+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 10:54:42 on 19-Nov-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02esp402 in P2(1)/c CELL 0.71073 6.1644 10.8967 24.7631 90.000 93.383 90.000 ZERR 4.00 0.0001 0.0003 0.0007 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O S UNIT 80 76 4 8 4 V = 1660.48 F(000) = 712.0 Mu = 0.21 mm-1 Cell Wt = 1349.69 Rho = 1.350 MERG 2 ACTA SHEL 7 0.84 FMAP 2 MOVE 1 1 1 -1 PLAN 20 SIZE 0.10 0.20 0.30 BOND L.S. 4 TEMP -153.00 WGHT 0.037200 0.576000 FVAR 0.33894 MOLE 1 C1 1 0.271138 0.106287 0.335890 11.00000 0.01996 0.02496 = 0.02155 0.00028 0.00172 0.00324 AFIX 43 H1 2 0.407927 0.074706 0.326802 11.00000 -1.20000 AFIX 0 C2 1 0.202304 0.092007 0.388044 11.00000 0.03250 0.02921 = 0.01750 0.00362 -0.00323 0.00037 AFIX 43 H2 2 0.290819 0.049164 0.414494 11.00000 -1.20000 AFIX 0 C3 1 0.004738 0.140296 0.401329 11.00000 0.03367 0.02496 = 0.01555 -0.00374 0.00547 -0.00726 AFIX 43 H3 2 -0.040292 0.132766 0.437213 11.00000 -1.20000 AFIX 0 C4 1 -0.127352 0.199555 0.362402 11.00000 0.02372 0.02292 = 0.02564 -0.00411 0.00830 -0.00072 AFIX 43 H4 2 -0.263747 0.231671 0.371498 11.00000 -1.20000 AFIX 0 C5 1 -0.060791 0.212136 0.310060 11.00000 0.02197 0.01871 = 0.02129 0.00022 0.00037 0.00199 AFIX 43 H5 2 -0.152249 0.251705 0.283181 11.00000 -1.20000 AFIX 0 C6 1 0.139093 0.166799 0.297314 11.00000 0.02090 0.01359 = 0.01404 -0.00226 0.00223 -0.00387 C7 1 0.201756 0.098408 0.204337 11.00000 0.01128 0.01872 = 0.01711 -0.00065 -0.00037 0.00181 C8 1 0.280629 0.158408 0.152003 11.00000 0.01503 0.01659 = 0.01539 -0.00223 -0.00066 -0.00175 C9 1 0.335109 0.064131 0.110381 11.00000 0.02158 0.01511 = 0.01274 0.00131 0.00289 0.00025 C10 1 0.543135 0.015355 0.108808 11.00000 0.02132 0.01921 = 0.01894 0.00276 0.00271 -0.00078 AFIX 43 H10 2 0.657743 0.047894 0.131837 11.00000 -1.20000 AFIX 0 C11 1 0.585150 -0.080645 0.073841 11.00000 0.02631 0.02102 = 0.02464 0.00203 0.00943 0.00500 AFIX 43 H11 2 0.727492 -0.113918 0.073441 11.00000 -1.20000 AFIX 0 C12 1 0.419872 -0.127708 0.039652 11.00000 0.03872 0.01727 = 0.01728 -0.00077 0.01038 -0.00009 AFIX 43 H12 2 0.448584 -0.192985 0.015665 11.00000 -1.20000 AFIX 0 C13 1 0.212721 -0.079265 0.040570 11.00000 0.03108 0.02098 = 0.01477 -0.00139 -0.00009 -0.00130 AFIX 43 H13 2 0.099303 -0.111115 0.016972 11.00000 -1.20000 AFIX 0 C14 1 0.169601 0.015609 0.075767 11.00000 0.02104 0.02000 = 0.01882 -0.00047 0.00063 0.00157 AFIX 43 H14 2 0.026519 0.047785 0.076325 11.00000 -1.20000 AFIX 0 C15 1 0.093568 0.252723 0.136548 11.00000 0.01686 0.01842 = 0.01714 -0.00194 0.00059 0.00011 AFIX 13 H15 2 -0.048216 0.209555 0.139808 11.00000 -1.20000 AFIX 0 C16 1 0.093660 0.307007 0.079622 11.00000 0.03479 0.01672 = 0.01781 -0.00500 -0.00186 0.00825 C17 1 0.296423 0.365322 0.060549 11.00000 0.04388 0.03494 = 0.01984 0.00745 0.00733 0.00471 