+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007jmw0006 started at 11:49:33 on 27-Feb-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007jmw0006 in P2(1)/n CELL 0.71073 7.4546 14.7589 14.8296 90.000 94.816 90.000 ZERR 8.00 0.0004 0.0009 0.0007 0.000 0.003 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 72 64 16 16 V = 1625.82 F(000) = 736.0 Mu = 0.10 mm-1 Cell Wt = 1409.39 Rho = 1.439 MERG 2 OMIT -3.00 50.00 FMAP 2 PLAN 5 SIZE 0.02 0.04 0.24 ACTA BOND $H L.S. 6 TEMP -153.00 WGHT 0.0000 4.4414 FVAR 0.34547 MOLE 1 C1 1 0.145113 0.225340 0.261796 11.00000 0.01450 0.02873 = 0.02438 -0.00499 -0.00179 -0.00129 C2 1 0.154732 0.134051 0.237153 11.00000 0.02079 0.03106 = 0.03453 -0.01239 -0.00017 0.00115 AFIX 43 H2 2 0.192185 0.115699 0.180268 11.00000 -1.20000 AFIX 0 C3 1 0.106527 0.072588 0.300507 11.00000 0.02734 0.02397 = 0.04443 -0.00847 -0.00456 0.00202 AFIX 43 H3 2 0.111330 0.009750 0.287036 11.00000 -1.20000 AFIX 0 C4 1 0.050458 0.099664 0.384428 11.00000 0.02947 0.02452 = 0.03208 0.00340 -0.00233 -0.00293 AFIX 43 H4 2 0.019338 0.054769 0.426293 11.00000 -1.20000 AFIX 0 C5 1 0.039424 0.190254 0.407649 11.00000 0.02543 0.02880 = 0.02466 -0.00072 0.00146 -0.00072 AFIX 43 H5 2 -0.000348 0.208205 0.464175 11.00000 -1.20000 AFIX 0 C6 1 0.089206 0.254685 0.344548 11.00000 0.01377 0.02448 = 0.02979 -0.00254 -0.00110 0.00013 C7 1 0.102738 0.351129 0.341338 11.00000 0.01628 0.02433 = 0.02360 0.00031 0.00069 0.00088 C8 1 0.241824 0.307067 0.123574 11.00000 0.03382 0.04559 = 0.02484 -0.00377 0.00686 -0.00430 AFIX 137 H8A 2 0.260889 0.370441 0.107121 11.00000 -1.50000 H8B 2 0.148349 0.280448 0.081251 11.00000 -1.50000 H8C 2 0.354320 0.273223 0.120754 11.00000 -1.50000 AFIX 0 C9 1 0.058147 0.417045 0.409140 11.00000 0.02035 0.02083 = 0.02655 0.00173 0.00171 0.00186 N1 3 0.185227 0.302741 0.215114 11.00000 0.02257 0.03277 = 0.02111 -0.00456 0.00526 -0.00274 N2 3 0.159740 0.378242 0.262295 11.00000 0.02411 0.02635 = 0.02316 -0.00243 0.00273 0.00136 O1 4 -0.009131 0.388011 0.478948 11.00000 0.03484 0.02980 = 0.02368 0.00120 0.00923 0.00175 O2 4 0.090798 0.500815 0.394038 11.00000 0.04356 0.02551 = 0.03161 -0.00489 0.01318 -0.00022 AFIX 147 H2O 2 0.067564 0.531934 0.439033 11.00000 -1.20000 AFIX 0 MOLE 2 C10 1 0.635961 0.214425 0.270031 11.00000 0.01527 0.02398 = 0.02976 -0.00218 -0.00226 0.00291 C11 1 0.690221 0.179335 0.188623 11.00000 0.02524 0.02936 = 0.03320 -0.01117 -0.00370 0.00411 AFIX 43 H11 2 0.689538 0.116111 0.176575 11.00000 -1.20000 AFIX 0 C12 1 0.744361 0.241306 0.127309 11.00000 0.02364 0.03829 = 0.02659 -0.00804 0.00072 0.00493 AFIX 43 H12 2 0.781319 0.220416 0.071173 11.00000 -1.20000 AFIX 0 C13 1 0.746502 0.334432 0.145375 11.00000 0.01939 0.03560 = 0.02898 -0.00017 0.00423 0.00155 AFIX 43 H13 2 0.785953 0.374766 0.101192 11.00000 -1.20000 AFIX 0 C14 1 0.693644 0.369485 0.224623 11.00000 0.01918 0.02397 = 0.03025 0.00009 0.00185 -0.00081 AFIX 43 H14 2 0.695792 0.432894 0.235682 11.00000 -1.20000 AFIX 0 C15 1 0.636335 0.308450 