+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 03src359 started at 18:04:02 on 17-Sep-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 03src0359 in P2(1)/n CELL 0.71073 10.9384 8.2970 17.3097 90.000 96.667 90.000 ZERR 4.00 0.0003 0.0002 0.0005 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 72 64 8 24 V = 1560.33 F(000) = 744.0 Mu = 0.12 mm-1 Cell Wt = 1425.31 Rho = 1.517 MERG 2 OMIT -3.00 55.00 OMIT 0 6 9 OMIT 3 6 3 OMIT 0 6 6 EXTI 0.01412 FMAP 2 PLAN 10 SIZE 0.01 0.20 0.30 BOND $H CONF WGHT 0.05690 0.93410 L.S. 4 TEMP -153.00 FVAR 0.45636 MOLE 1 C1 1 0.825947 0.737630 0.070076 11.00000 0.01556 0.01930 = 0.01777 -0.00122 0.00323 -0.00045 C2 1 0.719268 0.818797 0.040216 11.00000 0.01729 0.02060 = 0.01787 -0.00340 0.00350 -0.00183 C3 1 0.710941 0.909343 -0.035659 11.00000 0.01869 0.02285 = 0.01797 -0.00260 0.00096 0.00158 C4 1 0.818384 0.914961 -0.075109 11.00000 0.01950 0.02646 = 0.01626 0.00174 0.00305 0.00036 AFIX 43 H4 2 0.817149 0.972509 -0.122640 11.00000 -1.20000 AFIX 0 C5 1 0.921387 0.838603 -0.044846 11.00000 0.01666 0.02279 = 0.01588 -0.00207 0.00464 -0.00132 C6 1 0.934073 0.746578 0.028485 11.00000 0.01623 0.01889 = 0.01586 -0.00285 0.00303 -0.00080 C7 1 1.139106 0.697302 0.013561 11.00000 0.01657 0.01942 = 0.01743 -0.00243 0.00598 -0.00186 C8 1 1.254477 0.630417 0.041199 11.00000 0.01700 0.01932 = 0.02049 -0.00262 0.00466 -0.00032 C9 1 1.352028 0.641570 -0.003531 11.00000 0.01690 0.02407 = 0.02543 -0.00162 0.00491 0.00117 AFIX 43 H9 2 1.428842 0.593365 0.014506 11.00000 -1.20000 AFIX 0 C10 1 1.338106 0.722841 -0.074585 11.00000 0.01957 0.02916 = 0.02493 -0.00335 0.01014 -0.00157 AFIX 43 H10 2 1.405749 0.730481 -0.104208 11.00000 -1.20000 AFIX 0 C11 1 1.226526 0.792435 -0.102271 11.00000 0.02130 0.02739 = 0.01608 -0.00125 0.00617 -0.00312 AFIX 43 H11 2 1.216484 0.848621 -0.150410 11.00000 -1.20000 AFIX 0 C12 1 1.129969 0.777549 -0.057549 11.00000 0.01502 0.02120 = 0.01915 -0.00210 0.00201 0.00005 C13 1 0.823201 0.649569 0.144209 11.00000 0.01599 0.02196 = 0.01870 -0.00131 0.00357 -0.00152 C14 1 0.919304 0.477566 0.240945 11.00000 0.02084 0.02828 = 0.01610 0.00410 0.00540 -0.00264 AFIX 23 H14A 2 0.848713 0.402588 0.239818 11.00000 -1.20000 H14B 2 0.913062 0.558321 0.282409 11.00000 -1.20000 AFIX 0 C15 1 1.039145 0.386727 0.255343 11.00000 0.02616 0.02737 = 0.01753 0.00182 0.00384 0.00401 AFIX 137 H15A 2 1.043227 0.306117 0.214341 11.00000 -1.50000 H15B 2 1.044133 0.332761 0.305972 11.00000 -1.50000 H15C 2 1.107978 0.462252 0.255075 11.00000 -1.50000 AFIX 0 C16 1 1.276856 0.558129 0.120696 11.00000 0.01344 0.02270 = 0.02248 -0.00034 0.00373 -0.00019 C17 1 1.373610 0.342357 0.195429 11.00000 0.02732 0.02629 = 0.02245 0.00595 0.00378 0.00427 AFIX 23 H17A 2 1.394921 0.228526 0.186262 11.00000 -1.20000 H17B 2 1.299512 0.343290 0.223278 11.00000 -1.20000 AFIX 0 C18 1 1.478150 0.420684 0.245446 11.00000 0.03281 0.03313 = 0.02412 -0.00187 0.00068 0.00783 AFIX 137 H18A 2 1.552297 0.417662 0.218677 11.00000 -1.50000 