AFIX 137 H17A 2 0.269208 0.394504 0.023331 11.00000 -1.50000 H17B 2 0.414127 0.304751 0.061789 11.00000 -1.50000 H17C 2 0.338148 0.434736 0.084090 11.00000 -1.50000 AFIX 0 C18 1 0.114462 0.352106 0.181817 11.00000 0.02098 0.01740 = 0.01804 -0.00164 0.00152 0.00143 AFIX 23 H18A 2 0.158210 0.431883 0.166720 11.00000 -1.20000 H18B 2 -0.025621 0.362846 0.198843 11.00000 -1.20000 AFIX 0 C19 1 0.289729 0.304740 0.223344 11.00000 0.01716 0.01728 = 0.01737 -0.00116 0.00157 -0.00108 C20 1 0.361173 0.393777 0.267413 11.00000 0.02333 0.02115 = 0.01900 -0.00449 0.00167 -0.00366 AFIX 137 H20A 2 0.236709 0.415269 0.288391 11.00000 -1.50000 H20B 2 0.418762 0.468136 0.251208 11.00000 -1.50000 H20C 2 0.474524 0.355848 0.291309 11.00000 -1.50000 AFIX 0 N1 3 0.214311 0.185091 0.243848 11.00000 0.02037 0.01478 = 0.01452 -0.00087 0.00204 -0.00154 O1 4 0.132278 -0.005435 0.207894 11.00000 0.02565 0.01688 = 0.02242 -0.00145 0.00536 -0.00333 O2 4 -0.073950 0.305189 0.051080 11.00000 0.04493 0.03242 = 0.02641 -0.00141 -0.01648 0.00319 S1 5 0.506000 0.254901 0.179826 11.00000 0.01577 0.02284 = 0.01805 -0.00416 0.00194 -0.00323 HKLF 4 Covalent radii and connectivity table for 02esp402 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C1 - C6 C2 C2 - C3 C1 C3 - C2 C4 C4 - C3 C5 C5 - C6 C4 C6 - C5 C1 N1 C7 - O1 N1 C8 C8 - C9 C7 C15 S1 C9 - C10 C14 C8 C10 - C9 C11 C11 - C12 C10 C12 - C13 C11 C13 - C12 C14 C14 - C13 C9 C15 - C16 C18 C8 C16 - O2 C17 C15 C17 - C16 C18 - C19 C15 C19 - N1 C20 C18 S1 C20 - C19 N1 - C7 C6 C19 O1 - C7 O2 - C16 S1 - C8 C19 6818 Reflections read, of which 1509 rejected -7 =< h =< 7, -12 =< k =< 12, -29 =< l =< 29, Max. 2-theta = 50.05 0 Systematic absence violations 0 Inconsistent equivalents 2901 Unique reflections, of which 0 suppressed R(int) = 0.0243 R(sigma) = 0.0422 Friedel opposites merged Maximum memory for data reduction = 2102 / 28901 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 = 2723 / 272363 wR2 = 0.0867 before cycle 1 for 2901 data and 219 / 219 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0372 * P )^2 + 0.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33894 0.00057 0.006 OSF Mean shift/esd = 0.002 Maximum = -0.022 for z S1 Max. shift = 0.000 A for S1 Max. dU = 0.000 for C2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2723 / 272363 wR2 = 0.0867 before cycle 2 for 2901 data and 219 / 219 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0372 * P )^2 + 0.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33894 0.00057 -0.002 OSF Mean shift/esd = 0.001 Maximum = -0.007 for z S1 Max. shift = 0.000 A for H17A Max. dU = 0.000 for C2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2723 / 272363 wR2 = 0.0867 before cycle 3 for 2901 data and 219 / 219 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0372 * P )^2 + 0.