0.288729 11.00000 0.01853 0.02503 = 0.02525 -0.00514 -0.00330 0.00400 C16 1 0.576081 0.313461 0.376940 11.00000 0.02131 0.02508 = 0.02503 -0.00345 0.00020 -0.00021 C17 1 0.561657 0.075278 0.359263 11.00000 0.02918 0.02274 = 0.04896 0.00009 0.00036 -0.00282 AFIX 137 H17A 2 0.679962 0.050763 0.380383 11.00000 -1.50000 H17B 2 0.518090 0.045513 0.302531 11.00000 -1.50000 H17C 2 0.476750 0.064219 0.405047 11.00000 -1.50000 AFIX 0 C18 1 0.546046 0.393830 0.432437 11.00000 0.01992 0.02518 = 0.02512 -0.00241 -0.00048 -0.00151 N3 3 0.576700 0.171933 0.344218 11.00000 0.02910 0.02180 = 0.02876 -0.00173 0.00203 0.00143 N4 3 0.540290 0.230746 0.409328 11.00000 0.02259 0.02457 = 0.03257 -0.00351 0.00074 0.00068 O3 4 0.590495 0.469980 0.393788 11.00000 0.04333 0.02211 = 0.02464 -0.00255 0.00916 0.00096 AFIX 147 H3O 2 0.567820 0.513915 0.427000 11.00000 -1.20000 AFIX 0 O4 4 0.486849 0.389641 0.506788 11.00000 0.04485 0.02429 = 0.02523 -0.00196 0.01495 -0.00313 HKLF 4 Covalent radii and connectivity table for 2007jmw0006 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 C1 - N1 C6 C2 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 C6 - C1 C5 C7 C7 - N2 C6 C9 C8 - N1 C9 - O1 O2 C7 N1 - N2 C1 C8 N2 - N1 C7 O1 - C9 O2 - C9 C10 - N3 C11 C15 C11 - C12 C10 C12 - C11 C13 C13 - C14 C12 C14 - C13 C15 C15 - C14 C10 C16 C16 - N4 C15 C18 C17 - N3 C18 - O4 O3 C16 N3 - N4 C10 C17 N4 - N3 C16 O3 - C18 O4 - C18 17178 Reflections read, of which 2458 rejected -7 =< h =< 8, -17 =< k =< 17, -17 =< l =< 15, Max. 2-theta = 49.98 0 Systematic absence violations 0 Inconsistent equivalents 2849 Unique reflections, of which 0 suppressed R(int) = 0.0872 R(sigma) = 0.0655 Friedel opposites merged Maximum memory for data reduction = 2169 / 28071 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 = 2816 / 296411 wR2 = 0.1629 before cycle 1 for 2849 data and 239 / 239 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.44 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34498 0.00103 -0.471 OSF Mean shift/esd = 0.018 Maximum = -0.471 for OSF Max. shift = 0.000 A for H2O Max. dU = 0.000 for O2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2816 / 296411 wR2 = 0.1629 before cycle 2 for 2849 data and 239 / 239 parameters GooF = S = 1.104; Restrained GooF = 1.104 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.44 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34488 0.00103 -0.095 OSF Mean shift/esd = 0.006 Maximum = -0.095 for OSF Max. shift = 0.000 A for H2O Max. dU = 0.000 for O2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2816 / 296411 wR2 = 0.1628 before cycle 3 for 2849 data and 239 / 239 parameters GooF = S = 1.104; Restrained GooF = 1.104 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.44 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34488 0.00103 -0.002 OSF Mean shift/esd = 0.000 Maximum = 0.004 for tors H2O Max. shift = 0.000 A for H2O Max. dU = 0.000 for C8 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2816 / 296411 