********************************************** ** REDUCED 2 MBYTE VERSION ** ********************************************** +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-92 - CRYSTAL STRUCTURE REFINEMENT - LAHEY GAMMA-TEST + + S92 started at 14:15:18 on 12/03/98 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL S92 in P2(1)/c CELL 0.71073 8.252 10.535 19.923 90.00 99.17 90.00 ZERR 4.00 0.002 0.002 0.004 0.00 0.03 0.00 LATT 1 SYMM -X, .5+Y, .5-Z SFAC C H N O S UNIT 68 72 16 8 4 V = 1709.87 F(000) = 720.0 Mu = 0.21 mm-1 Cell Wt = 1369.66 Rho = 1.330 L.S. 4 FMAP 2 PLAN 10 WGHT 0.0881 0.5930 FVAR 0.48396 S11 5 0.22563 0.29430 0.14387 11.00000 0.02331 0.03335 = 0.03112 -0.00519 0.00424 0.00134 C17 1 0.15338 0.20806 0.02194 11.00000 0.02710 0.03137 = 0.02914 0.00204 0.00552 0.00150 C15 1 -0.09750 0.30378 0.16245 11.00000 0.02437 0.02884 = 0.03170 0.00130 0.00262 0.00284 N12 3 0.24890 0.20172 0.08360 11.00000 0.02973 0.03507 = 0.02618 -0.00229 0.00409 0.00737 O11 4 0.36514 0.27380 0.19690 11.00000 0.02381 0.06053 = 0.03476 -0.01075 0.00055 0.00119 N13 3 0.17367 0.10753 -0.01871 11.00000 0.03628 0.03365 = 0.02778 -0.00008 0.00176 0.00362 C14 1 0.05163 0.24003 0.17597 11.00000 0.02418 0.02929 = 0.02606 -0.00420 0.00169 0.00248 C13 1 0.06243 0.12815 0.21386 11.00000 0.02881 0.03340 = 0.03083 -0.00036 0.00244 0.00947 C31 1 0.45529 0.30209 -0.09095 11.00000 0.03781 0.03501 = 0.03783 0.00486 0.00354 0.00034 C34 1 0.62786 0.09065 -0.03262 11.00000 0.03903 0.02823 = 0.02756 0.00088 0.00009 0.00349 H34 2 0.62990 0.08678 -0.03527 11.00000 -1.20000 C36 1 0.47816 0.19536 -0.12954 11.00000 0.04977 0.04121 = 0.02811 0.00257 0.00027 0.00144 O12 4 0.19627 0.42593 0.12434 11.00000 0.03968 0.02893 = 0.05137 -0.00401 0.01481 -0.00263 C11 1 -0.22482 0.14452 0.22485 11.00000 0.02981 0.03217 = 0.02830 -0.00052 0.00578 0.00242 C18 1 0.09505 0.09486 -0.08338 11.00000 0.04877 0.04340 = 0.02948 -0.00127 -0.00107 0.00033 N11 3 -0.35961 0.09654 0.24758 11.00000 0.03437 0.04698 = 0.05504 0.01553 0.01579 0.00495 H11A 2 -0.44689 0.13923 0.23652 11.00000 -1.20000 H11B 2 -0.34995 0.03829 0.27511 11.00000 -1.20000 C32 1 0.51874 0.29768 -0.02211 11.00000 0.04701 0.03301 = 0.03598 -0.00418 0.00267 0.00112 C21 1 0.04025 0.30203 -0.00648 11.00000 0.03724 0.03501 = 0.04014 0.00384 0.00304 0.00743 C16 1 -0.23444 0.25715 0.18683 11.00000 0.02362 0.03216 = 0.03373 0.00031 0.00282 0.00473 C12 1 -0.07266 0.08146 0.23833 11.00000 0.03602 0.03272 = 0.03056 0.00494 0.00643 0.00695 C35 1 0.56461 0.09301 -0.09891 11.00000 0.04939 0.03737 = 0.03076 -0.00252 0.00497 0.00421 C20 1 -0.04115 0.28950 -0.07195 11.00000 0.04166 0.04724 = 0.04293 0.01063 -0.00386 0.00797 C33 1 0.60288 0.19218 0.00455 11.00000 0.04909 