0.00075 -0.00103 0.00250 AFIX 137 H14A 2 0.232733 -0.232909 0.406281 11.00000 -1.50000 H14B 2 0.215863 -0.292997 0.537783 11.00000 -1.50000 H14C 2 0.316969 -0.209279 0.543063 11.00000 -1.50000 AFIX 0 O1 3 0.299719 -0.107048 0.164416 11.00000 0.02173 0.02499 = 0.03121 -0.00739 -0.00497 -0.00044 O2 3 0.352032 0.018579 0.264256 11.00000 0.01931 0.01959 = 0.01978 -0.00209 -0.00485 -0.00019 O3 3 0.284510 0.063846 0.543794 11.00000 0.01376 0.02088 = 0.02167 0.00340 0.00178 -0.00061 O4 3 -0.093684 0.093588 0.445402 11.00000 0.01685 0.02765 = 0.03010 0.00427 -0.00205 0.00337 AFIX 147 H4 2 -0.146410 0.082103 0.512259 11.00000 -1.50000 AFIX 0 O5 3 -0.096425 -0.060475 0.572314 11.00000 0.02260 0.02366 = 0.05305 0.00231 0.01266 -0.00187 O6 3 0.124090 -0.093360 0.496201 11.00000 0.01874 0.01798 = 0.03342 0.00140 0.00359 -0.00010 HKLF 4 1.0 1.00 0.00 0.00 0.00 0.00 -1.00 0.00 1.00 0.00 Covalent radii and connectivity table for 02SOT082 in Pna2(1) C 0.770 H 0.320 O 0.660 C1 - O1 O2 C2 C2 - C1 C3 C3 - C2 C4 C4 - O2 C6 C5 C3 C5 - C4 C6 - O3 C4 C7 C7 - C8 C6 C8 - C7 C9 C9 - O3 C10 C8 C11 C10 - C9 C11 - O4 C12 C9 C12 - O5 O6 C11 C13 - O6 C14 C14 - C13 O1 - C1 O2 - C1 C4 O3 - C6 C9 O4 - C11 O5 - C12 O6 - C12 C13 Floating origin restraints generated h k l Fo^2 Sigma Why rejected 5 0 0 8.00 2.00 observed but should be systematically absent 15417 Reflections read, of which 682 rejected -10 =< h =< 12, -19 =< k =< 20, -12 =< l =< 12, Max. 2-theta = 54.98 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 2 5 -9 41.85 0.87 7 4.51 0 7 -9 146.57 5.47 3 41.09 1 9 -6 93.98 0.96 5 20.15 1 4 -5 162.29 1.77 7 14.27 5 6 -5 44.76 0.88 7 4.95 5 7 -4 29.53 0.87 5 6.38 0 4 -2 163.20 4.48 3 40.15 7 Inconsistent equivalents 3218 Unique reflections, of which 0 suppressed R(int) = 0.0585 R(sigma) = 0.0433 Friedel opposites not merged Maximum memory for data reduction = 2147 / 32377 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 = 2705 / 229828 wR2 = 0.0810 before cycle 1 for 3218 data and 186 / 186 parameters GooF = S = 1.024; Restrained GooF = 1.023 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0417 * P )^2 + 0.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50744 0.00091 0.453 OSF 2 0.00971 0.00160 0.194 EXTI Mean shift/esd = 0.061 Maximum = 0.453 for OSF Max. shift = 0.006 A for H4 Max. dU = 0.000 for C13 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2705 / 229828 wR2 = 0.0810 before cycle 2 for 3218 data and 186 / 186 parameters GooF = S = 1.024; Restrained GooF = 1.024 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0417 * P )^2 + 0.