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33894 0.00057 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for H17B Max. dU = 0.000 for C20 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2723 / 272363 wR2 = 0.0867 before cycle 4 for 2901 data and 219 / 219 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0372 * P )^2 + 0.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33894 0.00057 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C8 Max. shift = 0.000 A for H20B Max. dU = 0.000 for C8 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 H1 0.5921 0.9253 0.6732 43 0.950 0.000 C1 C6 C2 H2 0.7092 0.9508 0.5855 43 0.950 0.000 C2 C3 C1 H3 1.0403 0.8672 0.5628 43 0.950 0.000 C3 C2 C4 H4 1.2637 0.7683 0.6285 43 0.950 0.000 C4 C3 C5 H5 1.1522 0.7483 0.7168 43 0.950 0.000 C5 C6 C4 H10 0.3423 0.9521 0.8682 43 0.950 0.000 C10 C9 C11 H11 0.2725 1.1139 0.9266 43 0.950 0.000 C11 C12 C10 H12 0.5514 1.1930 0.9843 43 0.950 0.000 C12 C13 C11 H13 0.9007 1.1111 0.9830 43 0.950 0.000 C13 C12 C14 H14 0.9735 0.9522 0.9237 43 0.950 0.000 C14 C13 C9 H15 1.0482 0.7904 0.8602 13 1.000 0.000 C15 C16 C18 C8 H17A 0.7308 0.6055 0.9767 137 0.980 0.000 C17 C16 H17A H17B 0.6619 0.5653 0.9159 137 0.980 0.000 C17 C16 H17A H17C 0.5859 0.6952 0.9382 137 0.980 0.000 C17 C16 H17A H18A 1.0256 0.6372 0.8012 23 0.990 0.000 C18 C19 C15 H18B 0.8418 0.5681 0.8333 23 0.990 0.000 C18 C19 C15 H20A 0.7633 0.5847 0.7116 137 0.980 0.000 C20 C19 H20A H20B 0.5255 0.6442 0.7087 137 0.980 0.000 C20 C19 H20A H20C 0.5812 0.5319 0.7488 137 0.980 0.000 C20 C19 H20A 02esp402 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.72886 0.89371 0.66411 1.00000 0.01996 0.02496 0.02155 0.00028 0.00172 0.00324 0.02214 0.00313 0.00030 0.00017 0.00007 0.00000 0.00099 0.00109 0.00092 0.00080 0.00076 0.00084 0.00043 H1 0.59207 0.92529 0.67320 1.00000 0.02656 0.00000 0.00000 C2 0.79770 0.90799 0.61196 1.00000 0.03250 0.02921 0.01750 0.00362 -0.00323 0.00037 0.02659 0.00327 0.00032 0.00018 0.00007 0.00000 0.00116 0.00115 0.00090 0.00084 0.00080 0.00094 0.00046 H2 0.70918 0.95084 0.58551 1.00000 0.03191 0.00000 0.00000 C3 0.99526 0.85970 0.59867 1.00000 0.03367 0.02496 0.01555 -0.00374 0.00547 -0.00726 0.02457 0.00310 0.00031 0.00017 0.00007 0.00000 0.00115 0.00110 0.00088 0.00079 0.00080 0.00092 0.00045 H3 1.04029 0.86723 0.56279 1.00000 0.02949 0.00000 0.00000 C4 1.12735 0.80045 0.63760 1.00000 0.02372 0.02292 0.02564 -0.00411 0.00829 -0.00072 0.02382 0.00319 0.00030 0.00017 0.00007 0.00000 0.00102 0.00107 0.00097 0.00082 0.00080 0.00087 0.00043 H4 1.26375 0.76833 0.62850 1.00000 0.02859 0.00000 0.00000 C5 1.06079 0.78786 0.68994 1.00000 0.02197 0.01871 0.02129 0.00022 0.00037 0.00199 0.02069 0.00314 0.00029 0.00017 0.00007 0.00000 0.00100 0.00099 0.00091 0.00075 0.00075 0.00081 0.00041 H5 1.15225 0.74830 0.71682 1.00000 0.02483 0.00000 0.00000 