0.04105 = 0.02928 -0.00252 -0.00071 0.00177 C19 1 -0.01331 0.18483 -0.11182 11.00000 0.05104 0.05377 = 0.03228 0.00367 -0.00792 0.00077 N31 3 0.36359 0.41717 -0.12187 11.00000 0.08073 0.05682 = 0.07776 0.01693 0.00110 0.01696 H16 2 -0.33669 0.30466 0.17916 11.00000 0.03304 H33 2 0.65061 0.18540 0.05243 11.00000 0.05310 H13 2 0.16799 0.08347 0.22541 11.00000 0.03967 H15 2 -0.10739 0.38249 0.13649 11.00000 0.03660 H32 2 0.49492 0.36765 0.00528 11.00000 0.04750 H21 2 0.01979 0.36997 0.02058 11.00000 0.04437 H35 2 0.58409 0.01920 -0.12552 11.00000 0.03814 H12 2 -0.06135 0.01035 0.26220 11.00000 0.04987 H17 2 0.24190 0.04132 -0.00003 11.00000 0.04573 H36 2 0.42920 0.19427 -0.17538 11.00000 0.08854 H20 2 -0.11419 0.35806 -0.08816 11.00000 0.04954 H18 2 0.11562 0.01746 -0.10800 11.00000 0.05056 H19 2 -0.05870 0.17556 -0.15365 11.00000 0.05849 H30 2 0.45517 0.49574 -0.13282 11.00000 0.12226 H31 2 0.32220 0.47660 -0.07850 11.00000 0.05000 H37 2 0.28810 0.38810 -0.17240 11.00000 0.05000 HKLF 4 1 -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000-1.0000 Covalent radii and connectivity table for S92 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 S11 - O11 O12 N12 C14 C17 - N12 N13 C21 C15 - C16 C14 N12 - C17 S11 O11 - S11 N13 - C18 C17 C14 - C15 C13 S11 C13 - C12 C14 C31 - C32 C36 N31 C34 - C33 C35 C36 - C35 C31 O12 - S11 C11 - N11 C16 C12 C18 - N13 C19 N11 - C11 C32 - C33 C31 C21 - C20 C17 C16 - C15 C11 C12 - C13 C11 C35 - C34 C36 C20 - C21 C19 C33 - C34 C32 C19 - C18 C20 N31 - C31 h k l Fo^2 Sigma Why rejected -1 0 1 0.44 0.11 observed but should be systematically absent -1 0 3 4.67 0.43 observed but should be systematically absent 0 0 5 2.28 0.54 observed but should be systematically absent 0 1 0 1.61 0.11 observed but should be systematically absent 0 1 0 1.08 0.22 observed but should be systematically absent 1 0 5 2.82 0.54 observed but should be systematically absent 2 0 1 2.36 0.43 observed but should be systematically absent 37342 Reflections read, of which 1270 rejected -11 =< h =< 11, -15 =< k =< 15, -28 =< l =< 28, Max. 2-theta = 61.01 7 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 0 1 1 233.77 3.43 9 20.63 0 0 2 112.46 2.69 4 21.10 2 Inconsistent equivalents 5111 Unique reflections, of which 0 suppressed R(int) = 0.0457 R(sigma) = 0.0322 Friedel opposites merged Maximum memory for data reduction = 1740 / 51248 ** Cell contents from UNIT instruction and atom list do not agree ** Unit-cell contents from UNIT instruction and atom list resp. C 68.00 68.00 H 72.00 76.00 N 16.00 16.00 O 8.00 8.00 S 4.00 4.00 10.5 seconds CPU time Least-squares cycle 1 Maximum vector length = 511 Memory required = 2389 / 362661 wR2 = 0.1547 before cycle 1 for 5111 data and 290 / 290 parameters GooF = S = 1.034; Restrained GooF = 1.034 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0881 * P )^2 + 0.