+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 00ale002 started at 12:02:52 on 18-Apr-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 00ale002 in P 21/c stz form I CELL 0.71073 10.5340 12.9360 17.1910 90.000 107.770 90.000 ZERR 8.00 0.0020 0.0030 0.0030 0.000 0.030 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O S UNIT 72 72 24 16 16 V = 2230.81 F(000) = 1056.0 Mu = 0.47 mm-1 Cell Wt = 2042.50 Rho = 1.520 MERG 2 SHEL 7 0.84 FMAP 2 PLAN 5 SIZE 0.25 0.08 0.08 ACTA BOND $H CONF L.S. 5 TEMP -123.00 WGHT 0.052100 FVAR 0.15448 S11 5 0.692390 0.571869 -0.089593 11.00000 0.01917 0.03101 = 0.01767 0.00199 0.00264 -0.00216 S12 5 0.847233 0.755686 0.035771 11.00000 0.03080 0.02530 = 0.03301 -0.00239 0.00838 0.00191 S21 5 0.817765 0.073469 0.118501 11.00000 0.02412 0.02573 = 0.02132 0.00383 0.00400 0.00042 S22 5 0.635141 0.083064 -0.073381 11.00000 0.02229 0.05814 = 0.02697 -0.00719 -0.00166 0.01343 O11 4 0.662196 0.467873 -0.119917 11.00000 0.03288 0.02796 = 0.02767 0.00269 0.00142 -0.00869 O12 4 0.620194 0.611858 -0.037121 11.00000 0.02591 0.05082 = 0.02156 0.00317 0.01052 0.00256 O21 4 0.914443 0.033668 0.191572 11.00000 0.03917 0.03333 = 0.02232 0.00922 -0.00006 0.00407 O22 4 0.680187 0.043929 0.102447 11.00000 0.02663 0.03394 = 0.03496 0.00068 0.01093 -0.00604 N11 3 0.571596 0.842328 -0.380222 11.00000 0.03467 0.03047 = 0.02963 0.00809 0.01219 0.00596 N12 3 0.850866 0.570112 -0.045511 11.00000 0.01687 0.02775 = 0.01732 -0.00226 0.00067 -0.00047 N13 3 1.039105 0.632557 0.052168 11.00000 0.02152 0.02585 = 0.02664 -0.00273 0.00108 -0.00159 N21 3 0.843374 0.527599 0.151647 11.00000 0.03117 0.02690 = 0.02644 0.00064 0.00274 -0.00172 N22 3 0.874377 0.035641 0.045984 11.00000 0.02145 0.02521 = 0.02227 0.00068 0.00061 0.00454 N23 3 0.846561 0.011475 -0.091465 11.00000 0.01957 0.02886 = 0.02434 0.00046 0.00274 0.00561 C11 1 0.597744 0.777768 -0.313474 11.00000 0.02052 0.02690 = 0.02104 0.00172 0.00358 -0.00381 C12 1 0.663973 0.684490 -0.310918 11.00000 0.01909 0.03031 = 0.01906 -0.00324 0.00768 0.00130 C13 1 0.694366 0.622494 -0.242363 11.00000 0.01569 0.02432 = 0.02194 0.00103 0.00404 0.00237 C14 1 0.659428 0.653951 -0.174498 11.00000 0.01719 0.02788 = 0.01445 0.00068 0.00048 -0.00150 C15 1 0.592418 0.746492 -0.176537 11.00000 0.02640 0.03207 = 0.01880 -0.00384 0.00760 0.00281 C16 1 0.560170 0.807150 -0.245076 11.00000 0.02921 0.02452 = 0.02566 -0.00054 0.00679 0.00452 C17 1 0.910167 0.641797 0.008504 11.00000 0.02191 0.02391 = 0.01947 0.00444 0.00743 -0.00097 C18 1 1.087618 0.708928 0.109794 11.00000 0.03005 0.03383 = 0.02699 -0.00502 -0.00178 -0.00839 C19 1 0.998634 0.781011 0.109219 11.00000 0.03896 0.02386 = 0.03568 -0.00860 0.00770 -0.00621 C21 1 0.837329 0.423160 0.139892 11.00000 0.02590 0.02614 = 0.01577 0.00033 0.00734 -0.00069 C22 1 0.952335 0.362109 0.168395 11.00000 0.01872 0.03164 = 0.02390 -0.00561 0.00342 -0.00520 C23 1 0.947057 0.257213 0.159649 11.00000 0.01859 0.02935 = 0.02548 -0.00073 0.00286 0.00400 C24 1 0.825976 0.208204 0.123170 11.00000 0.02181 0.02582 = 0.01479 0.00028 0.00493 0.00079 C25 1 0.711026 0.267547 0.092679 11.00000 0.01776 0.03202 = 0.02353 -0.00310 0.00357 -0.00237 C26 1 0.716890 0.373219 0.100505 11.00000 0.02092 0.03201 = 0.02614 -0.00156 0.00234 0.00518 C27 1 0.798359 0.040775 -0.031936 11.00000 0.01728 0.02319 = 0.02573 -0.00026 0.00031 0.00038 C28 1 0.762602 0.026764 -0.169575 11.00000 0.02949 0.03533 = 0.02236 -0.00247 0.00071 0.00331 C29 1 0.645433 0.065652 -0.171456 11.00000 0.02974 0.05241 = 0.02089 -0.00725 -0.00464 0.01099 H10 2 0.500500 0.890104 -0.386157 11.00000 0.05441 H11 2 0.579582 0.815208 -0.422994 11.00000 0.03938 H12 2 0.685314 0.661187 -0.357025 11.00000 0.02244 H13 2 0.739448 0.559006 -0.241381 11.00000 0.01858 H15 2 0.565723 0.763343 -0.133260 11.00000 0.01792 H16 2 0.507338 0.866907 -0.249059 11.00000 0.02885 H17 2 1.083113 0.577672 0.052009 11.00000 0.02921 H18 2 1.173727 0.700157 0.144624 11.00000 0.03761 H19 2 1.007542 0.836723 0.142403 11.00000 0.02622 H20 2 0.763904 0.565836 0.135964 11.00000 0.02965 H21 2 0.919123 0.555003 0.181811 11.00000 0.03890 H22 2 1.033461 0.397313 0.194790 11.00000 0.02945 H23 2 1.022093 0.216676 0.178368 11.00000 0.02896 H25 2 0.628708 0.234666 0.070004 11.00000 0.03461 H26 2 0.639730 0.415624 0.081235 11.00000 0.03205 H27 2 0.928769 -0.011176 -0.079986 11.00000 0.04272 H28 2 0.793127 0.006333 -0.212661 11.00000 0.02918 H29 2 0.569429 0.079400 -0.216047 11.00000 0.06710 HKLF 4 Covalent radii and connectivity table for 00ale002 in P 21/c stz form I C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 S11 - O12 O11 N12 C14 S12 - C19 C17 S21 - O22 O21 N22 C24 S22 - C27 C29 O11 - S11 O12 - S11 O21 - S21 O22 - S21 N11 - C11 N12 - C17 S11 N13 - C17 C18 N21 - C21 N22 - C27 S21 N23 - C27 C28 C11 - N11 C12 C16 C12 - C13 C11 C13 - C12 C14 C14 - C15 C13 S11 C15 - C16 C14 C16 - C15 C11 C17 - N12 N13 S12 C18 - C19 N13 C19 - C18 S12 C21 - N21 C26 C22 C22 - C23 C21 C23 - C22 C24 C24 - C23 C25 S21 C25 - C26 C24 C26 - C25 C21 C27 - N23 N22 S22 C28 - C29 N23 C29 - C28 S22 h k l Fo^2 Sigma Why rejected -3 0 3 0.44 0.11 observed but should be systematically absent 23801 Reflections read, of which 4278 rejected -12 =< h =< 12, -13 =< k =< 15, -20 =< l =< 20, Max. 2-theta = 50.05 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -4 5 8 7.20 0.12 7 1.98 1 Inconsistent equivalents 3938 Unique reflections, of which 0 suppressed R(int) = 0.0878 R(sigma) = 0.0627 Friedel opposites merged Maximum memory for data reduction = 2931 / 39266 Least-squares cycle 1 Maximum vector length = 511 Memory required = 3784 / 459022 wR2 = 0.1016 before cycle 1 for 3938 data and 361 / 361 parameters GooF = S = 1.031; Restrained GooF = 1.031 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0521 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15448 0.00029 0.011 OSF Mean shift/esd = 0.002 Maximum = 0.012 for U12 S21 Max. shift = 0.000 A for H27 Max. dU = 0.000 for H10 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3784 / 459022 wR2 = 0.1016 before cycle 2 for 3938 data and 361 / 361 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0521 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15448 0.00029 0.000 OSF Mean shift/esd = 0.001 Maximum = 0.004 for U12 S21 Max. shift = 0.000 A for H27 Max. dU = 0.000 for H10 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3784 / 459022 wR2 = 0.1016 before cycle 3 for 3938 data and 361 / 361 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0521 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15448 0.00029 0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for x H27 Max. shift = 0.000 A for H27 Max. dU = 0.000 