H18B 2 1.493508 0.362623 0.294925 11.00000 -1.50000 H18C 2 1.456950 0.532943 0.255417 11.00000 -1.50000 AFIX 0 N1 3 1.039251 0.680585 0.055565 11.00000 0.01539 0.02283 = 0.01757 -0.00020 0.00429 -0.00030 N2 3 0.615715 0.825409 0.073217 11.00000 0.01466 0.03279 = 0.02385 0.00239 0.00480 0.00395 O1 4 1.020225 0.848017 -0.085814 11.00000 0.01620 0.02952 = 0.01683 0.00319 0.00506 0.00144 O2 4 0.612505 0.974432 -0.060481 11.00000 0.01915 0.03585 = 0.02421 0.00284 0.00242 0.00787 O3 4 0.737239 0.660331 0.184100 11.00000 0.01932 0.03800 = 0.02335 0.00501 0.00994 0.00515 O4 4 0.920049 0.556625 0.165804 11.00000 0.01828 0.02608 = 0.01752 0.00472 0.00608 0.00299 O5 4 1.241937 0.616488 0.178319 11.00000 0.02125 0.03437 = 0.02091 -0.00078 0.00566 0.00502 O6 4 1.345455 0.423824 0.120518 11.00000 0.02198 0.02476 = 0.02015 0.00097 0.00275 0.00452 H1N 2 0.613109 0.774590 0.120578 11.00000 0.03239 H2N 2 0.553098 0.886049 0.051686 11.00000 0.02844 HKLF 4 Covalent radii and connectivity table for 03src0359 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 C1 - C2 C6 C13 C2 - N2 C1 C3 C3 - O2 C4 C2 C4 - C5 C3 C5 - C4 O1 C6 C6 - N1 C1 C5 C7 - N1 C12 C8 C8 - C9 C7 C16 C9 - C8 C10 C10 - C11 C9 C11 - C10 C12 C12 - O1 C11 C7 C13 - O3 O4 C1 C14 - O4 C15 C15 - C14 C16 - O5 O6 C8 C17 - O6 C18 C18 - C17 N1 - C6 C7 N2 - C2 O1 - C5 C12 O2 - C3 O3 - C13 O4 - C13 C14 O5 - C16 O6 - C16 C17 h k l Fo^2 Sigma Why rejected 7 0 0 4.91 0.98 observed but should be systematically absent 15091 Reflections read, of which 452 rejected -14 =< h =< 14, -10 =< k =< 10, -22 =< l =< 22, Max. 2-theta = 54.93 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 1 0 69.94 1.31 5 20.77 -1 1 1 56.39 1.15 6 15.32 8 2 6 22.92 0.95 4 10.95 9 2 6 131.06 6.30 4 44.28 9 3 9 12.97 0.98 2 29.95 4 2 11 30.71 1.00 3 18.07 4 2 12 32.63 1.03 3 31.13 5 3 14 23.59 1.00 3 17.95 8 Inconsistent equivalents 3551 Unique reflections, of which 0 suppressed R(int) = 0.0791 R(sigma) = 0.0651 Friedel opposites merged Maximum memory for data reduction = 2576 / 35498 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 = 3221 / 305280 wR2 = 0.1396 before cycle 1 for 3551 data and 246 / 246 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0569 * P )^2 + 0.93 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45601 0.00132 -0.262 OSF 2 0.01398 0.00238 -0.060 EXTI Mean shift/esd = 0.073 Maximum = -0.357 for U22 N2 Max. shift = 0.004 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 3221 / 305280 wR2 = 0.1395 before cycle 2 for 3551 data and 246 / 246 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0569 * P )^2 + 0.93 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45591 0.00132 -0.074 OSF 2 0.01392 0.00237 -0.024 EXTI Mean shift/esd = 0.026 Maximum = -0.130 for U22 N2 Max. shift = 0.001 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 3 Maximum vector length = 511 Memory required = 3221 / 305280 wR2 = 0.1395 before cycle 3 for 3551 data and 246 / 246 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0569 * P )^2 + 0.93 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45592 0.00132 0.000 OSF 2 0.01392 0.00237 -0.001 EXTI Mean shift/esd = 0.001 Maximum = 0.008 for U22 C12 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 3221 / 305280 wR2 = 0.1395 before cycle 4 for 3551 data and 246 / 246 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0569 * P )^2 + 0.93 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45592 0.00132 0.000 OSF 2 0.01392 0.00237 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for U33 C7 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Largest correlation matrix elements 0.525 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H4 0.8172 0.9726 -0.1226 43 0.950 0.000 C4 C5 C3 H9 1.4288 0.5934 0.0145 43 0.950 0.000 C9 C8 C10 H10 1.4057 0.7303 -0.1042 43 0.950 0.000 C10 C11 C9 H11 1.2165 0.8487 -0.1504 43 0.950 0.000 C11 C10 C12 H14A 0.8487 0.4026 0.2398 23 0.990 0.000 C14 O4 C15 H14B 0.9131 0.5583 0.2824 23 0.990 0.000 C14 O4 C15 H15A 1.0432 0.3061 0.2143 137 0.980 0.000 C15 C14 H15A H15B 1.0441 0.3327 0.3060 137 0.980 0.000 C15 C14 H15A H15C 1.1080 0.4622 0.2551 137 0.980 0.000 C15 C14 H15A H17A 1.3949 0.2286 0.1863 23 0.990 0.000 C17 O6 C18 H17B 1.2995 0.3434 0.2233 23 0.990 0.000 C17 O6 C18 H18A 1.5523 0.4178 0.2187 137 0.980 0.000 C18 C17 H18A H18B 1.4936 0.3626 0.2949 137 0.980 0.000 C18 C17 H18A H18C 1.4569 0.5330 0.2554 137 0.980 0.000 C18 C17 H18A 03src0359 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.82593 0.73758 0.07007 1.00000 0.01540 0.01937 0.01772 -0.00131 0.00324 -0.00052 0.01739 0.00303 0.00015 0.00021 0.00010 0.00000 0.00084 0.00091 0.00083 0.00068 0.00070 0.00067 0.00038 C2 0.71927 0.81877 0.04022 1.00000 0.01716 0.02059 0.01780 -0.00332 0.00347 -0.00187 0.01840 0.00312 0.00016 0.00022 0.00010 0.00000 0.00084 0.00092 0.00084 0.00068 0.00070 0.00067 0.00038 C3 0.71094 0.90931 -0.03564 1.00000 0.01863 0.02292 0.01783 -0.00261 0.00099 0.00161 0.01988 0.00318 0.00016 0.00023 0.00010 0.00000 0.00086 0.00094 0.00084 0.00070 0.00072 0.00070 0.00039 C4 0.81840 0.91498 -0.07510 1.00000 0.01934 0.02670 0.01622 0.00170 0.00305 0.00035 0.02067 0.00325 0.00016 0.00023 0.00010 0.00000 0.00088 0.00100 0.00082 0.00072 0.00071 0.00073 0.00040 H4 0.81717 0.97258 -0.12261 1.00000 0.02481 0.00000 0.00000 C5 0.92138 0.83861 -0.04485 1.00000 0.01653 0.02289 0.01578 -0.00198 0.00468 -0.00130 0.01818 0.00311 0.00016 0.00022 0.00010 0.00000 0.00084 0.00094 0.00082 0.00068 0.00070 0.00068 0.00038 C6 0.93406 0.74660 0.02846 1.00000 0.01615 0.01892 0.01578 -0.00289 0.00306 -0.00083 0.01686 0.00299 0.00015 0.00021 0.00010 0.00000 0.00082 0.00090 0.00082 0.00066 0.00068 0.00066 0.00037 C7 1.13911 0.69740 0.01355 1.00000 0.01640 0.01962 0.01734 -0.00249 0.00596 -0.00184 0.01747 0.00308 0.00016 0.00021 0.00010 0.00000 0.00084 0.00090 0.00083 0.00066 0.00070 0.00066 0.00038 C8 1.25447 0.63044 0.04120 1.00000 0.01695 0.01912 0.02034 -0.00240 0.00463 -0.00022 0.01861 0.00316 0.00016 0.00021 