wR2 = 0.1628 before cycle 4 for 2849 data and 239 / 239 parameters GooF = S = 1.104; Restrained GooF = 1.104 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.44 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34488 0.00103 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.002 for tors H2O Max. shift = 0.000 A for H2O Max. dU = 0.000 for C1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2816 / 296411 wR2 = 0.1628 before cycle 5 for 2849 data and 239 / 239 parameters GooF = S = 1.104; Restrained GooF = 1.104 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.44 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34488 0.00103 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for tors H2O Max. shift = 0.000 A for H2O Max. dU = 0.000 for N1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2816 / 296411 wR2 = 0.1628 before cycle 6 for 2849 data and 239 / 239 parameters GooF = S = 1.104; Restrained GooF = 1.104 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.44 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34488 0.00103 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H2O Max. dU = 0.000 for O2 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.1922 0.1157 0.1803 43 0.950 0.000 C2 C3 C1 H3 0.1113 0.0097 0.2870 43 0.950 0.000 C3 C2 C4 H4 0.0193 0.0548 0.4263 43 0.950 0.000 C4 C5 C3 H5 -0.0004 0.2082 0.4642 43 0.950 0.000 C5 C4 C6 H8A 0.2608 0.3704 0.1071 137 0.980 0.000 C8 N1 H8A H8B 0.1484 0.2804 0.0812 137 0.980 0.000 C8 N1 H8A H8C 0.3544 0.2733 0.1208 137 0.980 0.000 C8 N1 H8A H2O 0.0677 0.5319 0.4391 147 0.840 0.000 O2 C9 H2O H11 0.6895 0.1161 0.1766 43 0.950 0.000 C11 C12 C10 H12 0.7813 0.2204 0.0712 43 0.950 0.000 C12 C11 C13 H13 0.7860 0.3748 0.1012 43 0.950 0.000 C13 C14 C12 H14 0.6958 0.4329 0.2357 43 0.950 0.000 C14 C13 C15 H17A 0.6799 0.0508 0.3804 137 0.980 0.000 C17 N3 H17A H17B 0.5181 0.0455 0.3025 137 0.980 0.000 C17 N3 H17A H17C 0.4767 0.0642 0.4050 137 0.980 0.000 C17 N3 H17A H3O 0.5679 0.5139 0.4270 147 0.840 0.000 O3 C18 H3O 2007jmw0006 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.14512 0.22534 0.26179 1.00000 0.01445 0.02864 0.02427 -0.00499 -0.00179 -0.00128 0.02265 0.00628 0.00047 0.00026 0.00024 0.00000 0.00181 0.00218 0.00205 0.00168 0.00149 0.00154 0.00084 C2 0.15472 0.13404 0.23715 1.00000 0.02072 0.03094 0.03440 -0.01239 -0.00015 0.00115 0.02883 0.00661 0.00050 0.00027 0.00027 0.00000 0.00203 0.00231 0.00228 0.00184 0.00168 0.00168 0.00093 H2 0.19217 0.11569 0.18027 1.00000 0.03459 0.00000 0.00000 C3 0.10652 0.07258 0.30050 1.00000 0.02725 0.02386 0.04431 -0.00846 -0.00456 0.00202 0.03224 0.00698 0.00052 0.00028 0.00028 0.00000 0.00226 0.00215 0.00258 0.00190 0.00187 0.00171 0.00098 H3 0.11132 0.00975 0.28703 1.00000 0.03868 0.00000 0.00000 C4 0.05045 0.09966 0.38443 1.00000 0.02940 0.02441 0.03197 0.00342 -0.00231 -0.00293 0.02887 0.00674 0.00052 0.00027 0.00026 0.00000 0.00221 0.00217 0.00232 0.00173 0.00175 0.00172 0.00093 H4 0.01933 0.05476 0.42629 1.00000 0.03464 