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48459 0.00116 0.547 OSF 85 -0.03321 0.00017 -3.463 z C34 94 -0.02686 0.00223 3.768 z H34 218 0.36467 0.00033 3.235 x N31 224 0.01329 0.00113 -3.218 U23 N31 286 0.08470 0.00609 5.700 U11 H31 287 0.27852 0.00301 -3.179 x H37 290 0.09556 0.00617 7.388 U11 H37 Mean shift/esd = 0.482 Maximum = 7.388 for U11 H37 Max. shift = 0.180 A for H34 Max. dU = 0.046 for H37 16.4 seconds CPU time Least-squares cycle 2 Maximum vector length = 511 Memory required = 2389 / 362661 wR2 = 0.1512 before cycle 2 for 5111 data and 290 / 290 parameters GooF = S = 1.010; Restrained GooF = 1.010 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0881 * P )^2 + 0.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48446 0.00113 -0.121 OSF 85 -0.03250 0.00014 5.020 z C34 94 -0.03909 0.00193 -6.326 z H34 Mean shift/esd = 0.233 Maximum = -6.326 for z H34 Max. shift = 0.254 A for H34 Max. dU = 0.025 for H37 16.5 seconds CPU time Least-squares cycle 3 Maximum vector length = 511 Memory required = 2389 / 362661 wR2 = 0.1513 before cycle 3 for 5111 data and 290 / 290 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0881 * P )^2 + 0.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48432 0.00114 -0.125 OSF 85 -0.03304 0.00015 -3.655 z C34 94 -0.02918 0.00206 4.814 z H34 Mean shift/esd = 0.165 Maximum = 4.814 for z H34 Max. shift = 0.200 A for H34 Max. dU = 0.006 for H37 16.3 seconds CPU time Least-squares cycle 4 Maximum vector length = 511 Memory required = 2389 / 362661 wR2 = 0.1510 before cycle 4 for 5111 data and 290 / 290 parameters GooF = S = 1.009; Restrained GooF = 1.009 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0881 * P )^2 + 0.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48439 0.00113 0.069 OSF 85 -0.03259 0.00016 2.761 z C34 88 0.02808 0.00085 -1.527 U33 C34 89 0.00097 0.00060 -1.314 U23 C34 94 -0.03607 0.00212 -3.256 z H34 Mean shift/esd = 0.107 Maximum = -3.256 for z H34 Max. shift = 0.137 A for H34 Max. dU =-0.003 for H30 Largest correlation matrix elements 0.871 x H34 / x C34 0.863 z H34 / z C34 0.866 y H34 / y C34 0.515 U11 S11 / OSF 21.9 seconds CPU time S92 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S11 0.22563 0.29432 0.14386 1.00000 0.02335 0.03339 0.03117 -0.00517 0.00425 0.00132 0.02931 0.00004 0.00004 0.00002 0.00000 0.00018 0.00022 0.00021 0.00014 0.00013 0.00013 0.00012 C17 0.15330 0.20803 0.02192 1.00000 0.02725 0.03154 0.02885 0.00209 0.00553 0.00159 0.02910 0.00019 0.00014 0.00008 0.00000 0.00067 0.00075 0.00074 0.00057 0.00054 0.00056 0.00030 C15 -0.09751 