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50749 0.00091 0.059 OSF 2 0.00981 0.00161 0.063 EXTI Mean shift/esd = 0.020 Maximum = 0.167 for tors H4 Max. shift = 0.003 A for H4 Max. dU = 0.000 for C13 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2705 / 229828 wR2 = 0.0810 before cycle 3 for 3218 data and 186 / 186 parameters GooF = S = 1.024; Restrained GooF = 1.024 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0417 * P )^2 + 0.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50750 0.00091 0.003 OSF 2 0.00981 0.00162 0.000 EXTI Mean shift/esd = 0.002 Maximum = 0.048 for tors H4 Max. shift = 0.001 A for H4 Max. dU = 0.000 for C1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2705 / 229828 wR2 = 0.0810 before cycle 4 for 3218 data and 186 / 186 parameters GooF = S = 1.024; Restrained GooF = 1.024 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0417 * P )^2 + 0.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50750 0.00091 0.000 OSF 2 0.00981 0.00162 0.000 EXTI Mean shift/esd = 0.001 Maximum = 0.014 for tors H4 Max. shift = 0.000 A for H4 Max. dU = 0.000 for C9 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 H2A 0.5879 -0.1011 0.2597 23 0.990 0.000 C2 C1 C3 H2B 0.4847 -0.1534 0.3623 23 0.990 0.000 C2 C1 C3 H3A 0.6277 -0.0180 0.4465 23 0.990 0.000 C3 C2 C4 H3B 0.4739 -0.0416 0.5121 23 0.990 0.000 C3 C2 C4 H5A 0.6219 0.0660 0.2189 137 0.980 0.000 C5 C4 H5A H5B 0.6360 0.1337 0.3412 137 0.980 0.000 C5 C4 H5A H5C 0.5198 0.1493 0.2240 137 0.980 0.000 C5 C4 H5A H6 0.4504 0.1436 0.5156 13 1.000 0.000 C6 O3 C4 C7 H7A 0.3370 0.2366 0.3747 23 0.990 0.000 C7 C8 C6 H7B 0.2446 0.1612 0.3021 23 0.990 0.000 C7 C8 C6 H8A 0.0753 0.2155 0.4512 23 0.990 0.000 C8 C7 C9 H8B 0.1940 0.2352 0.5664 23 0.990 0.000 C8 C7 C9 H10A 0.1054 0.0424 0.7352 137 0.980 0.000 C10 C9 H10A H10B -0.0040 0.1201 0.7060 137 0.980 0.000 C10 C9 H10A H10C 0.1570 0.1406 0.7529 137 0.980 0.000 C10 C9 H10A H11 0.0846 0.0448 0.3682 13 1.000 0.000 C11 O4 C12 C9 H13A 0.0128 -0.2052 0.5179 23 0.990 0.000 C13 O6 C14 H13B 0.1003 -0.1779 0.6520 23 0.990 0.000 C13 O6 C14 H14A 0.2327 -0.2329 0.4063 137 0.980 0.000 C14 C13 H14A H14B 0.2159 -0.2930 0.5378 137 0.980 0.000 C14 C13 H14A H14C 0.3170 -0.2093 0.5431 137 0.980 0.000 C14 C13 H14A H4 -0.1460 0.0826 0.5128 147 0.840 0.000 O4 C11 H4 02SOT082 in Pna2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.37380 -0.06606 0.24155 1.00000 0.01684 0.02061 0.01904 0.00071 0.00310 0.00097 0.01883 0.00265 0.00015 0.00009 0.00016 0.00000 0.00073 0.00071 0.00076 0.00064 0.00058 0.00054 0.00031 C2 0.50287 -0.09643 0.31964 1.00000 0.01964 0.02435 0.02462 -0.00060 0.00005 0.00289 0.02287 0.00279 0.00017 0.00010 0.00017 0.00000 0.00079 0.00073 0.00080 0.00063 0.00062 0.00059 0.00034 H2A 0.58792 -0.10106 0.25973 1.00000 0.02745 0.00000 0.00000 H2B 0.48471 -0.15343 0.36233 1.00000 0.02745 0.00000 0.00000 C3 0.52451 -0.02669 0.42679 1.00000 0.01855 0.02439 0.01949 -0.00084 -0.00139 0.00378 0.02081 0.00262 0.00016 0.00009 0.00016 0.00000 0.00073 0.00072 0.00078 0.00064 0.00063 0.00057 0.00032 H3A 0.62774 -0.01797 0.44652 1.00000 0.02497 0.00000 0.00000 H3B 0.47392 -0.04155 0.51213 1.00000 0.02497 0.00000 0.00000 C4 0.45854 0.05412 0.35985 1.00000 0.01541 0.02210 0.01717 -0.00106 -0.00271 -0.00087 0.01822 0.00243 0.00016 0.00009 0.00015 0.00000 0.00068 0.00071 0.00074 0.00060 0.00057 0.00055 0.00031 C5 0.56890 0.10534 0.27875 1.00000 0.02117 0.02738 0.02237 -0.00117 0.00219 -0.00217 0.02364 0.00278 0.00017 0.00010 0.00017 0.00000 0.00080 0.00078 0.00080 0.00066 0.00063 0.00062 0.00034 H5A 0.62191 0.06600 0.21886 1.00000 0.03546 0.00000 0.00000 H5B 0.63598 0.13369 0.34125 1.00000 0.03546 0.00000 0.00000 H5C 0.51981 0.14928 0.22396 1.00000 0.03546 0.00000 0.00000 C6 0.37830 0.11338 0.45706 1.00000 0.01454 0.01993 0.01760 -0.00088 0.00011 -0.00318 0.01736 0.00248 0.00015 0.00009 0.00016 0.00000 0.00066 0.00065 0.00073 0.00059 0.00056 0.00051 0.00030 H6 0.45037 0.14360 0.51558 1.00000 0.02083 0.00000 0.00000 C7 0.28343 0.18203 0.38981 1.00000 0.01831 0.01880 0.02539 0.00312 0.00051 -0.00157 0.02083 0.00264 0.00015 0.00010 0.00016 0.00000 0.00073 0.00067 0.00074 0.00059 0.00061 0.00055 0.00031 H7A 0.33697 0.23656 0.37467 1.00000 0.02500 0.00000 0.00000 H7B 0.24457 0.16122 0.30206 1.00000 0.02500 0.00000 0.00000 C8 0.16444 0.19414 0.49444 1.00000 0.02010 0.01692 0.03017 -0.00154 0.00055 0.00033 0.02240 0.00269 0.00017 0.00009 0.00017 0.00000 0.00075 0.00064 0.00080 0.00065 0.00065 0.00056 0.00032 H8A 0.07527 0.21554 0.45120 1.00000 0.02688 0.00000 0.00000 H8B 0.19396 0.23520 0.56644 1.00000 0.02688 0.00000 0.00000 C9 0.14376 0.10315 0.55174 1.00000 0.01514 0.01956 0.02178 -0.00061 0.00062 0.00193 0.01883 0.00252 0.00016 0.00009 0.00016 0.00000 0.00070 0.00065 0.00077 0.00063 0.00059 0.00053 0.00031 C10 0.09630 0.10143 0.69963 1.00000 0.01914 0.03554 0.02499 -0.00684 0.00242 -0.00171 0.02656 0.00282 0.00018 0.00011 0.00017 0.00000 0.00079 0.00087 0.00089 0.00070 0.00065 0.00065 0.00037 H10A 0.10539 0.04242 0.73524 1.00000 0.03984 0.00000 0.00000 H10B -0.00403 0.12012 0.70603 1.00000 0.03984 0.00000 0.00000 H10C 0.15697 0.14062 0.75288 1.00000 0.03984 