0.00000 0.00000 C5 0.03942 0.19025 0.40766 1.00000 0.02539 0.02867 0.02454 -0.00071 0.00149 -0.00072 0.02624 0.00676 0.00050 0.00026 0.00026 0.00000 0.00204 0.00223 0.00208 0.00166 0.00161 0.00170 0.00088 H5 -0.00035 0.20820 0.46418 1.00000 0.03148 0.00000 0.00000 C6 0.08920 0.25468 0.34455 1.00000 0.01373 0.02437 0.02969 -0.00256 -0.00108 0.00013 0.02276 0.00644 0.00048 0.00025 0.00026 0.00000 0.00182 0.00207 0.00217 0.00163 0.00153 0.00152 0.00084 C7 0.10274 0.35113 0.34134 1.00000 0.01623 0.02419 0.02353 0.00030 0.00069 0.00088 0.02137 0.00639 0.00047 0.00025 0.00024 0.00000 0.00185 0.00200 0.00200 0.00160 0.00150 0.00153 0.00081 C8 0.24183 0.30707 0.12357 1.00000 0.03376 0.04544 0.02474 -0.00376 0.00688 -0.00430 0.03440 0.00740 0.00056 0.00031 0.00026 0.00000 0.00239 0.00269 0.00223 0.00189 0.00181 0.00202 0.00102 H8A 0.26084 0.37045 0.10711 1.00000 0.05159 0.00000 0.00000 H8B 0.14838 0.28043 0.08125 1.00000 0.05159 0.00000 0.00000 H8C 0.35436 0.27325 0.12075 1.00000 0.05159 0.00000 0.00000 C9 0.05815 0.41705 0.40914 1.00000 0.02029 0.02074 0.02643 0.00171 0.00171 0.00187 0.02250 0.00656 0.00048 0.00025 0.00025 0.00000 0.00194 0.00213 0.00212 0.00158 0.00158 0.00153 0.00084 N1 0.18523 0.30274 0.21511 1.00000 0.02251 0.03264 0.02100 -0.00455 0.00527 -0.00274 0.02519 0.00540 0.00040 0.00022 0.00020 0.00000 0.00171 0.00192 0.00171 0.00144 0.00132 0.00143 0.00075 N2 0.15974 0.37824 0.26229 1.00000 0.02404 0.02624 0.02304 -0.00241 0.00274 0.00135 0.02439 0.00537 0.00041 0.00021 0.00020 0.00000 0.00173 0.00184 0.00171 0.00142 0.00133 0.00138 0.00074 O1 -0.00914 0.38801 0.47895 1.00000 0.03476 0.02966 0.02356 0.00118 0.00922 0.00175 0.02895 0.00475 0.00036 0.00018 0.00017 0.00000 0.00158 0.00154 0.00148 0.00119 0.00121 0.00126 0.00065 O2 0.09080 0.50082 0.39404 1.00000 0.04345 0.02541 0.03146 -0.00489 0.01316 -0.00023 0.03288 0.00501 0.00039 0.00018 0.00018 0.00000 0.00176 0.00155 0.00159 0.00123 0.00132 0.00132 0.00069 H2O 0.06770 0.53193 0.43906 1.00000 0.03945 0.00000 0.00000 C10 0.63596 0.21442 0.27003 1.00000 0.01523 0.02384 0.02969 -0.00219 -0.00226 0.00291 0.02316 0.00644 0.00047 0.00025 0.00025 0.00000 0.00181 0.00213 0.00216 0.00164 0.00153 0.00151 0.00085 C11 0.69022 0.17933 0.18861 1.00000 0.02518 0.02925 0.03307 -0.01117 -0.00368 0.00412 0.02951 0.00678 0.00051 0.00028 0.00027 0.00000 0.00214 0.00228 0.00233 0.00179 0.00173 0.00171 0.00095 H11 0.68954 0.11611 0.17656 1.00000 0.03541 0.00000 0.00000 C12 0.74436 0.24130 0.12731 1.00000 0.02355 0.03819 0.02648 -0.00803 0.00072 0.00493 0.02948 0.00695 0.00052 0.00028 0.00027 0.00000 0.00213 0.00250 0.00220 0.00181 0.00168 0.00178 0.00095 H12 0.78132 0.22041 0.07117 1.00000 0.03538 0.00000 0.00000 C13 0.74652 0.33444 0.14537 1.00000 0.01931 0.03549 0.02887 -0.00016 0.00423 0.00155 0.02776 0.00692 0.00050 0.00027 0.00026 0.00000 0.00199 0.00240 0.00220 0.00178 0.00162 0.00168 0.00092 H13 0.78598 0.37477 0.10119 1.00000 0.03332 0.00000 0.00000 C14 0.69366 0.36949 0.22462 1.00000 0.01913 