0.30375 0.16247 1.00000 0.02443 0.02864 0.03181 0.00135 0.00260 0.00287 0.02850 0.00018 0.00014 0.00008 0.00000 0.00066 0.00072 0.00076 0.00058 0.00054 0.00054 0.00031 N12 0.24895 0.20172 0.08360 1.00000 0.02976 0.03483 0.02644 -0.00221 0.00398 0.00748 0.03040 0.00016 0.00013 0.00007 0.00000 0.00063 0.00068 0.00064 0.00050 0.00048 0.00050 0.00028 O11 0.36513 0.27382 0.19696 1.00000 0.02381 0.06031 0.03518 -0.01075 0.00062 0.00115 0.04021 0.00014 0.00013 0.00006 0.00000 0.00053 0.00079 0.00064 0.00056 0.00045 0.00050 0.00030 N13 0.17364 0.10753 -0.01870 1.00000 0.03639 0.03352 0.02819 0.00006 0.00155 0.00370 0.03309 0.00018 0.00014 0.00007 0.00000 0.00069 0.00068 0.00067 0.00053 0.00052 0.00056 0.00029 C14 0.05159 0.24003 0.17599 1.00000 0.02424 0.02956 0.02604 -0.00421 0.00166 0.00251 0.02687 0.00017 0.00014 0.00008 0.00000 0.00063 0.00070 0.00069 0.00055 0.00050 0.00054 0.00029 C13 0.06248 0.12815 0.21381 1.00000 0.02882 0.03361 0.03067 -0.00053 0.00244 0.00953 0.03128 0.00019 0.00015 0.00008 0.00000 0.00070 0.00078 0.00077 0.00059 0.00056 0.00060 0.00032 C31 0.45530 0.30208 -0.09091 1.00000 0.03765 0.03502 0.03817 0.00467 0.00344 0.00029 0.03723 0.00022 0.00016 0.00009 0.00000 0.00084 0.00084 0.00089 0.00066 0.00067 0.00066 0.00036 C34 0.62780 0.09062 -0.03259 1.00000 0.03911 0.02837 0.02808 0.00097 0.00037 0.00355 0.03240 0.00042 0.00030 0.00016 0.00000 0.00085 0.00073 0.00085 0.00060 0.00063 0.00062 0.00035 H34 0.63042 0.08771 -0.03607 1.00000 0.03888 0.00517 0.00380 0.00212 0.00000 0.00000 C36 0.47828 0.19524 -0.12957 1.00000 0.04966 0.04137 0.02784 0.00254 0.00023 0.00154 0.04027 0.00025 0.00017 0.00010 0.00000 0.00100 0.00093 0.00083 0.00069 0.00069 0.00076 0.00039 O12 0.19632 0.42595 0.12433 1.00000 0.03951 0.02918 0.05123 -0.00432 0.01482 -0.00283 0.03915 0.00015 0.00011 0.00007 0.00000 0.00063 0.00058 0.00075 0.00051 0.00053 0.00047 0.00029 C11 -0.22476 0.14455 0.22484 1.00000 0.02978 0.03225 0.02837 -0.00055 0.00570 0.00215 0.03002 0.00019 0.00015 0.00008 0.00000 0.00070 0.00075 0.00074 0.00058 0.00054 0.00058 0.00031 C18 0.09498 0.09488 -0.08336 1.00000 0.04886 0.04343 0.02889 -0.00154 -0.00096 0.00050 0.04117 0.00024 0.00019 0.00009 0.00000 0.00099 0.00096 0.00086 0.00071 0.00069 0.00078 0.00040 N11 -0.35954 0.09657 0.24776 1.00000 0.03458 0.04687 0.05482 0.01505 0.01603 0.00488 0.04445 0.00020 0.00017 0.00009 0.00000 0.00075 0.00091 0.00101 0.00074 0.00068 0.00066 0.00039 H11A -0.44740 0.13973 0.23844 1.00000 0.05334 0.00319 0.00228 0.00126 0.00000 0.00000 H11B -0.35490 0.03455 0.27414 1.00000 0.05334 0.00299 0.00236 0.00127 0.00000 0.00000 C32 0.51875 0.29776 -0.02215 1.00000 0.04683 0.03333 0.03601 -0.00421 0.00280 0.00089 0.03914 0.00024 0.00016 