0.00000 0.00000 C11 0.03997 0.05050 0.46021 1.00000 0.01545 0.02038 0.02164 -0.00012 -0.00090 0.00082 0.01915 0.00251 0.00016 0.00009 0.00015 0.00000 0.00072 0.00067 0.00079 0.00060 0.00059 0.00056 0.00032 H11 0.08459 0.04478 0.36824 1.00000 0.02298 0.00000 0.00000 C12 0.01326 -0.03991 0.51586 1.00000 0.01772 0.02125 0.02362 -0.00223 -0.00133 -0.00099 0.02086 0.00261 0.00016 0.00010 0.00016 0.00000 0.00074 0.00066 0.00079 0.00060 0.00063 0.00055 0.00032 C13 0.10388 -0.18003 0.55150 1.00000 0.02640 0.01854 0.04790 0.00642 0.00465 -0.00087 0.03094 0.00318 0.00018 0.00009 0.00021 0.00000 0.00085 0.00071 0.00106 0.00079 0.00078 0.00060 0.00039 H13A 0.01280 -0.20520 0.51790 1.00000 0.03713 0.00000 0.00000 H13B 0.10031 -0.17788 0.65197 1.00000 0.03713 0.00000 0.00000 C14 0.22797 -0.23337 0.50574 1.00000 0.02638 0.02241 0.04763 -0.00074 -0.00089 0.00249 0.03214 0.00300 0.00018 0.00010 0.00019 0.00000 0.00084 0.00073 0.00110 0.00077 0.00082 0.00063 0.00040 H14A 0.23274 -0.23291 0.40628 1.00000 0.04821 0.00000 0.00000 H14B 0.21585 -0.29301 0.53777 1.00000 0.04821 0.00000 0.00000 H14C 0.31698 -0.20930 0.54307 1.00000 0.04821 0.00000 0.00000 O1 0.29969 -0.10705 0.16442 1.00000 0.02178 0.02501 0.03121 -0.00743 -0.00495 -0.00041 0.02600 0.00179 0.00011 0.00007 0.00012 0.00000 0.00058 0.00054 0.00062 0.00049 0.00052 0.00044 0.00026 O2 0.35204 0.01858 0.26424 1.00000 0.01933 0.01950 0.01985 -0.00206 -0.00482 -0.00016 0.01956 0.00174 0.00011 0.00006 0.00011 0.00000 0.00054 0.00050 0.00051 0.00043 0.00043 0.00040 0.00023 O3 0.28451 0.06383 0.54379 1.00000 0.01385 0.02078 0.02164 0.00339 0.00176 -0.00056 0.01876 0.00173 0.00010 0.00006 0.00011 0.00000 0.00050 0.00049 0.00053 0.00044 0.00041 0.00038 0.00023 O4 -0.09369 0.09359 0.44542 1.00000 0.01695 0.02764 0.03011 0.00421 -0.00193 0.00343 0.02490 0.00201 0.00011 0.00007 0.00013 0.00000 0.00054 0.00053 0.00062 0.00050 0.00049 0.00043 0.00025 H4 -0.14601 0.08263 0.51278 1.00000 0.03735 0.00000 0.00000 O5 -0.09641 -0.06047 0.57232 1.00000 0.02265 0.02362 0.05307 0.00226 0.01270 -0.00185 0.03311 0.00223 0.00013 0.00007 0.00014 0.00000 0.00061 0.00053 0.00082 0.00056 0.00058 0.00046 0.00030 O6 0.12410 -0.09335 0.49619 1.00000 0.01878 0.01790 0.03349 0.00143 0.00364 -0.00003 0.02339 0.00186 0.00011 0.00006 0.00012 0.00000 0.00053 0.00049 0.00064 0.00047 0.00047 0.00038 0.00025 Final Structure Factor Calculation for 02SOT082 in Pna2(1) Total number of l.s. parameters = 186 Maximum vector length = 511 Memory required = 2521 / 24024 wR2 = 0.0810 before cycle 5 for 3218 data and 2 / 186 parameters GooF = S = 1.024; Restrained GooF = 1.024 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0417 * P )^2 + 0.