for H27 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3784 / 459022 wR2 = 0.1016 before cycle 4 for 3938 data and 361 / 361 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0521 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15448 0.00029 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x H27 Max. shift = 0.000 A for H27 Max. dU = 0.000 for H10 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3784 / 459022 wR2 = 0.1016 before cycle 5 for 3938 data and 361 / 361 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0521 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15448 0.00029 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x S21 Max. shift = 0.000 A for H11 Max. dU = 0.000 for H10 No correlation matrix elements larger than 0.500 00ale002 in P 21/c stz form I ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S11 0.69239 0.57187 -0.08959 1.00000 0.01917 0.03101 0.01767 0.00199 0.00264 -0.00216 0.02329 0.00128 0.00006 0.00005 0.00004 0.00000 0.00034 0.00040 0.00036 0.00029 0.00028 0.00028 0.00018 S12 0.84723 0.75569 0.03577 1.00000 0.03080 0.02530 0.03301 -0.00239 0.00838 0.00191 0.03001 0.00138 0.00007 0.00005 0.00004 0.00000 0.00040 0.00039 0.00044 0.00031 0.00034 0.00029 0.00020 S21 0.81776 0.07347 0.11850 1.00000 0.02412 0.02573 0.02132 0.00383 0.00400 0.00042 0.02438 0.00131 0.00006 0.00005 0.00004 0.00000 0.00036 0.00039 0.00038 0.00029 0.00029 0.00028 0.00019 S22 0.63514 0.08306 -0.07338 1.00000 0.02229 0.05814 0.02697 -0.00719 -0.00166 0.01343 0.03786 0.00148 0.00007 0.00007 0.00005 0.00000 0.00037 0.00055 0.00044 0.00036 0.00032 0.00034 0.00023 O11 0.66220 0.46787 -0.11992 1.00000 0.03288 0.02796 0.02767 0.00269 0.00142 -0.00869 0.03126 0.00343 0.00017 0.00014 0.00011 0.00000 0.00104 0.00111 0.00109 0.00085 0.00087 0.00084 0.00046 O12 0.62019 0.61186 -0.03712 1.00000 0.02591 0.05082 0.02156 0.00317 0.01052 0.00256 0.03203 0.00369 0.00017 0.00015 0.00011 0.00000 0.00097 0.00130 0.00104 0.00090 0.00085 0.00089 0.00047 O21 0.91444 0.03367 0.19157 1.00000 0.03917 0.03333 0.02232 0.00922 -0.00006 0.00407 0.03372 0.00365 0.00018 0.00014 0.00011 0.00000 0.00113 0.00117 0.00107 0.00086 0.00090 0.00090 0.00048 O22 0.68019 0.04393 0.10245 1.00000 0.02663 0.03394 0.03496 0.00068 0.01093 -0.00604 0.03150 0.00355 0.00017 0.00014 0.00011 0.00000 0.00101 0.00116 0.00119 0.00088 0.00090 0.00084 0.00047 N11 0.57160 0.84233 -0.38022 1.00000 0.03466 0.03047 0.02963 0.00809 0.01219 0.00596 0.03105 0.00515 0.00024 0.00020 0.00016 0.00000 0.00141 0.00147 0.00154 0.00120 0.00119 0.00115 0.00058 N12 0.85087 0.57011 -0.04551 1.00000 0.01687 0.02775 0.01732 -0.00226 0.00067 -0.00047 0.02167 0.00394 0.00019 0.00016 0.00012 0.00000 0.00106 0.00123 0.00117 0.00097 0.00092 0.00091 0.00049 N13 1.03910 0.63256 0.05217 1.00000 0.02152 0.02585 0.02664 -0.00273 0.00108 -0.00159 0.02608 0.00421 0.00021 0.00019 0.00014 0.00000 0.00120 0.00137 0.00136 0.00106 0.00103 0.00105 0.00054 N21 0.84337 0.52760 0.15165 1.00000 0.03117 0.02690 0.02644 0.00064 0.00274 -0.00172 0.02952 0.00513 0.00027 0.00019 0.00015 0.00000 0.00142 0.00140 0.00140 0.00108 0.00118 0.00122 0.00057 N22 0.87438 0.03564 0.04598 1.00000 0.02145 0.02521 0.02227 0.00068 0.00061 0.00454 0.02433 0.00410 0.00020 0.00016 0.00013 0.00000 0.00112 0.00126 0.00128 0.00097 0.00099 0.00094 0.00051 N23 