C6 0.86091 0.83320 0.70269 1.00000 0.02090 0.01359 0.01405 -0.00226 0.00223 -0.00387 0.01613 0.00286 0.00028 0.00016 0.00006 0.00000 0.00096 0.00091 0.00080 0.00069 0.00069 0.00077 0.00038 C7 0.79824 0.90159 0.79566 1.00000 0.01128 0.01872 0.01711 -0.00065 -0.00037 0.00181 0.01575 0.00296 0.00026 0.00017 0.00006 0.00000 0.00088 0.00103 0.00085 0.00075 0.00068 0.00077 0.00039 C8 0.71937 0.84159 0.84800 1.00000 0.01503 0.01659 0.01539 -0.00223 -0.00066 -0.00175 0.01573 0.00281 0.00027 0.00016 0.00006 0.00000 0.00090 0.00095 0.00083 0.00072 0.00067 0.00074 0.00038 C9 0.66489 0.93587 0.88962 1.00000 0.02158 0.01511 0.01274 0.00131 0.00289 0.00025 0.01640 0.00295 0.00028 0.00016 0.00006 0.00000 0.00097 0.00094 0.00080 0.00070 0.00069 0.00080 0.00039 C10 0.45686 0.98465 0.89119 1.00000 0.02132 0.01921 0.01894 0.00276 0.00271 -0.00078 0.01976 0.00321 0.00029 0.00016 0.00007 0.00000 0.00099 0.00100 0.00086 0.00076 0.00074 0.00081 0.00041 H10 0.34226 0.95211 0.86816 1.00000 0.02372 0.00000 0.00000 C11 0.41485 1.08064 0.92616 1.00000 0.02631 0.02102 0.02464 0.00203 0.00943 0.00500 0.02368 0.00335 0.00031 0.00017 0.00007 0.00000 0.00106 0.00104 0.00095 0.00081 0.00081 0.00087 0.00043 H11 0.27251 1.11392 0.92656 1.00000 0.02841 0.00000 0.00000 C12 0.58013 1.12771 0.96035 1.00000 0.03872 0.01727 0.01728 -0.00077 0.01038 -0.00009 0.02408 0.00333 0.00032 0.00017 0.00007 0.00000 0.00121 0.00100 0.00089 0.00075 0.00082 0.00090 0.00044 H12 0.55142 1.19298 0.98433 1.00000 0.02889 0.00000 0.00000 C13 0.78728 1.07926 0.95943 1.00000 0.03108 0.02098 0.01477 -0.00139 -0.00009 -0.00130 0.02233 0.00323 0.00031 0.00017 0.00007 0.00000 0.00112 0.00102 0.00085 0.00076 0.00075 0.00086 0.00043 H13 0.90070 1.11111 0.98303 1.00000 0.02680 0.00000 0.00000 C14 0.83040 0.98439 0.92423 1.00000 0.02104 0.02000 0.01882 -0.00047 0.00063 0.00157 0.01998 0.00304 0.00030 0.00016 0.00007 0.00000 0.00098 0.00103 0.00087 0.00076 0.00074 0.00081 0.00041 H14 0.97348 0.95221 0.92368 1.00000 0.02397 0.00000 0.00000 C15 0.90643 0.74728 0.86345 1.00000 0.01686 0.01842 0.01714 -0.00194 0.00059 0.00011 0.01749 0.00298 0.00028 0.00016 0.00006 0.00000 0.00092 0.00097 0.00085 0.00075 0.00071 0.00078 0.00039 H15 1.04822 0.79044 0.86019 1.00000 0.02098 0.00000 0.00000 C16 0.90634 0.69299 0.92038 1.00000 0.03479 0.01672 0.01781 -0.00500 -0.00186 0.00825 0.02324 0.00320 0.00031 0.00016 0.00007 0.00000 0.00116 0.00101 0.00090 0.00077 0.00084 0.00090 0.00043 C17 0.70358 0.63468 0.93945 1.00000 0.04388 0.03494 0.01984 0.00745 0.00733 0.00471 0.03267 0.00376 0.00034 0.00020 0.00007 0.00000 0.00131 0.00125 0.00095 0.00088 0.00087 0.00103 0.00051 H17A 0.73079 0.60550 0.97667 1.00000 0.04901 0.00000 0.00000 H17B 0.66185 0.56526 0.91591 1.00000 0.04901 0.00000 0.00000 H17C 0.58587 0.69525 0.93821 1.00000 0.04901 0.00000 0.00000 C18 0.88554 0.64789 