0.00010 0.00000 0.00083 0.00092 0.00087 0.00068 0.00072 0.00066 0.00039 C9 1.35203 0.64156 -0.00353 1.00000 0.01671 0.02408 0.02537 -0.00171 0.00484 0.00112 0.02186 0.00332 0.00017 0.00022 0.00011 0.00000 0.00084 0.00100 0.00095 0.00073 0.00075 0.00069 0.00041 H9 1.42885 0.59338 0.01452 1.00000 0.02624 0.00000 0.00000 C10 1.33809 0.72278 -0.07458 1.00000 0.01940 0.02938 0.02487 -0.00340 0.01014 -0.00163 0.02396 0.00346 0.00017 0.00024 0.00011 0.00000 0.00089 0.00104 0.00093 0.00079 0.00076 0.00076 0.00041 H10 1.40572 0.73034 -0.10422 1.00000 0.02875 0.00000 0.00000 C11 1.22654 0.79245 -0.10227 1.00000 0.02127 0.02726 0.01601 -0.00120 0.00616 -0.00317 0.02120 0.00326 0.00017 0.00023 0.00010 0.00000 0.00089 0.00100 0.00082 0.00072 0.00073 0.00074 0.00040 H11 1.21652 0.84867 -0.15040 1.00000 0.02544 0.00000 0.00000 C12 1.12997 0.77759 -0.05755 1.00000 0.01488 0.02131 0.01905 -0.00233 0.00201 -0.00002 0.01841 0.00310 0.00016 0.00022 0.00010 0.00000 0.00081 0.00094 0.00087 0.00069 0.00069 0.00068 0.00038 C13 0.82321 0.64955 0.14420 1.00000 0.01593 0.02185 0.01860 -0.00128 0.00350 -0.00146 0.01868 0.00315 0.00016 0.00021 0.00010 0.00000 0.00083 0.00093 0.00085 0.00069 0.00070 0.00067 0.00038 C14 0.91931 0.47754 0.24095 1.00000 0.02081 0.02816 0.01595 0.00413 0.00541 -0.00262 0.02138 0.00338 0.00016 0.00023 0.00010 0.00000 0.00089 0.00102 0.00083 0.00072 0.00072 0.00074 0.00040 H14A 0.84871 0.40257 0.23981 1.00000 0.02566 0.00000 0.00000 H14B 0.91307 0.55827 0.28243 1.00000 0.02566 0.00000 0.00000 C15 1.03915 0.38667 0.25535 1.00000 0.02595 0.02773 0.01745 0.00177 0.00385 0.00398 0.02361 0.00353 0.00017 0.00024 0.00010 0.00000 0.00096 0.00104 0.00085 0.00073 0.00076 0.00077 0.00042 H15A 1.04323 0.30608 0.21434 1.00000 0.03541 0.00000 0.00000 H15B 1.04412 0.33268 0.30597 1.00000 0.03541 0.00000 0.00000 H15C 1.10799 0.46219 0.25509 1.00000 0.03541 0.00000 0.00000 C16 1.27686 0.55810 0.12069 1.00000 0.01333 0.02280 0.02237 -0.00003 0.00371 -0.00011 0.01937 0.00320 0.00015 0.00022 0.00010 0.00000 0.00078 0.00096 0.00090 0.00071 0.00070 0.00067 0.00039 C17 1.37363 0.34241 0.19545 1.00000 0.02719 0.02641 0.02236 0.00591 0.00379 0.00425 0.02525 0.00363 0.00018 0.00024 0.00011 0.00000 0.00099 0.00104 0.00095 0.00077 0.00080 0.00078 0.00043 H17A 1.39493 0.22857 0.18629 1.00000 0.03030 0.00000 0.00000 H17B 1.29954 0.34337 0.22330 1.00000 0.03030 0.00000 0.00000 C18 1.47816 0.42073 0.24545 1.00000 0.03259 0.03361 0.02400 -0.00184 0.00068 0.00786 0.03027 0.00375 0.00019 0.00026 0.00012 0.00000 0.00107 0.00117 0.00098 0.00083 0.00086 0.00087 0.00047 H18A 1.55229 0.41775 0.21866 1.00000 0.04540 0.00000 0.00000 H18B 1.49355 0.36263 0.29492 1.00000 0.04540 0.00000 0.00000 H18C 1.45695 0.53297 0.25544 1.00000 0.04540 0.00000 0.00000 N1 1.03923 0.68058 0.05558 1.00000 0.01531 0.02274 0.01750 -0.00015 0.00434 -0.00024 0.01832 0.00264 0.00013 0.00018 0.00008 0.00000 0.00072 0.00080 0.00073 0.00060 0.00061 0.00058 0.00034 N2 0.61570 0.82545 0.07322 1.00000 