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0340 for 2831 Fo > 4sig(Fo) and 0.0435 for all 3218 data wR2 = 0.0810, GooF = S = 1.024, Restrained GooF = 1.024 for all data Flack x parameter = 0.6735 with esd 0.6999 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 20.00 for non-hydrogen and 22.00 for hydrogen atoms Principal mean square atomic displacements U 0.0221 0.0198 0.0146 C1 0.0259 0.0244 0.0183 C2 0.0265 0.0195 0.0164 C3 0.0223 0.0191 0.0132 C4 0.0286 0.0230 0.0194 C5 0.0216 0.0174 0.0131 C6 0.0266 0.0196 0.0162 C7 0.0304 0.0201 0.0167 C8 0.0219 0.0202 0.0143 C9 0.0392 0.0222 0.0182 C10 0.0218 0.0205 0.0152 C11 0.0250 0.0207 0.0169 C12 0.0501 0.0260 0.0168 C13 0.0477 0.0275 0.0212 C14 0.0372 0.0234 0.0174 O1 0.0248 0.0196 0.0143 O2 0.0247 0.0183 0.0132 O3 0.0333 0.0261 0.0153 O4 0.0577 0.0245 0.0171 O5 0.0345 0.0182 0.0175 O6 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.025 0.036 0.047 0.058 0.070 0.084 0.104 0.132 0.188 1.000 Number in group 348. 312. 316. 323. 310. 324. 329. 313. 321. 322. GooF 0.930 1.085 1.006 1.085 1.019 1.048 1.100 0.975 0.980 1.003 K 1.066 0.977 0.991 1.023 1.000 1.005 1.000 1.001 1.011 1.011 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 326. 318. 334. 312. 323. 319. 324. 316. 322. 324. GooF 0.970 0.995 0.951 0.980 1.053 0.967 1.019 1.036 1.094 1.157 K 1.046 1.072 1.037 1.024 0.980 0.996 1.005 1.013 1.024 1.003 R1 0.125 0.108 0.080 0.059 0.054 0.033 0.027 0.026 0.024 0.022 Recommended weighting scheme: WGHT 0.0401 0.1666 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) 0 7 3 64.58 46.01 4.52 0.053 1.83 2 0 0 1213.74 1490.08 3.97 0.301 4.66 0 2 2 322.72 394.51 3.86 0.155 4.15 7 6 1 99.51 125.84 3.59 0.088 1.17 3 1 0 71.43 89.80 3.42 0.074 3.04 7 16 1 2.99 24.34 3.32 0.039 0.78 4 10 7 28.68 42.69 3.29 0.051 0.95 1 1 -12 70.68 39.51 3.28 0.049 0.82 1 15 4 69.56 90.09 3.27 0.074 0.94 6 6 0 673.43 577.54 3.19 0.188 1.33 4 5 -8 35.75 48.74 3.14 0.054 1.03 6 2 -2 105.65 85.56 3.10 0.072 1.45 0 16 4 88.90 114.66 3.04 0.084 0.90 3 7 -2 107.28 88.99 3.00 0.074 1.69 0 16 -4 76.39 114.46 2.98 0.084 0.90 5 6 0 446.21 382.49 2.95 0.153 1.51 5 10 -3 125.30 150.13 2.94 0.096 1.12 0 10 0 1378.10 1176.82 2.93 0.268 1.54 2 0 7 329.43 278.63 2.93 0.130 1.35 0 2 -2 329.28 394.33 2.91 0.155 4.15 5 6 -10 249.94 193.42 2.89 0.109 0.82 6 8 -5 50.07 63.14 2.89 0.062 1.03 7 14 3 5.73 23.78 2.87 0.038 0.82 9 2 4 29.72 47.92 2.87 0.054 0.95 5 1 9 10.17 19.60 2.87 0.035 0.94 2 7 -11 86.52 53.66 2.84 