0.81818 1.00000 0.02098 0.01740 0.01804 -0.00164 0.00152 0.00143 0.01879 0.00293 0.00028 0.00016 0.00007 0.00000 0.00099 0.00101 0.00086 0.00074 0.00073 0.00078 0.00041 H18A 1.02562 0.63715 0.80116 1.00000 0.02255 0.00000 0.00000 H18B 0.84179 0.56812 0.83328 1.00000 0.02255 0.00000 0.00000 C19 0.71027 0.69526 0.77666 1.00000 0.01716 0.01728 0.01737 -0.00116 0.00157 -0.00108 0.01725 0.00297 0.00027 0.00016 0.00006 0.00000 0.00091 0.00097 0.00085 0.00072 0.00071 0.00078 0.00039 C20 0.63883 0.60622 0.73259 1.00000 0.02333 0.02115 0.01900 -0.00449 0.00167 -0.00366 0.02115 0.00295 0.00029 0.00017 0.00007 0.00000 0.00101 0.00104 0.00089 0.00077 0.00075 0.00083 0.00042 H20A 0.76329 0.58473 0.71161 1.00000 0.03172 0.00000 0.00000 H20B 0.52548 0.64415 0.70869 1.00000 0.03172 0.00000 0.00000 H20C 0.58124 0.53186 0.74879 1.00000 0.03172 0.00000 0.00000 N1 0.78569 0.81491 0.75615 1.00000 0.02037 0.01478 0.01452 -0.00087 0.00204 -0.00154 0.01652 0.00239 0.00023 0.00013 0.00005 0.00000 0.00080 0.00078 0.00070 0.00061 0.00059 0.00065 0.00033 O1 0.86772 1.00544 0.79211 1.00000 0.02565 0.01688 0.02242 -0.00145 0.00536 -0.00333 0.02149 0.00211 0.00020 0.00011 0.00005 0.00000 0.00072 0.00071 0.00064 0.00054 0.00053 0.00060 0.00030 O2 1.07395 0.69481 0.94892 1.00000 0.04493 0.03242 0.02641 -0.00141 -0.01648 0.00319 0.03532 0.00231 0.00023 0.00013 0.00005 0.00000 0.00093 0.00085 0.00071 0.00063 0.00066 0.00071 0.00037 S1 0.49400 0.74510 0.82017 1.00000 0.01577 0.02284 0.01805 -0.00416 0.00194 -0.00323 0.01885 0.00074 0.00007 0.00004 0.00002 0.00000 0.00025 0.00027 0.00023 0.00019 0.00017 0.00020 0.00014 Final Structure Factor Calculation for 02esp402 in P2(1)/c Total number of l.s. parameters = 219 Maximum vector length = 511 Memory required = 2504 / 24017 wR2 = 0.0867 before cycle 5 for 2901 data and 0 / 219 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0372 * P )^2 + 0.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0352 for 2320 Fo > 4sig(Fo) and 0.0506 for all 2901 data wR2 = 0.0867, GooF = S = 1.035, Restrained GooF = 1.035 for all data Occupancy sum of asymmetric unit = 24.00 for non-hydrogen and 19.00 for hydrogen atoms Principal mean square atomic displacements U 0.0266 0.0215 0.0183 C1 0.0343 0.0300 0.0155 C2 0.0387 0.0210 0.0140 C3 0.0325 0.0225 0.0165 C4 0.0233 0.0211 0.0177 C5 0.0229 0.0144 0.0111 C6 0.0196 0.0169 0.0107 C7 0.0184 0.0168 0.0121 C8 0.0219 0.0155 0.0118 C9 0.0222 0.0214 0.0157 C10 0.0348 0.0202 0.0160 C11 0.0413 0.0174 0.0135 C12 0.0314 0.0212 0.0144 C13 0.0224 0.0189 0.0186 C14 0.0199 0.0169 0.0157 C15 0.0395 0.0190 0.0112 C16 0.0478 0.0341 0.0161 C17 0.0215 0.0192 0.0156 C18 0.0191 0.0167 0.0160 C19 0.0272 0.0212 0.0151 C20 0.0209 0.0149 0.0138 N1 0.0291 0.0196 0.0158 O1 0.0581 0.0319 0.0159 O2 0.0261 0.0160 0.0144 S1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.032 0.048 0.066 0.084 0.108 0.138 0.177 0.248 1.000 Number in group 292. 