0.84656 0.01147 -0.09147 1.00000 0.01957 0.02886 0.02434 0.00046 0.00274 0.00561 0.02515 0.00431 0.00022 0.00017 0.00013 0.00000 0.00117 0.00134 0.00134 0.00101 0.00106 0.00102 0.00053 C11 0.59774 0.77777 -0.31347 1.00000 0.02052 0.02690 0.02104 0.00172 0.00358 -0.00381 0.02344 0.00498 0.00024 0.00020 0.00016 0.00000 0.00130 0.00153 0.00148 0.00117 0.00115 0.00112 0.00060 C12 0.66397 0.68449 -0.31092 1.00000 0.01909 0.03031 0.01906 -0.00324 0.00768 0.00130 0.02240 0.00504 0.00023 0.00021 0.00016 0.00000 0.00131 0.00156 0.00149 0.00122 0.00116 0.00111 0.00059 C13 0.69437 0.62249 -0.24236 1.00000 0.01569 0.02432 0.02194 0.00103 0.00404 0.00237 0.02103 0.00493 0.00023 0.00021 0.00015 0.00000 0.00123 0.00147 0.00152 0.00118 0.00113 0.00113 0.00058 C14 0.65943 0.65395 -0.17450 1.00000 0.01719 0.02788 0.01445 0.00068 0.00048 -0.00150 0.02081 0.00474 0.00023 0.00019 0.00015 0.00000 0.00124 0.00151 0.00136 0.00111 0.00105 0.00111 0.00057 C15 0.59242 0.74649 -0.17654 1.00000 0.02640 0.03207 0.01880 -0.00384 0.00760 0.00281 0.02560 0.00529 0.00025 0.00021 0.00017 0.00000 0.00144 0.00163 0.00150 0.00124 0.00125 0.00119 0.00063 C16 0.56017 0.80715 -0.24508 1.00000 0.02921 0.02452 0.02566 -0.00054 0.00679 0.00452 0.02682 0.00526 0.00026 0.00022 0.00016 0.00000 0.00149 0.00157 0.00160 0.00125 0.00125 0.00126 0.00063 C17 0.91017 0.64180 0.00850 1.00000 0.02191 0.02391 0.01947 0.00444 0.00743 -0.00097 0.02151 0.00498 0.00023 0.00019 0.00015 0.00000 0.00134 0.00147 0.00143 0.00115 0.00117 0.00112 0.00058 C18 1.08762 0.70893 0.10979 1.00000 0.03005 0.03383 0.02699 -0.00502 -0.00178 -0.00839 0.03264 0.00549 0.00029 0.00023 0.00018 0.00000 0.00162 0.00176 0.00167 0.00136 0.00140 0.00143 0.00069 C19 0.99863 0.78101 0.10922 1.00000 0.03896 0.02386 0.03568 -0.00860 0.00770 -0.00621 0.03366 0.00587 0.00029 0.00023 0.00019 0.00000 0.00175 0.00163 0.00181 0.00141 0.00146 0.00138 0.00070 C21 0.83733 0.42316 0.13989 1.00000 0.02590 0.02614 0.01577 0.00033 0.00734 -0.00069 0.02238 0.00502 0.00024 0.00020 0.00015 0.00000 0.00140 0.00151 0.00139 0.00112 0.00119 0.00115 0.00059 C22 0.95233 0.36211 0.16839 1.00000 0.01872 0.03164 0.02390 -0.00561 0.00342 -0.00520 0.02545 0.00532 0.00025 0.00021 0.00016 0.00000 0.00136 0.00164 0.00154 0.00124 0.00119 0.00122 0.00062 C23 0.94706 0.25721 0.15965 1.00000 0.01859 0.02935 0.02548 -0.00073 0.00286 0.00400 0.02534 0.00522 0.00026 0.00021 0.00017 0.00000 0.00139 0.00160 0.00156 0.00123 0.00125 0.00121 0.00062 C24 0.82598 0.20820 0.12317 1.00000 0.02181 0.02582 0.01479 0.00028 0.00493 0.00079 0.02096 0.00487 0.00023 0.00020 0.00015 0.00000 0.00130 0.00149 0.00133 0.00113 0.00110 0.00114 0.00057 C25 0.71103 0.26755 0.09268 1.00000 0.01776 0.03202 0.02353 -0.00310 0.00357 -0.00237 0.02505 0.00535 0.00025 0.00022 0.00016 0.00000 0.00138 0.00169 0.00156 0.00121 0.00123 0.00120 0.00063 C26 0.71689 0.37322 0.10050 1.00000 0.02092 0.03201 0.02613 -0.00156 0.00234 0.00518 0.02744 0.00536 0.00026 0.00022 0.00017 0.00000 0.00140 0.00169 0.00161 0.00127 0.00124 0.00126 0.00064 C27 0.79836 0.04077 -0.03194 1.00000 0.01728 0.02319 0.02573 -0.00026 0.00031 0.00038 0.02347 0.00491 0.00023 0.00020 0.00016 0.00000 0.00131 0.00147 0.00160 0.00117 0.00121 0.00107 0.00060 C28 0.76260 0.02676 -0.16958 1.00000 0.02949 0.03533 0.02236 -0.00247 0.00071 0.00331 0.03067 0.00544 0.00027 0.00023 