0.057 0.82 2 9 6 51.07 63.88 2.83 0.062 1.15 7 11 5 120.86 90.50 2.82 0.074 0.87 2 5 -5 64.90 78.66 2.77 0.069 1.56 6 11 3 19.27 28.27 2.76 0.041 0.99 5 3 -3 447.00 389.86 2.73 0.154 1.55 3 13 -3 71.50 86.78 2.72 0.073 1.05 7 16 -2 -1.27 13.16 2.71 0.028 0.77 7 7 -3 42.22 56.52 2.71 0.059 1.08 0 15 -3 611.43 498.75 2.69 0.174 0.98 6 2 -6 5.60 1.01 2.68 0.008 1.12 8 8 -4 4.73 13.64 2.67 0.029 0.92 11 5 -1 160.27 125.04 2.66 0.087 0.81 5 10 5 209.95 243.97 2.62 0.122 1.02 1 14 3 122.38 142.98 2.58 0.093 1.04 1 6 -2 18.01 24.68 2.56 0.039 2.22 3 14 5 125.74 104.11 2.56 0.080 0.92 5 9 0 3.07 10.62 2.56 0.025 1.26 4 8 0 28.39 20.99 2.54 0.036 1.49 4 5 5 69.81 85.17 2.52 0.072 1.35 2 3 0 142.06 163.43 2.49 0.100 3.45 3 12 -2 625.08 552.21 2.49 0.183 1.16 7 11 -7 -7.84 12.84 2.48 0.028 0.80 2 5 -4 8.79 14.89 2.48 0.030 1.78 1 2 10 -0.90 5.02 2.47 0.017 0.97 Bond lengths and angles C1 - Distance Angles O1 1.2056 (0.0019) O2 1.3416 (0.0017) 122.00 (0.14) C2 1.5019 (0.0022) 128.06 (0.14) 109.88 (0.13) C1 - O1 O2 C2 - Distance Angles C1 1.5019 (0.0022) C3 1.5208 (0.0021) 103.87 (0.12) H2A 0.9900 110.98 110.98 H2B 0.9900 110.98 110.98 108.98 C2 - C1 C3 H2A C3 - Distance Angles C2 1.5208 (0.0021) C4 1.5393 (0.0020) 102.98 (0.12) H3A 0.9900 111.17 111.17 H3B 0.9900 111.17 111.17 109.11 C3 - C2 C4 H3A C4 - Distance Angles O2 1.4733 (0.0017) C6 1.5204 (0.0020) 107.18 (0.11) C5 1.5228 (0.0021) 108.24 (0.12) 110.42 (0.12) C3 1.5393 (0.0020) 103.89 (0.11) 114.52 (0.12) 112.09 (0.12) C4 - O2 C6 C5 C5 - Distance Angles C4 1.5228 (0.0021) H5A 0.9800 109.47 H5B 0.9800 109.47 109.47 H5C 0.9800 109.47 109.47 109.47 C5 - C4 H5A H5B C6 - Distance Angles O3 1.4412 (0.0017) C4 1.5204 (0.0020) 110.55 (0.11) C7 1.5306 (0.0020) 105.91 (0.11) 115.37 (0.13) H6 1.0000 108.26 108.26 108.26 C6 - O3 C4 C7 C7 - Distance Angles C8 1.5243 (0.0022) C6 1.5306 (0.0020) 102.26 (0.12) H7A 0.9900 111.32 111.32 H7B 0.9900 111.32 111.32 109.20 C7 - C8 C6 H7A C8 - Distance Angles C7 1.5243 (0.0022) C9 1.5264 (0.0020) 103.20 (0.12) H8A 0.9900 111.12 111.12 H8B 0.9900 111.12 111.12 109.07 C8 - C7 C9 H8A C9 - Distance Angles O3 1.4468 (0.0017) C10 1.5215 (0.0023) 107.92 (0.12) C8 1.5264 (0.0020) 104.60 (0.11) 113.97 (0.13) C11 1.5515 (0.0020) 108.25 (0.11) 111.43 (0.12) 110.28 (0.13) C9 - O3 C10 C8 C10 - Distance Angles C9 1.5215 (0.0023) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - C9 H10A H10B C11 - Distance Angles O4 1.4190 (0.0017) C12 1.5204 (0.0020) 108.91 (0.12) C9 1.5515 (0.0020) 111.12 (0.11) 111.97 (0.12) H11 1.0000 108.24 108.24 108.24 C11 - O4 C12 C9 C12 - Distance