299. 280. 292. 290. 294. 284. 293. 288. 289. GooF 0.773 0.941 1.047 1.176 1.153 1.022 1.113 1.096 0.951 1.019 K 1.777 0.982 1.017 1.006 0.997 0.995 0.990 0.997 1.009 1.011 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.25 1.44 1.80 inf Number in group 298. 288. 289. 296. 279. 292. 290. 292. 287. 290. GooF 0.990 0.903 0.920 0.956 0.953 0.935 0.869 0.877 1.329 1.444 K 1.032 1.033 1.028 1.007 1.016 1.005 0.995 0.997 1.019 1.003 R1 0.109 0.089 0.074 0.073 0.062 0.043 0.031 0.031 0.036 0.026 Recommended weighting scheme: WGHT 0.0349 0.6091 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 3 12 73.87 39.26 4.99 0.047 1.79 0 4 8 39.04 71.72 4.72 0.063 2.04 2 3 11 171.50 119.42 4.15 0.081 1.59 1 4 0 79.65 115.80 4.04 0.080 2.49 -1 3 11 97.97 67.06 3.94 0.061 1.85 3 2 2 66.15 102.50 3.93 0.075 1.88 0 1 12 412.73 332.15 3.80 0.135 2.02 1 0 8 81.82 55.41 3.59 0.055 2.70 2 1 10 73.84 110.99 3.43 0.078 1.85 2 2 10 194.76 248.95 3.40 0.117 1.77 -2 3 8 52.74 33.24 3.35 0.043 1.91 1 0 4 26.98 45.67 3.34 0.050 4.24 1 6 6 26.24 59.16 3.32 0.057 1.59 3 3 5 452.22 371.99 3.25 0.143 1.65 5 6 12 229.51 299.41 3.19 0.128 0.90 0 5 8 96.82 70.63 3.03 0.062 1.78 1 5 2 21.03 9.01 3.01 0.022 2.02 0 9 18 1242.40 1051.97 2.99 0.241 0.91 0 3 10 318.38 378.93 2.94 0.144 2.04 2 3 6 38.54 23.01 2.92 0.036 2.00 -2 9 19 465.24 570.09 2.92 0.177 0.86 -1 4 7 3104.03 2750.65 2.90 0.389 2.06 -2 10 8 5.22 50.04 2.90 0.053 0.98 -3 2 2 1761.06 1527.58 2.81 0.290 1.91 5 5 0 30.47 55.02 2.79 0.055 1.07 3 3 0 0.29 6.92 2.77 0.020 1.79 0 2 15 38.71 60.86 2.72 0.058 1.58 -5 4 1 28.99 2.35 2.72 0.011 1.12 2 2 5 860.01 751.76 2.72 0.203 2.31 1 7 17 189.61 236.81 2.72 0.114 1.04 -3 1 6 27.52 42.45 2.70 0.048 1.85 -1 1 13 278.75 234.38 2.67 0.114 1.82 0 5 4 423.24 490.37 2.64 0.164 2.06 -3 2 8 104.74 133.73 2.61 0.086 1.67 -2 3 3 14.24 6.69 2.61 0.019 2.29 1 3 5 180.31 148.56 2.61 0.090 2.61 -4 5 8 129.77 175.26 2.60 0.098 1.18 1 1 0 14111.95 15737.42 2.59 0.931 5.36 3 5 0 345.50 293.55 2.56 0.127 1.49 4 7 15 123.28 69.65 2.56 0.062 0.89 1 2 14 30.61 13.83 2.55 0.028 1.60 2 4 4 582.02 508.45 2.55 0.167 1.91 -2 3 12 32.77 21.49 2.55 0.034 1.58 0 3 25 207.14 253.58 2.54 0.118 0.95 -5 6 3 63.01 97.87 2.53 0.073 1.02 -1 11 10 184.54 123.79 2.52 0.083 0.91 1 2 5 369.62 426.31 2.52 0.153 3.09 1 4 10 2614.66 2326.64 2.52 0.358 1.73 3 3 2 613.43 533.99 2.50 0.171 1.76 -1 2 13 939.51 834.62 2.50 0.214 1.75 Bond lengths and angles C1 - Distance Angles C6 1.3850 (0.0024) C2 1.3917 (0.0025) 119.63 (0.17) C1 - C6 C2 - Distance Angles C3 1.3841 (0.0027) C1 1.3917 (0.0025) 119.92 (0.17) C2 - C3 C3 - Distance Angles C2 1.3841 (0.0027) C4 1.3844 (0.0026) 120.10 (0.16) C3 - C2 C4 - Distance Angles C3 1.3844 (0.0026) C5 1.3892 (0.0025) 120.11 (0.17) C4 - C3 C5 - Distance Angles C6 1.3812 (0.0024) C4 1.3892 (0.0025) 119.64 (0.17) C5 - C6 C6 - Distance Angles C5 1.3812 (0.0024) C1 1.3850 (0.0024) 120.57 (0.15) N1 1.4422 (0.0021) 119.99 (0.15) 119.42 (0.15) C6 - C5 C1 C7 - Distance Angles O1 1.2149 (0.0021) N1 1.3589 (0.0021) 126.91 (0.15) C8 1.5549 (0.0023) 125.52 (0.15) 107.49 (0.14) C7 - O1 N1 C8 - Distance Angles C9 1.5071 (0.0023) C7 1.5549 (0.0023) 112.13 (0.14) C15 1.5749 (0.0024) 117.91 (0.13) 102.50 (0.13) S1 1.8432 (0.0017) 116.81 (0.12) 101.20 (0.10) 104.09 (0.11) C8 - C9 C7 C15 C9 - Distance Angles C10 1.3908 (0.0024) C14 1.3971 (0.0024) 118.64 (0.16) C8 1.5071 (0.0023) 121.51 (0.15) 119.56 (0.15) C9 - C10 C14 C10 - Distance Angles C9 1.3908 (0.0024) C11 1.3920 (0.0025) 120.69 (0.17) C10 - C9 C11 - Distance Angles C12 1.3842 (0.0026) C10 1.3920 (0.0025) 120.11 (0.17) C11 - C12 C12 - Distance Angles C13 1.3832 (0.0027) C11 1.3842 (0.0026) 119.70 (0.17) C12 - C13 C13 - Distance Angles C12 1.3832 (0.0027) C14 1.3880 (0.0025) 120.38 (0.17) C13 - C12 C14 - Distance Angles C13 1.3880 (0.0025) C9 1.3971 (0.0024) 120.47 (0.17) C14 - C13 C15 - Distance Angles C16 1.5288 (0.0023) C18 1.5585 (0.0023) 112.95 (0.14) C8 1.5749 (0.0024) 115.88 (0.14) 104.50 (0.13) C15 - C16 C18 C16 - Distance Angles O2 1.2171 (0.0022) C17 1.5029 (0.0028) 121.17 (0.17) C15 1.5288 (0.0023) 118.86 (0.17) 119.93 (0.16) C16 - O2 C17 C17 - Distance Angles C16 1.5029 (0.0028) C17 - C18 - Distance Angles C19 1.5362 (0.0023) C15 1.5585 (0.0023) 105.84 (0.14) C18 - C19 C19 - Distance Angles N1 1.4838 (0.0023) C20 1.5065 (0.0023) 113.71 (0.13) C18 1.5362 (0.0023) 107.58 (0.14) 115.63 (0.15) S1 1.8448 (0.0017) 101.13 (0.11) 114.98 (0.12) 102.23 (0.11) C19 - N1 C20 C18 C20 - Distance Angles C19 1.5065 (0.0023) C20 - N1 - Distance Angles C7 1.3589 (0.0021) C6 1.4422 (0.0021) 123.86 (0.14) C19 1.4838 (0.0023) 111.72 (0.13) 124.04 (0.13) N1 - C7 C6 O1 - Distance Angles C7 1.2149 (0.0021) O1 - O2 - Distance Angles C16 1.2171 (0.0022) O2 - S1 - Distance Angles C8 1.8432 (0.0017) C19 1.8448 (0.0017) 80.30 (0.08) S1 - C8 FMAP and GRID set by program FMAP 2 1 16 GRID -3.846 -2 -1 3.846 2 1 R1 = 0.0504 for 2901 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.27 at 0.3147 0.1150 0.1299 [ 0.75 A from C9 ] Deepest hole -0.25 at 0.2431 0.2469 0.2013 [ 0.87 A from C19 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2874 / 27212 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6853 0.8850 0.8701 1.00000 0.05 0.27 0.75 C9 0.76 C8 1.88 C10 1.91 C14 Q2 1 0.5744 0.9814 0.8790 1.00000 0.05 0.23 0.78 C9 0.80 C10 1.48 H10 1.88 C14 Q3 1 0.8048 0.7964 0.8574 1.00000 0.05 0.22 0.75 C8 0.83 C15 1.50 H15 1.91 C7 Q4 1 0.6140 0.8005 0.8393 1.00000 0.05 0.22 0.81 C8 1.05 S1 1.94 C9 1.95 C15 Q5 1 0.7425 0.8702 0.8217 1.00000 0.05 0.20 0.74 C8 0.82 C7 1.77 N1 1.84 O1 Q6 1 0.9296 0.7795 0.6850 