0.00010 0.00000 0.00097 0.00084 0.00089 0.00068 0.00071 0.00070 0.00038 C21 0.04024 0.30207 -0.00642 1.00000 0.03730 0.03511 0.03986 0.00406 0.00315 0.00737 0.03775 0.00022 0.00016 0.00010 0.00000 0.00085 0.00085 0.00093 0.00071 0.00068 0.00067 0.00037 C16 -0.23441 0.25712 0.18681 1.00000 0.02391 0.03207 0.03341 0.00022 0.00269 0.00478 0.03000 0.00018 0.00015 0.00008 0.00000 0.00065 0.00075 0.00080 0.00060 0.00055 0.00057 0.00031 C12 -0.07278 0.08137 0.23828 1.00000 0.03595 0.03262 0.03085 0.00488 0.00661 0.00682 0.03300 0.00020 0.00016 0.00009 0.00000 0.00079 0.00079 0.00080 0.00062 0.00061 0.00063 0.00034 C35 0.56453 0.09302 -0.09892 1.00000 0.04936 0.03715 0.03139 -0.00274 0.00525 0.00419 0.03943 0.00024 0.00017 0.00009 0.00000 0.00098 0.00087 0.00089 0.00068 0.00071 0.00073 0.00038 C20 -0.04113 0.28941 -0.07194 1.00000 0.04167 0.04758 0.04337 0.01091 -0.00401 0.00801 0.04538 0.00025 0.00019 0.00011 0.00000 0.00094 0.00102 0.00102 0.00082 0.00076 0.00080 0.00044 C33 0.60290 0.19216 0.00450 1.00000 0.04888 0.04082 0.02956 -0.00239 -0.00090 0.00151 0.04053 0.00024 0.00017 0.00010 0.00000 0.00100 0.00096 0.00086 0.00069 0.00070 0.00075 0.00040 C19 -0.01322 0.18484 -0.11176 1.00000 0.05131 0.05353 0.03225 0.00363 -0.00783 0.00080 0.04728 0.00027 0.00020 0.00011 0.00000 0.00109 0.00112 0.00095 0.00079 0.00077 0.00087 0.00046 N31 0.36450 0.41707 -0.12192 1.00000 0.08178 0.05725 0.07389 0.01352 -0.00007 0.01883 0.07233 0.00032 0.00022 0.00013 0.00000 0.00153 0.00122 0.00152 0.00106 0.00120 0.00110 0.00062 H16 -0.34064 0.30427 0.17887 1.00000 0.03320 0.00251 0.00171 0.00101 0.00000 0.00481 H33 0.64917 0.18479 0.05158 1.00000 0.04930 0.00289 0.00210 0.00125 0.00000 0.00613 H13 0.16717 0.08139 0.22480 1.00000 0.04200 0.00268 0.00194 0.00109 0.00000 0.00539 H15 -0.10787 0.38070 0.13591 1.00000 0.04042 0.00258 0.00197 0.00109 0.00000 0.00516 H32 0.49361 0.36759 0.00683 1.00000 0.04727 0.00290 0.00207 0.00123 0.00000 0.00568 H21 0.01965 0.37135 0.02017 1.00000 0.04206 0.00273 0.00202 0.00111 0.00000 0.00544 H35 0.58340 0.01849 -0.12475 1.00000 0.03798 0.00240 0.00192 0.00102 0.00000 0.00503 H12 -0.06287 0.00967 0.26186 1.00000 0.05048 0.00275 0.00225 0.00118 0.00000 0.00599 H17 0.24209 0.04379 -0.00040 1.00000 0.04939 0.00277 0.00221 0.00113 0.00000 0.00597 H36 0.43147 0.19029 -0.17345 1.00000 0.08065 0.00386 0.00264 0.00166 0.00000 0.00906 H20 -0.11333 0.35787 -0.08979 1.00000 0.05524 0.00302 0.00229 0.00129 0.00000 0.00636 H18 0.11704 0.01909 -0.10676 1.00000 0.04513 0.00260 0.00208 0.00113 0.00000 0.00550 H19 -0.05778 0.17329 -0.15428 1.00000 0.05888 0.00315 0.00231 0.00139 0.00000 0.00689 H30 0.45688 0.49884 -0.13797 1.00000 0.11990 0.00497 0.00399 0.00192 0.00000 0.01232 H31 