0.01465 0.03232 0.02385 0.00240 0.00480 0.00394 0.02340 0.00301 0.00015 0.00021 0.00010 0.00000 0.00075 0.00096 0.00084 0.00071 0.00067 0.00066 0.00037 O1 1.02024 0.84797 -0.08581 1.00000 0.01615 0.02933 0.01678 0.00314 0.00509 0.00140 0.02050 0.00229 0.00011 0.00016 0.00007 0.00000 0.00062 0.00074 0.00061 0.00050 0.00050 0.00050 0.00031 O2 0.61251 0.97444 -0.06049 1.00000 0.01910 0.03581 0.02410 0.00283 0.00243 0.00793 0.02634 0.00250 0.00012 0.00017 0.00008 0.00000 0.00066 0.00082 0.00069 0.00057 0.00056 0.00056 0.00034 O3 0.73725 0.66032 0.18411 1.00000 0.01917 0.03822 0.02328 0.00513 0.00998 0.00522 0.02630 0.00256 0.00012 0.00017 0.00008 0.00000 0.00067 0.00083 0.00069 0.00057 0.00056 0.00055 0.00034 O4 0.92006 0.55666 0.16581 1.00000 0.01825 0.02592 0.01744 0.00474 0.00609 0.00307 0.02022 0.00229 0.00011 0.00015 0.00007 0.00000 0.00063 0.00070 0.00061 0.00050 0.00051 0.00050 0.00030 O5 1.24193 0.61644 0.17831 1.00000 0.02115 0.03438 0.02089 -0.00083 0.00567 0.00496 0.02522 0.00242 0.00012 0.00017 0.00007 0.00000 0.00066 0.00080 0.00067 0.00056 0.00056 0.00055 0.00033 O6 1.34546 0.42382 0.12053 1.00000 0.02192 0.02464 0.02011 0.00105 0.00275 0.00451 0.02220 0.00231 0.00012 0.00015 0.00007 0.00000 0.00065 0.00072 0.00065 0.00052 0.00053 0.00052 0.00031 H1N 0.61357 0.77446 0.12076 1.00000 0.03280 0.04219 0.00214 0.00285 0.00142 0.00000 0.00604 H2N 0.55298 0.88593 0.05158 1.00000 0.02866 0.04040 0.00211 0.00274 0.00130 0.00000 0.00578 Final Structure Factor Calculation for 03src0359 in P2(1)/n Total number of l.s. parameters = 246 Maximum vector length = 511 Memory required = 2975 / 22995 wR2 = 0.1395 before cycle 5 for 3551 data and 0 / 246 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0569 * P )^2 + 0.93 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0525 for 2748 Fo > 4sig(Fo) and 0.0716 for all 3551 data wR2 = 0.1395, GooF = S = 1.011, Restrained GooF = 1.011 for all data Occupancy sum of asymmetric unit = 26.00 for non-hydrogen and 16.00 for hydrogen atoms Principal mean square atomic displacements U 0.0203 0.0173 0.0146 C1 0.0234 0.0163 0.0154 C2 0.0248 0.0181 0.0167 C3 0.0270 0.0195 0.0156 C4 0.0238 0.0178 0.0129 C5 0.0209 0.0160 0.0137 C6 0.0230 0.0171 0.0123 C7 0.0227 0.0181 0.0150 C8 0.0266 0.0235 0.0154 C9 0.0329 0.0259 0.0131 C10 0.0290 0.0213 0.0133 C11 0.0228 0.0176 0.0149 C12 0.0227 0.0184 0.0150 C13 0.0299 0.0221 0.0122 C14 0.0311 0.0228 0.0170 C15 0.0228 0.0225 0.0128 C16 0.0329 0.0249 0.0180 C17 0.0420 0.0253 0.0235 C18 0.0228 0.0188 0.0134 N1 0.0338 0.0233 0.0131 N2 0.0303 0.0185 0.0128 O1 0.0392 0.0239 0.0159 O2 0.0417 0.0248 0.0124 O3 0.0294 0.0182 0.0130 O4 0.0360 0.0233 0.0163 O5 0.0280 0.0200 0.0186 O6 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.017 0.026 0.035 0.046 0.059 0.076 0.102 0.152 1.000 Number in group 372. 358. 381. 311. 372. 343. 351. 351. 354. 358. GooF 0.946 0.925 1.015 1.012 1.114 0.997 0.982 1.017 1.093 0.989 K 3.832 1.118 1.029 0.998 1.005 1.006 1.014 1.020 1.017 1.021 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.64 inf Number in group 356. 