0.00018 0.00000 0.00157 0.00176 0.00165 0.00132 0.00133 0.00130 0.00068 C29 0.64543 0.06565 -0.17146 1.00000 0.02974 0.05241 0.02089 -0.00725 -0.00464 0.01099 0.03712 0.00601 0.00030 0.00025 0.00018 0.00000 0.00160 0.00203 0.00166 0.00143 0.00135 0.00148 0.00075 H10 0.50051 0.89010 -0.38616 1.00000 0.05438 0.06240 0.00319 0.00258 0.00200 0.00000 0.00988 H11 0.57958 0.81520 -0.42300 1.00000 0.03940 0.06010 0.00276 0.00241 0.00193 0.00000 0.00943 H12 0.68531 0.66119 -0.35703 1.00000 0.02244 0.04949 0.00235 0.00188 0.00162 0.00000 0.00666 H13 0.73945 0.55901 -0.24138 1.00000 0.01858 0.04629 0.00228 0.00193 0.00147 0.00000 0.00650 H15 0.56572 0.76334 -0.13326 1.00000 0.01792 0.04837 0.00227 0.00181 0.00160 0.00000 0.00666 H16 0.50734 0.86691 -0.24906 1.00000 0.02885 0.05084 0.00247 0.00218 0.00157 0.00000 0.00732 H17 1.08311 0.57767 0.05201 1.00000 0.02920 0.05389 0.00266 0.00218 0.00170 0.00000 0.00830 H18 1.17373 0.70016 0.14462 1.00000 0.03761 0.06007 0.00288 0.00224 0.00178 0.00000 0.00794 H19 1.00754 0.83672 0.14240 1.00000 0.02622 0.05434 0.00241 0.00213 0.00165 0.00000 0.00728 H20 0.76391 0.56584 0.13596 1.00000 0.02964 0.05458 0.00279 0.00211 0.00170 0.00000 0.00764 H21 0.91912 0.55500 0.18181 1.00000 0.03890 0.06386 0.00298 0.00222 0.00191 0.00000 0.00905 H22 1.03346 0.39731 0.19479 1.00000 0.02945 0.05534 0.00259 0.00203 0.00167 0.00000 0.00737 H23 1.02209 0.21668 0.17837 1.00000 0.02896 0.05207 0.00259 0.00210 0.00161 0.00000 0.00733 H25 0.62871 0.23467 0.07000 1.00000 0.03461 0.05981 0.00284 0.00213 0.00176 0.00000 0.00778 H26 0.63973 0.41562 0.08123 1.00000 0.03205 0.05397 0.00269 0.00209 0.00170 0.00000 0.00761 H27 0.92875 -0.01117 -0.07999 1.00000 0.04270 0.05927 0.00300 0.00230 0.00182 0.00000 0.00891 H28 0.79313 0.00633 -0.21266 1.00000 0.02919 0.05246 0.00253 0.00201 0.00169 0.00000 0.00748 H29 0.56943 0.07940 -0.21605 1.00000 0.06710 0.07255 0.00339 0.00259 0.00234 0.00000 0.01095 Final Structure Factor Calculation for 00ale002 in P 21/c stz form I Total number of l.s. parameters = 361 Maximum vector length = 511 Memory required = 3423 / 24017 wR2 = 0.1016 before cycle 6 for 3938 data and 0 / 361 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0521 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0400 for 2890 Fo > 4sig(Fo) and 0.0646 for all 3938 data wR2 = 0.1016, GooF = S = 1.032, Restrained GooF = 1.032 for all data Occupancy sum of asymmetric unit = 32.00 for non-hydrogen and 18.00 for hydrogen atoms Principal mean square atomic displacements U 0.0323 0.0215 0.0160 S11 0.0355 0.0306 0.0239 S12 0.0293 0.0252 0.0186 S21 0.0683 0.0292 0.0161 S22 0.0473 0.0253 0.0212 O11 0.0513 0.0265 0.0183 O12 0.0477 0.0380 0.0155 O21 0.0376 0.0349 0.0220 O22 0.0412 0.0301 0.0219 N11 0.0284 0.0232 0.0134 N12 0.0339 0.0264 0.0180 N13 0.0383 0.0265 0.0237 N21 0.0322 0.0249 0.0159 N22 0.0328 0.0263 0.0163 N23 0.0307 0.0214 0.0182 C11 0.0314 0.0204 0.0154 C12 0.0249 0.0232 0.0150 C13 0.0285 0.0217 0.0123 C14 0.0346 0.0254 0.0167 C15 0.0333 0.0255 0.0217 C16 0.0270 0.0221 0.0155 C17 0.0451 0.0363 0.0165 C18 0.0430 0.0397 0.0183 C19 0.0268 0.0253 0.0151 C21 0.0347 0.0261 0.0155 C22 0.0326 0.0266 0.0168 C23 0.0260 0.0221 0.0148 C24 0.0330 0.0254 0.0167 C25 0.0370 0.0272 0.0181 C26 0.0318 0.0232 0.0154 C27 0.0412 0.0313 0.0195 C28 0.0644 0.0319 0.0151 C29 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.024 0.037 0.051 0.067 0.085 0.108 0.140 0.202 1.000 Number in group 416. 