1.00000 0.05 0.19 0.82 C5 0.86 C6 1.58 H5 1.76 C4 Q7 1 0.9247 0.9104 0.6119 1.00000 0.05 0.18 0.78 C2 0.79 C3 1.51 H2 1.52 H3 Q8 1 0.7370 0.9754 0.8999 1.00000 0.05 0.18 0.66 C9 0.82 C14 1.56 H14 1.73 C10 Q9 1 0.5881 0.7032 0.7892 1.00000 0.05 0.18 0.84 C19 1.09 S1 1.80 C20 1.94 N1 Q10 1 0.3998 0.8117 0.7950 1.00000 0.05 0.17 1.10 S1 2.32 C8 2.36 C19 2.41 H10 Q11 1 0.4709 0.6823 0.8552 1.00000 0.05 0.17 1.12 S1 2.14 H17C 2.25 H17B 2.33 C8 Q12 1 0.8770 0.6930 0.8441 1.00000 0.05 0.16 0.78 C15 0.81 C18 1.40 H18B 1.53 H15 Q13 1 1.0090 0.7769 0.8673 1.00000 0.05 0.16 0.34 H15 0.71 C15 1.75 C16 1.95 C8 Q14 1 0.7402 0.7599 0.7616 1.00000 0.05 0.16 0.68 N1 0.82 C19 1.79 C7 1.86 C6 Q15 1 0.5772 0.9133 0.9000 1.00000 0.05 0.16 0.66 C9 1.09 C10 1.66 H10 1.78 C8 Q16 1 0.6660 0.6513 0.7582 1.00000 0.05 0.16 0.71 C19 0.81 C20 1.42 H20C 1.46 H20B Q17 1 0.3088 0.6189 0.7153 1.00000 0.05 0.16 1.38 H20B 1.65 O1 1.71 H5 2.06 C20 Q18 1 0.8841 0.7255 0.8900 1.00000 0.05 0.15 0.72 C15 0.83 C16 1.47 H15 1.85 O2 Q19 1 0.5065 0.8593 0.8107 1.00000 0.05 0.15 1.27 S1 1.57 C8 1.91 C7 2.06 H10 Q20 1 0.8077 0.6755 0.7965 1.00000 0.05 0.15 0.76 C18 0.78 C19 1.41 H18A 1.49 H18B Shortest distances between peaks (including symmetry equivalents) 2 15 0.90 10 19 0.91 1 15 1.07 9 16 1.09 2 8 1.10 13 18 1.13 4 19 1.14 12 18 1.19 8 15 1.19 4 5 1.20 3 18 1.20 3 4 1.23 3 5 1.24 12 20 1.24 1 4 1.26 1 8 1.26 3 12 1.26 1 3 1.26 14 16 1.27 1 5 1.28 16 20 1.28 1 2 1.28 3 13 1.29 14 20 1.31 12 13 1.33 9 14 1.34 9 20 1.39 5 19 1.47 4 11 1.62 4 9 1.63 9 10 1.67 4 10 1.67 1 19 1.81 9 11 1.84 9 19 1.86 5 14 1.91 4 15 1.97 4 12 2.00 3 20 2.00 10 11 2.08 4 20 2.13 5 12 2.16 4 14 2.16 1 18 2.17 2 19 2.17 2 5 2.17 9 12 2.18 4 18 2.18 5 9 2.18 5 13 2.19 3 15 2.21 14 19 2.22 3 19 2.22 2 4 2.22 11 19 2.24 5 8 2.25 5 20 2.25 3 8 2.27 5 10 2.27 12 14 2.28 5 15 2.29 6 14 2.29 6 7 2.30 15 19 2.31 1 13 2.32 3 9 2.32 13 20 2.36 10 14 2.37 18 20 2.40 3 11 2.40 3 14 2.41 16 17 2.41 5 18 2.44 12 16 2.47 1 12 2.51 4 13 2.51 4 8 2.51 11 12 2.54 2 3 2.54 1 11 2.59 10 16 2.60 11 20 2.60 9 17 2.60 1 10 2.61 4 16 2.62 11 18 2.68 19 20 2.77 11 16 2.77 5 11 2.80 15 18 2.81 11 15 2.81 16 19 2.82 8 19 2.85 1 9 2.85 3 10 2.86 6 16 2.87 5 17 2.87 8 13 2.88 5 16 2.88 8 18 2.88 2 17 2.90 10 17 2.91 10 20 2.92 2 10 2.94 10 15 2.97 6 17 2.98 12 19 2.99 Time profile in seconds ----------------------- 0.11: 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. 0.27: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.06: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.00: Structure factors and derivatives 1.39: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.11: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.11: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 10:54:45 Total elapsed time: 3.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++