357. 352. 355. 356. 355. 357. 357. 349. 357. GooF 0.938 0.986 0.989 0.911 0.975 0.983 1.011 0.917 1.070 1.276 K 1.067 1.081 1.037 1.042 1.027 1.000 1.029 1.031 1.020 1.010 R1 0.159 0.166 0.122 0.102 0.087 0.063 0.051 0.043 0.050 0.041 Recommended weighting scheme: WGHT 0.0581 0.7744 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) 3 6 12 49.57 11.19 5.31 0.020 0.94 3 6 6 838.82 482.13 5.10 0.130 1.16 5 0 3 430.34 273.69 4.81 0.098 1.96 6 6 3 87.43 38.76 4.63 0.037 1.07 1 1 2 759.33 1006.08 4.02 0.188 5.06 -9 0 11 227.26 355.38 4.01 0.112 1.01 -5 0 5 107.97 51.17 4.00 0.042 1.94 3 6 9 539.43 368.37 3.97 0.114 1.05 0 3 9 399.33 248.46 3.95 0.094 1.57 -6 0 6 257.65 112.37 3.69 0.063 1.62 -7 0 17 34.02 79.78 3.62 0.053 0.90 8 6 8 21.58 59.58 3.59 0.046 0.86 -7 0 9 101.22 59.18 3.53 0.046 1.28 -2 3 16 10.78 33.36 3.44 0.034 1.00 0 3 21 43.28 16.47 3.43 0.024 0.79 5 1 1 25.88 10.77 3.40 0.019 2.06 -6 0 12 71.45 0.59 3.32 0.005 1.19 -3 0 3 129.26 69.53 3.24 0.050 3.24 -5 1 7 735.76 576.58 3.18 0.143 1.69 0 3 16 263.34 354.41 3.13 0.112 1.00 -2 1 6 39.65 22.21 3.01 0.028 2.54 0 2 5 288.19 369.19 3.00 0.114 2.65 8 2 8 33.82 58.95 2.98 0.046 1.06 -4 4 2 137.38 99.59 2.93 0.059 1.64 -4 3 10 -1.75 6.31 2.85 0.015 1.34 11 5 3 55.34 105.85 2.82 0.061 0.83 0 5 16 46.93 85.61 2.82 0.055 0.90 1 0 3 623.34 804.55 2.79 0.168 4.84 -6 4 2 51.33 30.28 2.78 0.033 1.37 3 2 4 87.76 121.25 2.76 0.065 2.22 6 3 3 15.14 5.68 2.75 0.014 1.43 -1 7 11 13.75 31.80 2.74 0.033 0.95 0 7 7 21.88 0.32 2.74 0.003 1.07 3 7 13 195.40 120.19 2.72 0.065 0.84 -3 6 10 -3.27 8.24 2.70 0.017 1.05 7 2 13 561.75 398.00 2.67 0.118 0.93 0 3 13 59.21 37.64 2.67 0.036 1.19 1 2 0 2619.05 3103.14 2.65 0.331 3.88 0 1 16 14.70 4.91 2.64 0.013 1.07 -9 0 13 323.55 471.47 2.64 0.129 0.95 8 2 11 226.90 142.08 2.63 0.071 0.95 -9 2 16 3.41 24.19 2.62 0.029 0.84 -6 1 6 371.20 297.72 2.61 0.102 1.59 2 1 3 1034.98 1252.71 2.61 0.210 3.40 0 2 0 3567.02 4231.04 2.60 0.386 4.15 -7 3 19 20.37 44.76 2.59 0.040 0.79 -4 1 6 9660.45 8167.06 2.58 0.537 2.03 0 6 3 46.11 27.75 2.57 0.031 1.34 1 5 5 173.04 221.95 2.56 0.088 1.47 -7 7 14 -2.08 18.10 2.55 0.025 0.77 Bond lengths and angles C1 - Distance Angles C2 1.3936 (0.0025) C6 1.4564 (0.0023) 119.00 (0.16) C13 1.4798 (0.0024) 117.38 (0.15) 123.60 (0.15) C1 - C2 C6 C2 - Distance Angles N2 1.3278 (0.0023) C1 1.3936 (0.0025) 125.45 (0.17) C3 1.5064 (0.0025) 112.71 (0.16) 121.84 (0.16) C2 - N2 C1 C3 - Distance Angles O2 1.2365 (0.0022) C4 1.4271 (0.0024) 123.47 (0.17) C2 1.5064 (0.0025) 118.89 (0.16) 117.63 (0.15) C3 - O2 C4 C4 - Distance Angles C5 1.3444 (0.0025) C3 1.4271 (0.0024) 119.83 (0.16) H4 0.9500 120.08 120.08 C4 - C5 C3 C5 - Distance Angles C4 1.3444 (0.0025) O1 1.3625 (0.0020) 116.75 (0.15) C6 1.4736 (0.0024) 124.78 (0.16) 118.47 (0.15) C5 - C4 O1 C6 - Distance Angles N1 1.3108 (0.0022) C1 1.4564 (0.0023) 122.06 (0.16) C5 1.4736 (0.0024) 121.05 (0.15) 116.86 (0.15) C6 - N1 