Angles O5 1.2053 (0.0019) O6 1.3358 (0.0018) 123.98 (0.14) C11 1.5204 (0.0020) 123.14 (0.13) 112.88 (0.12) C12 - O5 O6 C13 - Distance Angles O6 1.4573 (0.0017) C14 1.4890 (0.0022) 107.15 (0.13) H13A 0.9900 110.29 110.29 H13B 0.9900 110.29 110.29 108.54 C13 - O6 C14 H13A C14 - Distance Angles C13 1.4890 (0.0022) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - C13 H14A H14B O1 - Distance Angles C1 1.2056 (0.0019) O1 - O2 - Distance Angles C1 1.3416 (0.0017) C4 1.4733 (0.0017) 111.57 (0.11) O2 - C1 O3 - Distance Angles C6 1.4412 (0.0017) C9 1.4468 (0.0017) 110.99 (0.10) O3 - C6 O4 - Distance Angles C11 1.4190 (0.0017) H4 0.8400 109.47 O4 - C11 O5 - Distance Angles C12 1.2053 (0.0019) O5 - O6 - Distance Angles C12 1.3358 (0.0018) C13 1.4573 (0.0017) 114.43 (0.12) O6 - C12 FMAP and GRID set by program FMAP 2 2 20 GRID -1.471 -2 -2 1.471 2 2 R1 = 0.0365 for 1717 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.17 at 0.5089 0.0883 0.3386 [ 0.74 A from C4 ] Deepest hole -0.17 at 0.3371 0.1427 0.5002 [ 0.73 A from C6 ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 2494 / 18353 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5089 0.0883 0.3386 1.00000 0.05 0.17 0.74 C4 0.85 C5 1.38 H5B 1.47 H5C Q2 1 0.1557 0.1430 0.5188 1.00000 0.05 0.15 0.70 C9 0.83 C8 1.50 H8A 1.54 H8B Q3 1 0.1132 0.0990 0.6168 1.00000 0.05 0.14 0.70 C9 0.83 C10 1.44 H10B 1.46 H10A Q4 1 0.0962 0.0817 0.5024 1.00000 0.05 0.14 0.74 C9 0.82 C11 1.44 H11 1.82 O3 Q5 1 -0.0770 0.0983 0.5611 1.00000 0.05 0.14 0.84 H4 1.15 O4 1.62 H10B 1.65 C11 Q6 1 0.2076 -0.0787 0.5018 1.00000 0.05 0.14 0.81 O6 1.90 C13 1.91 C12 2.30 H14C Q7 1 0.0210 0.0058 0.4792 1.00000 0.05 0.13 0.74 C11 0.80 C12 1.38 H11 1.76 O5 Q8 1 0.2827 0.0841 0.1926 1.00000 0.05 0.13 1.39 O2 1.65 H7B 2.13 O5 2.37 C4 Q9 1 -0.2165 0.0278 0.5238 1.00000 0.05 0.13 1.08 H4 1.71 O4 1.78 H3A 1.83 O5 Q10 1 0.1668 -0.0962 0.3992 1.00000 0.05 0.13 1.04 O6 2.03 C12 2.07 C13 2.20 H14A Shortest distances between peaks (including symmetry equivalents) 2 4 1.11 6 10 1.11 3 4 1.17 2 3 1.24 4 7 1.38 4 5 1.73 5 9 1.73 3 5 1.85 5 7 1.88 3 7 2.15 6 7 2.18 7 10 2.22 7 9 2.28 2 5 2.31 8 9 2.47 2 7 2.49 1 8 2.55 4 6 2.69 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.39: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.53: Structure factors and derivatives 0.66: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.00: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.16: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 13:25:55 Total elapsed time: 3.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++