406. 376. 392. 398. 382. 391. 387. 396. 394. GooF 0.813 0.974 1.014 1.080 1.113 1.186 0.959 0.996 0.990 1.154 K 1.290 1.018 0.940 0.987 0.972 0.983 0.995 1.000 1.014 0.985 Resolution(A) 0.84 0.87 0.90 0.95 1.00 1.06 1.14 1.26 1.43 1.81 inf Number in group 413. 375. 394. 398. 398. 388. 398. 393. 389. 392. GooF 0.865 0.908 0.945 0.907 0.997 0.954 0.843 0.972 1.191 1.547 K 0.981 0.982 0.987 1.007 1.015 1.021 1.021 1.026 1.027 0.952 R1 0.165 0.134 0.115 0.084 0.072 0.049 0.037 0.036 0.036 0.040 Recommended weighting scheme: WGHT 0.0521 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) 0 2 0 4457.14 7196.33 5.79 0.364 6.47 -3 1 3 173.70 251.00 5.76 0.068 3.24 -1 5 1 2766.65 3636.81 4.43 0.258 2.51 0 3 6 160.35 102.01 4.40 0.043 2.31 -2 2 9 817.27 629.54 3.97 0.108 1.83 -4 0 2 112.92 159.98 3.90 0.054 2.63 0 6 0 12660.33 16413.56 3.87 0.549 2.16 -3 1 5 597.52 761.02 3.84 0.118 2.74 -5 1 7 236.08 310.80 3.79 0.076 1.80 -10 5 11 -2.65 61.75 3.73 0.034 0.92 -1 3 1 2136.86 2776.31 3.73 0.226 3.96 -1 4 1 38117.43 47579.78 3.71 0.935 3.08 -1 5 6 1088.15 874.34 3.62 0.127 1.92 -4 2 2 152.40 193.55 3.54 0.060 2.44 -6 12 4 8.39 57.71 3.52 0.033 0.92 -3 1 10 508.11 382.52 3.42 0.084 1.67 -2 9 5 22.95 6.54 3.39 0.011 1.31 1 5 5 400.74 307.34 3.37 0.075 1.92 -1 2 5 505.20 406.75 3.36 0.086 3.04 -5 5 5 415.74 511.61 3.34 0.097 1.58 4 1 1 2738.57 2279.52 3.33 0.205 2.33 2 4 7 154.47 210.77 3.30 0.062 1.64 3 3 1 1498.68 1235.07 3.28 0.151 2.51 1 1 2 15.38 5.87 3.27 0.010 5.11 -4 3 2 140.83 180.08 3.18 0.058 2.25 3 5 3 14.54 0.24 3.17 0.002 1.81 2 1 5 1085.84 867.41 3.17 0.126 2.38 5 4 1 1534.25 1881.58 3.14 0.186 1.65 -7 4 17 14.87 78.85 3.13 0.038 0.91 0 4 0 2829.24 3484.85 3.13 0.253 3.23 -10 6 11 88.48 28.04 3.10 0.023 0.89 0 4 8 290.30 227.36 3.10 0.065 1.73 4 5 15 110.83 327.63 3.05 0.078 0.85 0 4 1 221.60 287.41 3.00 0.073 3.17 2 8 2 68.81 139.59 2.99 0.051 1.49 -6 0 4 165.19 114.75 2.95 0.046 1.75 -1 5 8 2581.53 2181.84 2.92 0.200 1.65 -4 1 6 279.01 334.53 2.91 0.078 2.18 -5 1 8 277.26 227.87 2.90 0.065 1.70 7 5 1 414.87 524.42 2.87 0.098 1.23 -5 7 12 254.07 366.92 2.84 0.082 1.08 7 7 0 114.94 190.13 2.84 0.059 1.13 -4 1 4 186.16 226.25 2.81 0.064 2.46 -6 9 10 3478.91 2882.99 2.79 0.230 1.00 4 3 2 74.02 116.46 2.79 0.046 1.97 8 1 3 47.13 91.91 2.78 0.041 1.14 1 0 6 -2.61 26.17 2.78 0.022 2.45 9 5 0 136.59 229.32 2.77 0.065 1.02 -1 12 5 138.91 65.11 2.77 0.035 1.03 5 8 10 45.02 158.53 2.77 0.054 0.92 Bond lengths and angles S11 - Distance Angles O12 1.4417 (0.0019) O11 1.4427 (0.0019) 117.42 (0.11) N12 1.6092 (0.0020) 112.33 (0.11) 103.86 (0.11) C14 1.7519 (0.0025) 107.19 (0.12) 107.36 (0.12) 108.32 (0.11) S11 - O12 O11 N12 S12 - Distance Angles C19 1.7367 (0.0031) C17 1.7376 (0.0026) 90.85 (0.13) S12 - C19 S21 - Distance Angles O22 1.4417 (0.0018) O21 1.4489 (0.0019) 118.12 (0.12) N22 1.6134 (0.0022) 111.02 (0.11) 103.55 (0.11) C24 1.7457 (0.0027) 107.83 (0.11) 107.64 (0.12) 108.27 (0.11) S21 - O22 O21 N22 S22 - Distance Angles C27 1.7365 (0.0025) C29 1.7369 (0.0030) 90.58 (0.14) S22 - C27 O11 - Distance Angles S11 1.4427 (0.0019) O11 - O12 - Distance Angles S11 1.4417 (0.0019) O12 - O21 - Distance Angles S21 1.4489 (0.0019) O21 - O22 - Distance Angles S21 1.4417 (0.0018) O22 - N11 - Distance Angles C11 1.3774 (0.0034) H10 0.9520 (0.0335) 115.70 (1.93) H11 0.8419 (0.0306) 115.28 (2.15) 117.51 (2.90) N11 - C11 H10 N12 - Distance Angles C17 1.3260 (0.0033) S11 1.6092 (0.0020) 121.28 (0.18) N12 - C17 N13 - Distance Angles C17 1.3417 (0.0032) C18 1.3819 (0.0035) 115.28 (0.24) H17 0.8484 (0.0276) 122.25 (1.89) 121.18 (1.92) N13 - C17 C18 N21 - Distance Angles C21 1.3647 (0.0034) H20 0.9383 (0.0279) 118.82 (1.68) H21 0.8824 (0.0310) 118.54 (1.89) 121.64 (2.56) N21 - C21 H20 N22 - Distance Angles C27 1.3361 (0.0032) S21 1.6134 (0.0022) 120.65 (0.18) N22 - C27 N23 - Distance Angles C27 1.3289 (0.0032) C28 1.3782 (0.0035) 115.28 (0.23) H27 0.8776 (0.0293) 120.31 (1.97) 124.24 (1.97) N23 - C27 C28 C11 - Distance Angles N11 1.3774 (0.0034) C12 1.3878 (0.0036) 121.62 (0.24) C16 1.4028 (0.0036) 119.88 (0.26) 118.48 (0.24) C11 - N11 C12 C12 - Distance Angles C13 1.3800 (0.0036) C11 1.3878 (0.0036) 121.04 (0.24) H12 0.9373 (0.0258) 118.84 (1.53) 120.06 (1.53) C12 - C13 C11 C13 - Distance Angles C12 1.3800 (0.0036) C14 1.3872 (0.0035) 119.73 (0.25) H13 0.9463 (0.0244) 120.26 (1.48) 120.01 (1.49) C13 - C12 C14 C14 - Distance Angles C15 1.3847 (0.0035) C13 1.3872 (0.0035) 119.76 (0.24) S11 1.7519 (0.0025) 120.99 (0.19) 119.14 (0.20) C14 - C15 C13 C15 - Distance Angles C16 1.3693 (0.0037) C14 1.3847 (0.0035) 120.52 (0.25) H15 0.8988 (0.0243) 121.01 (1.58) 118.33 (1.57) C15 - C16 C14 C16 - Distance Angles C15 1.3693 (0.0037) C11 1.4028 (0.0036) 120.44 (0.26) H16 0.9427 (0.0269) 121.22 (1.57) 118.21 (1.57) C16 - C15 C11 C17 - Distance Angles N12 1.3260 (0.0033) N13 1.3417 (0.0032) 120.63 (0.22) S12 1.7376 (0.0026) 130.15 (0.19) 109.21 (0.19) C17 - N12 N13 C18 - Distance Angles C19 1.3201 (0.0041) N13 1.3819 (0.0035) 113.16 (0.27) H18 0.9288 (0.0293) 129.99 (1.81) 116.72 (1.82) C18 - C19 N13 C19 - Distance Angles C18 1.3201 (0.0041) S12 1.7367 (0.0031) 111.38 (0.23) H19 0.9061 (0.0272) 128.34 (1.66) 120.23 (1.63) C19 - C18 S12 C21 - Distance Angles N21 1.3647 (0.0034) C26 1.4004 (0.0037) 121.52 (0.25) C22 1.4033 (0.0036) 120.61 (0.25) 117.87 (0.26) C21 - N21 C26 C22 - Distance Angles C23 1.3645 (0.0037) C21 1.4033 (0.0036) 121.29 (0.25) H22 0.9523 (0.0268) 121.91 (1.59) 116.79 (1.58) C22 - C23 C21 C23 - Distance Angles C22 1.3645 (0.0037) C24 1.3906 (0.0035) 120.26 (0.25) H23 0.9209 (0.0268) 121.74 (1.68) 117.99 (1.68) C23 - C22 C24 C24 - Distance Angles C23 1.3906 (0.0035) C25 1.3939 (0.0036) 119.37 (0.26) S21 1.7457 (0.0027) 120.11 (0.20) 120.49 (0.20) C24 - C23 C25 C25 - Distance Angles C26 1.3731 (0.0038) C24 1.3939 (0.0036) 120.23 (0.25) H25 0.9373 (0.0288) 120.05 (1.69) 119.59 (1.70) C25 - C26 C24 C26 - Distance Angles C25 1.3731 (0.0038) C21 1.4004 (0.0037) 120.91 (0.25) H26 0.9523 (0.0273) 122.09 (1.66) 116.97 (1.67) C26 - C25 C21 C27 - Distance Angles N23 1.3289 (0.0032) N22 1.3361 (0.0032) 120.33 (0.22) S22 1.7365 (0.0025) 109.70 (0.19) 129.97 (0.21) C27 - N23 N22 C28 - Distance Angles C29 1.3241 (0.0039) N23 1.3782 (0.0035) 113.24 (0.27) H28 0.9313 (0.0265) 129.34 (1.65) 117.36 (1.65) C28 - C29 N23 C29 - Distance Angles C28 1.3241 (0.0039) S22 1.7369 (0.0030) 111.07 (0.23) H29 0.9411 (0.0369) 130.29 (2.09) 118.46 (2.07) C29 - C28 S22 Selected torsion angles -33.32 ( 0.24) O12 - S11 - N12 - C17 -161.20 ( 0.20) O11 - S11 - N12 - C17 84.88 ( 0.22) C14 - S11 - N12 - C17 39.29 ( 0.24) O22 - S21 - N22 - C27 167.02 ( 0.20) O21 - S21 - N22 - C27 -78.90 ( 0.23) C24 - S21 - N22 - C27 177.33 ( 0.23) N11 - C11 - C12 - C13 -1.03 ( 0.37) C16 - C11 - C12 - C13 -0.57 ( 0.37) C11 - C12 - C13 - C14 1.05 ( 0.36) C12 - C13 - C14 - C15 177.32 ( 0.19) C12 - C13 - C14 - S11 9.04 ( 0.24) O12 - S11 - C14 - C15 136.03 ( 0.21) O11 - S11 - C14 - C15 -112.38 ( 0.21) N12 - S11 - C14 - C15 -167.18 ( 0.19) O12 - S11 - C14 - C13 -40.19 ( 0.22) O11 - S11 - C14 - C13 71.40 ( 0.22) N12 - S11 - C14 - C13 0.10 ( 0.38) C13 - C14 - C15 - C16 -176.10 ( 0.20) S11 - C14 - C15 - C16 -1.73 ( 0.40) C14 - C15 - C16 - C11 -176.21 ( 0.25) N11 - C11 - C16 - C15 2.18 ( 0.38) C12 - C11 - C16 - C15 171.72 ( 0.18) S11 - N12 - C17 - N13 -8.46 ( 0.34) S11 - N12 - C17 - S12 -176.39 ( 0.23) C18 - N13 - C17 - N12 3.76 ( 0.28) C18 - N13 - C17 - S12 177.29 ( 0.25) C19 - S12 - C17 - N12 -2.88 ( 0.20) C19 - S12 - C17 - N13 -2.81 ( 0.36) C17 - N13 - C18 - C19 0.41 ( 0.33) N13 - C18 - C19 - S12 1.42 ( 0.24) C17 - S12 - C19 - C18 177.67 ( 0.24) N21 - C21 - C22 - C23 -1.31 ( 0.38) C26 - C21 - C22 - C23 -1.09 ( 0.40) C21 - C22 - C23 - C24 2.58 ( 0.37) C22 - C23 - C24 - C25 -175.53 ( 0.21) C22 - C23 - C24 - S21 162.10 ( 0.20) O22 - S21 - C24 - C23 33.65 ( 0.23) O21 - S21 - C24 - C23 -77.70 ( 0.22) N22 - S21 - C24 - C23 -15.99 ( 0.23) O22 - S21 - C24 - C25 -144.44 ( 0.20) O21 - S21 - C24 - C25 104.21 ( 0.21) N22 - S21 - C24 - C25 -1.65 ( 0.37) C23 - C24 - C25 - C26 176.45 ( 0.20) S21 - C24 - C25 - C26 -0.78 ( 0.39) C24 - C25 - C26 - C21 -176.73 ( 0.24) N21 - C21 - C26 - C25 2.24 ( 0.37) C22 - C21 - C26 - C25 -175.72 ( 0.24) C28 - N23 - C27 - N22 3.78 ( 0.29) C28 - N23 - C27 - S22 178.61 ( 0.19) S21 - N22 - C27 - N23 -0.78 ( 0.36) S21 - N22 - C27 - S22 -3.51 ( 0.21) C29 - S22 - C27 - N23 175.93 ( 0.27) C29 - S22 - C27 - N22 -1.95 ( 0.37) C27 - N23 - C28 - C29 -0.89 ( 0.35) N23 - C28 - C29 - S22 2.51 ( 0.26) C27 - S22 - C29 - C28 FMAP and GRID set by program FMAP 2 3 22 GRID -1.316 -2 -2 1.316 2 2 R1 = 0.0642 for 3938 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.32 at 0.4485 0.1376 0.0300 [ 2.20 A from H25 ] Deepest hole -0.47 at 0.7698 0.0783 0.0608 [ 0.97 A from S21 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 3353 / 21953 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4485 0.1376 0.0300 1.00000 0.05 0.32 2.20 H25 2.23 H15 2.67 O22 2.89 H12 Q2 1 0.6356 0.6785 -0.0281 1.00000 0.05 0.23 0.88 O12 1.94 S11 2.05 H15 2.07 H11 Q3 1 0.9376 -0.0683 0.1831 1.00000 0.05 0.22 1.36 O21 1.69 H19 2.07 H22 2.31 S21 Q4 1 0.5669 0.8801 -0.2389 1.00000 0.05 0.22 0.62 H16 0.95 C16 1.94 C11 2.01 C15 Q5 1 0.6688 0.6168 -0.3815 1.00000 0.05 0.22 0.70 H12 1.51 C12 2.11 O22 2.32 C13 Shortest distances between peaks (including symmetry equivalents) 1 5 2.49 1 2 2.53 3 5 2.78 Time profile in seconds ----------------------- 0.30: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.02: 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. 1.56: 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 0.02: Generate idealized H-atoms 1.33: Structure factors and derivatives 4.22: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.59: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 00ale002 finished at 12:03:00 Total CPU time: 8.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++