C1 C7 - Distance Angles N1 1.3880 (0.0022) C12 1.3925 (0.0024) 122.08 (0.16) C8 1.4106 (0.0024) 120.68 (0.16) 117.23 (0.16) C7 - N1 C12 C8 - Distance Angles C9 1.3922 (0.0025) C7 1.4106 (0.0024) 119.90 (0.16) C16 1.4951 (0.0025) 118.96 (0.16) 120.98 (0.15) C8 - C9 C7 C9 - Distance Angles C8 1.3922 (0.0024) C10 1.3952 (0.0027) 120.66 (0.17) H9 0.9500 119.67 119.67 C9 - C8 C10 C10 - Distance Angles C11 1.3846 (0.0027) C9 1.3952 (0.0027) 120.56 (0.17) H10 0.9500 119.72 119.72 C10 - C11 C9 C11 - Distance Angles C10 1.3846 (0.0027) C12 1.3857 (0.0025) 117.90 (0.17) H11 0.9500 121.05 121.05 C11 - C10 C12 C12 - Distance Angles O1 1.3728 (0.0021) C11 1.3857 (0.0025) 117.05 (0.16) C7 1.3925 (0.0024) 119.23 (0.15) 123.72 (0.16) C12 - O1 C11 C13 - Distance Angles O3 1.2330 (0.0021) O4 1.3282 (0.0021) 121.30 (0.16) C1 1.4798 (0.0024) 122.92 (0.16) 115.79 (0.15) C13 - O3 O4 C14 - Distance Angles O4 1.4577 (0.0020) C15 1.5076 (0.0025) 106.13 (0.14) H14A 0.9900 110.51 110.51 H14B 0.9900 110.51 110.51 108.68 C14 - O4 C15 H14A C15 - Distance Angles C14 1.5076 (0.0025) H15A 0.9800 109.47 H15B 0.9800 109.47 109.47 H15C 0.9800 109.47 109.47 109.47 C15 - C14 H15A H15B C16 - Distance Angles O5 1.2098 (0.0022) O6 1.3435 (0.0022) 124.29 (0.17) C8 1.4951 (0.0025) 124.37 (0.16) 111.27 (0.15) C16 - O5 O6 C17 - Distance Angles O6 1.4629 (0.0021) C18 1.4996 (0.0029) 112.31 (0.16) H17A 0.9900 109.14 109.14 H17B 0.9900 109.14 109.14 107.87 C17 - O6 C18 H17A C18 - Distance Angles C17 1.4996 (0.0029) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - C17 H18A H18B N1 - Distance Angles C6 1.3108 (0.0022) C7 1.3880 (0.0022) 118.80 (0.15) N1 - C6 N2 - Distance Angles C2 1.3278 (0.0023) H1N 0.9280 (0.0243) 118.23 (1.47) H2N 0.8962 (0.0234) 119.57 (1.42) 121.94 (2.02) N2 - C2 H1N O1 - Distance Angles C5 1.3625 (0.0020) C12 1.3728 (0.0021) 120.28 (0.14) O1 - C5 O2 - Distance Angles C3 1.2365 (0.0022) O2 - O3 - Distance Angles C13 1.2330 (0.0021) O3 - O4 - Distance Angles C13 1.3282 (0.0021) C14 1.4577 (0.0020) 115.20 (0.13) O4 - C13 O5 - Distance Angles C16 1.2098 (0.0022) O5 - O6 - Distance Angles C16 1.3435 (0.0022) C17 1.4629 (0.0021) 116.18 (0.14) O6 - C16 Selected torsion angles -177.64 ( 0.16) C6 - C1 - C2 - N2 0.87 ( 0.27) C13 - C1 - C2 - N2 2.79 ( 0.25) C6 - C1 - C2 - C3 -178.70 ( 0.15) C13 - C1 - C2 - C3 -2.06 ( 0.25) N2 - C2 - C3 - O2 177.56 ( 0.17) C1 - C2 - C3 - O2 177.93 ( 0.16) N2 - C2 - C3 - C4 -2.45 ( 0.26) C1 - C2 - C3 - C4 -178.86 ( 0.18) O2 - C3 - C4 - C5 1.15 ( 0.26) C2 - C3 - C4 - C5 179.52 ( 0.16) C3 - C4 - C5 - O1 -0.34 ( 0.28) C3 - C4 - C5 - C6 176.14 ( 0.16) C2 - C1 - C6 - N1 -2.26 ( 0.26) C13 - C1 - C6 - N1 -1.85 ( 0.24) C2 - C1 - C6 - C5 179.74 ( 0.16) C13 - C1 - C6 - C5 -177.37 ( 0.17) C4 - C5 - C6 - N1 2.77 ( 0.25) O1 - C5 - C6 - N1 0.65 ( 0.26) C4 - C5 - C6 - C1 -179.21 ( 0.15) O1 - C5 - C6 - C1 176.83 ( 0.16) N1 - C7 - C8 - C9 -2.11 ( 0.25) C12 - C7 - C8 - C9 -7.81 ( 0.25) N1 - C7 - C8 - C16 173.25 ( 0.16) C12 - C7 - C8 - C16 1.98 ( 0.27) C7 - C8 - C9 - C10 -173.47 ( 0.17) C16 - C8 - C9 - C10 -0.64 ( 0.28) C8 - C9 - C10 - C11 -0.50 ( 0.27) C9 - C10 - C11 - C12 179.76 ( 0.16) C10 - C11 - C12 - O1 0.30 ( 0.28) C10 - C11 - C12 - C7 2.62 ( 0.26) N1 - C7 - C12 - O1 -178.46 ( 0.15) C8 - C7 - C12 - O1 -177.92 ( 0.16) N1 - C7 - C12 - C11 1.00 ( 0.27) C8 - C7 - C12 - C11 -8.43 ( 0.26) C2 - C1 - C13 - O3 170.00 ( 0.17) C6 - C1 - C13 - O3 171.57 ( 0.15) C2 - C1 - C13 - O4 -10.00 ( 0.25) C6 - C1 - C13 - O4 133.20 ( 0.19) C9 - C8 - C16 - O5 -42.20 ( 0.26) C7 - C8 - C16 - O5 -44.03 ( 0.22) C9 - C8 - C16 - O6 140.57 ( 0.17) C7 - C8 - C16 - O6 -178.51 ( 0.15) C1 - C6 - N1 - C7 -0.59 ( 0.24) C5 - C6 - N1 - C7 -2.10 ( 0.25) C12 - C7 - N1 - C6 179.01 ( 0.16) C8 - C7 - N1 - C6 177.90 ( 0.16) C4 - C5 - O1 - C12 -2.23 ( 0.23) C6 - C5 - O1 - C12 -179.81 ( 0.15) C11 - C12 - O1 - C5 -0.32 ( 0.24) C7 - C12 - O1 - C5 -3.19 ( 0.24) O3 - C13 - O4 - C14 176.81 ( 0.14) C1 - C13 - O4 - C14 -177.18 ( 0.15) C15 - C14 - O4 - C13 2.64 ( 0.26) O5 - C16 - O6 - C17 179.88 ( 0.14) C8 - C16 - O6 - C17 -80.34 ( 0.20) C18 - C17 - O6 - C16 FMAP and GRID set by program FMAP 2 3 22 GRID -1.316 -2 -2 1.316 2 2 R1 = 0.0716 for 3551 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.27 at 0.0729 0.1766 0.0014 [ 0.76 A from C5 ] Deepest hole -0.30 at 0.0661 0.1376 0.0836 [ 0.73 A from C5 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2906 / 19069 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9271 0.8234 -0.0014 1.00000 0.05 0.27 0.76 C5 0.82 C6 1.81 C4 1.89 O1 Q2 1 1.2661 0.6115 0.0765 1.00000 0.05 0.27 0.63 C8 0.88 C16 1.78 C9 1.81 C7 Q3 1 0.8157 0.6504 0.0904 1.00000 0.05 0.25 0.82 C1 0.93 C13 1.81 O4 1.90 C2 Q4 1 0.9201 0.7717 -0.0130 1.00000 0.05 0.25 0.75 C6 0.78 C5 1.82 N1 1.87 O1 Q5 1 1.1463 0.7695 -0.0147 1.00000 0.05 0.24 0.75 C12 0.78 C7 1.84 C8 1.85 C11 Q6 1 0.7385 0.7087 0.0536 1.00000 0.05 0.24 0.96 C2 1.00 C1 1.72 N2 1.80 C13 Q7 1 0.9376 0.6765 0.1695 1.00000 0.05 0.23 1.01 O4 1.30 C13 1.80 H18B 2.06 C1 Q8 1 1.0059 0.9612 -0.0937 1.00000 0.05 0.23 0.96 O1 1.67 C5 2.07 H4 2.09 C12 Q9 1 0.5987 1.1287 -0.0899 1.00000 0.05 0.23 1.38 O2 1.86 H15B 1.86 H2N 2.33 C3 Q10 1 1.0541 0.5729 0.0677 1.00000 0.05 0.23 0.93 N1 1.74 C7 2.01 C6 2.34 C8 Shortest distances between peaks (including symmetry equivalents) 1 4 0.47 3 6 1.11 3 7 1.81 1 8 2.22 2 10 2.33 2 5 2.33 4 8 2.37 3 4 2.45 7 10 2.45 5 10 2.46 4 6 2.47 1 5 2.47 4 5 2.48 1 8 2.48 5 8 2.50 4 10 2.52 1 3 2.55 1 6 2.55 2 9 2.61 1 10 2.70 3 10 2.76 10 10 2.78 6 7 2.80 4 8 2.94 Time profile in seconds ----------------------- 0.17: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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. 2.11: 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 1.27: Structure factors and derivatives 1.72: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 0.36: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 03src359 finished at 18:04:08 Total CPU time: 5.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++