0.30651 0.47896 -0.08051 1.00000 0.09855 0.00399 0.00320 0.00166 0.00000 0.01004 H37 0.26501 0.39302 -0.17284 1.00000 0.12577 0.00532 0.00374 0.00226 0.00000 0.01306 Final Structure Factor Calculation for S92 in P2(1)/c Total number of l.s. parameters = 290 Maximum vector length = 511 Memory required = 2099 / 23506 wR2 = 0.1505 before cycle 5 for 5111 data and 0 / 290 parameters GooF = S = 1.005; Restrained GooF = 1.005 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0881 * P )^2 + 0.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0498 for 3877 Fo > 4.sigma(Fo) and 0.0696 for all 5111 data wR2 = 0.1505, GooF = S = 1.005, Restrained GooF = 1.005 for all data 3.6 seconds CPU time Principal mean square atomic displacements U 0.0379 0.0271 0.0229 S11 0.0331 0.0277 0.0265 C17 0.0327 0.0301 0.0227 C15 0.0409 0.0267 0.0236 N12 0.0648 0.0329 0.0230 O11 0.0403 0.0318 0.0271 N13 0.0342 0.0235 0.0229 C14 0.0419 0.0306 0.0214 C13 0.0429 0.0373 0.0314 C31 0.0426 0.0292 0.0254 C34 0.0524 0.0418 0.0266 C36 0.0548 0.0344 0.0283 O12 0.0335 0.0296 0.0270 C11 0.0527 0.0434 0.0274 C18 0.0679 0.0363 0.0292 N11 0.0492 0.0380 0.0302 C32 0.0437 0.0421 0.0275 C21 0.0352 0.0332 0.0216 C16 0.0421 0.0311 0.0258 C12 0.0513 0.0369 0.0301 C35 0.0574 0.0527 0.0260 C20 0.0531 0.0406 0.0279 C33 0.0621 0.0538 0.0260 C19 0.0955 0.0812 0.0404 N31 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.016 0.024 0.034 0.044 0.057 0.073 0.099 0.150 1.000 Number in group 556. 498. 492. 514. 511. 501. 505. 517. 505. 512. GooF 0.857 1.013 0.994 1.077 1.113 1.078 1.007 0.928 1.017 0.961 K 0.877 0.891 1.009 0.949 0.953 0.972 0.998 1.021 1.036 1.003 Resolution(A) 0.70 0.73 0.76 0.79 0.83 0.89 0.96 1.05 1.20 1.51 inf Number in group 519. 506. 507. 514. 507. 516. 510. 512. 507. 513. GooF 0.855 0.869 0.854 0.870 0.883 0.841 0.875 0.929 1.030 1.719 K 0.989 1.002 1.034 1.051 1.031 1.020 1.020 1.037 1.026 0.984 R1 0.184 0.146 0.117 0.100 0.078 0.058 0.050 0.041 0.037 0.054 Recommended weighting scheme: WGHT 0.0827 0.5409 Most Disagreeable Reflections (* if suppressed) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 1 0 4 154.63 65.58 7.83 0.056 3.94 3 0 8 161.40 77.15 6.79 0.061 1.69 -1 0 12 55.64 21.83 6.05 0.032 1.66 -3 4 4 53.86 22.85 5.86 0.033 1.83 2 2 5 55.61 25.97 5.26 0.035 2.35 2 2 6 10.92 1.42 5.19 0.008 2.17 -1 2 8 0.96 11.30 4.47 0.023 2.23 0 3 6 432.26 290.41 4.32 0.118 2.40 -4 3 8 198.50 128.81 4.28 0.078 1.54 4 2 1 8.06 1.36 4.24 0.008 1.86 2 1 7 25.30 51.57 4.23 0.050 2.11 -1 2 6 43.20 21.58 4.23 0.032 2.75 -3 0 10 72.28 40.68 4.20 0.044 1.73 3 3 6 0.72 9.71 4.20 0.022 1.70 -2 3 4 9.11 25.13 4.17 0.035 2.45 0 2 13 29.90 56.14 3.86 0.052 1.45 -2 5 5 266.66 183.65 3.85 0.094 1.74 3 0 14 -5.34 9.12 3.80 0.021 1.17 4 1 6 104.32 161.98 3.77 0.088 1.60 1 6 4 10.01 24.51 3.76 0.034 1.60 3 3 0 302.11 213.12 3.68 0.101 2.15 2 0 10 674.95 487.49 3.57 0.153 1.67 4 1 2 17.47 34.48 3.57 0.041 1.90 -1 1 11 87.62 57.17 3.49 0.052 1.78 -1 3 6 55.26 88.09 3.47 0.065 2.38 -1 5 1 78.15 119.50 3.43 0.076 2.04 -1 2 9 50.70 31.13 3.37 0.039 2.03 -3 5 6 119.57 82.20 3.35 0.063 1.55 -10 0 16 13.42 50.41 3.35 0.049 0.74 4 2 24 4.22 30.33 3.30 0.038 0.71 -1 4 1 173.47 123.34 3.29 0.077 2.50 1 2 15 19.54 38.31 3.28 0.043 1.23 -3 1 2 514.77 384.32 3.24 0.136 2.64 -4 5 1 84.78 56.89 3.24 0.052 1.47 -1 0 14 10.62 3.00 3.21 0.012 1.42 -2 6 3 84.97 57.00 3.20 0.052 1.59 -6 0 4 76.00 49.60 3.13 0.049 1.37 -1 4 6 133.16 94.57 3.12 0.067 2.04 3 1 7 7.12 2.04 3.12 0.010 1.79 -3 1 6 688.57 926.67 3.12 0.210 2.23 -3 6 4 24.08 13.04 3.11 0.025 1.45 2 4 1 17.40 8.66 3.10 0.020 2.18 -1 14 1 0.16 15.82 3.07 0.027 0.75 -1 1 5 0.50 5.26 3.03 0.016 3.56 -6 1 10 4.49 0.27 3.03 0.004 1.20 -3 6 2 17.85 31.93 3.03 0.039 1.48 3 4 5 63.54 94.09 3.03 0.067 1.63 0 6 6 42.52 66.09 3.02 0.056 1.55 -2 4 1 50.30 75.96 3.01 0.060 2.22 0 0 10 1051.05 805.65 2.99 0.196 1.97 2.1 seconds CPU time FMAP and GRID set by program FMAP 2 1 23 GRID -2.500 -2 -1 2.500 2 1 R1 = 0.0692 for 5111 unique reflections after merging Electron density synthesis with coefficients Fo-Fc Maximum = 0.53, Minimum = -0.51 e/A^3, Highest memory used = 1683 / 38833 Mean = 0.00, Rms deviation from mean = 0.06 e/A^3 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.1560 0.2810 0.1775 1.00000 0.05 0.26 0.65 C15 0.74 C16 1.43 H15 1.55 H16 Q2 1 0.3731 0.4344 -0.1771 1.00000 0.05 0.25 1.01 H37 1.13 N31 1.17 H30 2.14 H31 Q3 1 0.1127 0.2608 0.1690 1.00000 0.05 0.25 0.59 C14 1.18 S11 1.74 C13 1.78 C15 Q4 1 0.0514 0.1773 0.1824 1.00000 0.05 0.23 0.67 C14 0.81 C13 1.55 H13 1.81 C15 Q5 1 -0.0110 0.2985 -0.0800 1.00000 0.05 0.23 0.33 C20 1.04 H20 1.35 C19 1.46 C21 Q6 1 -0.0277 0.2630 0.1628 1.00000 0.05 0.21 0.71 C14 0.72 C15 1.47 H15 1.83 C13 Q7 1 -0.2324 0.1872 0.1977 1.00000 0.05 0.21 0.70 C11 0.77 C16 1.53 H16 1.81 C12 Q8 1 0.1965 0.2056 0.0585 1.00000 0.05 0.21 0.61 N12 0.76 C17 1.84 N13 1.92 S11 Q9 1 -0.1531 0.1126 0.2312 1.00000 0.05 0.21 0.67 C11 0.73 C12 1.40 H12 1.79 N11 Q10 1 0.2214 0.3836 -0.1339 1.00000 0.05 0.20 0.91 H37 1.22 N31 1.55 H31 2.16 C31 Shortest distances between peaks (including symmetry equivalents) 3 4 1.07 3 6 1.15 4 6 1.15 1 6 1.16 7 9 1.16 1 7 1.27 2 10 1.71 1 4 2.02 1 9 2.07 6 7 2.09 4 9 2.19 1 3 2.26 4 7 2.41 6 9 2.43 3 8 2.48 5 10 2.51 4 8 2.92 5.0 seconds CPU time +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + S92 finished at 14:16:50 Total CPU time: 92.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++