0.02384 0.03014 0.00010 0.00185 -0.00082 0.02438 0.00659 0.00047 0.00026 0.00025 0.00000 0.00195 0.00210 0.00217 0.00166 0.00157 0.00154 0.00086 H14 0.69581 0.43290 0.23568 1.00000 0.02926 0.00000 0.00000 C15 0.63634 0.30845 0.28873 1.00000 0.01849 0.02492 0.02515 -0.00514 -0.00328 0.00400 0.02314 0.00642 0.00048 0.00026 0.00025 0.00000 0.00185 0.00207 0.00206 0.00162 0.00153 0.00157 0.00084 C16 0.57608 0.31346 0.37695 1.00000 0.02127 0.02499 0.02490 -0.00346 0.00022 -0.00021 0.02382 0.00642 0.00048 0.00026 0.00025 0.00000 0.00197 0.00215 0.00209 0.00161 0.00158 0.00160 0.00086 C17 0.56164 0.07527 0.35926 1.00000 0.02911 0.02263 0.04880 0.00008 0.00039 -0.00282 0.03368 0.00735 0.00056 0.00026 0.00030 0.00000 0.00230 0.00218 0.00268 0.00189 0.00191 0.00174 0.00100 H17A 0.67994 0.05076 0.38039 1.00000 0.05051 0.00000 0.00000 H17B 0.51810 0.04551 0.30252 1.00000 0.05051 0.00000 0.00000 H17C 0.47672 0.06421 0.40503 1.00000 0.05051 0.00000 0.00000 C18 0.54605 0.39383 0.43244 1.00000 0.01985 0.02506 0.02503 -0.00244 -0.00049 -0.00149 0.02345 0.00640 0.00048 0.00025 0.00025 0.00000 0.00192 0.00214 0.00212 0.00168 0.00158 0.00161 0.00084 N3 0.57669 0.17193 0.34422 1.00000 0.02904 0.02168 0.02864 -0.00171 0.00205 0.00142 0.02647 0.00558 0.00043 0.00020 0.00021 0.00000 0.00184 0.00175 0.00185 0.00142 0.00141 0.00138 0.00076 N4 0.54029 0.23074 0.40933 1.00000 0.02253 0.02445 0.03244 -0.00349 0.00076 0.00067 0.02656 0.00555 0.00042 0.00021 0.00021 0.00000 0.00174 0.00182 0.00189 0.00147 0.00140 0.00137 0.00076 O3 0.59050 0.46998 0.39379 1.00000 0.04322 0.02200 0.02452 -0.00256 0.00915 0.00095 0.02956 0.00486 0.00038 0.00018 0.00017 0.00000 0.00176 0.00147 0.00147 0.00114 0.00125 0.00125 0.00067 H3O 0.56786 0.51391 0.42701 1.00000 0.03547 0.00000 0.00000 O4 0.48685 0.38964 0.50679 1.00000 0.04476 0.02415 0.02513 -0.00196 0.01494 -0.00314 0.03067 0.00489 0.00038 0.00018 0.00018 0.00000 0.00173 0.00147 0.00150 0.00116 0.00126 0.00127 0.00066 Final Structure Factor Calculation for 2007jmw0006 in P2(1)/n Total number of l.s. parameters = 239 Maximum vector length = 511 Memory required = 2577 / 22995 wR2 = 0.1628 before cycle 7 for 2849 data and 0 / 239 parameters GooF = S = 1.104; Restrained GooF = 1.104 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.44 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0772 for 2008 Fo > 4sig(Fo) and 0.1186 for all 2849 data wR2 = 0.1628, GooF = S = 1.104, Restrained GooF = 1.104 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 0.0320 0.0227 0.0132 C1 0.0458 0.0208 0.0200 C2 0.0508 0.0251 0.0208 C3 0.0378 0.0260 0.0227 C4 0.0289 0.0257 0.0241 C5 0.0314 0.0234 0.0134 C6 0.0243 0.0237 0.0161 C7 0.0477 0.0331 0.0224 C8 0.0269 0.0221 0.0185 C9 0.0351 0.0228 0.0176 N1 0.0278 0.0244 0.0210 N2 0.0379 0.0292 0.0197 O1 0.0486 0.0292 0.0208 O2 0.0323 0.0233 0.0139 C10 0.0459 0.0228 0.0198 C11 0.0439 0.0234 0.0211 C12 0.0356 0.0292 0.0185 C13 0.0302 0.0240 0.0190 C14 0.0336 0.0200 0.0159 C15 0.0287 0.0226 0.0201 C16 0.0495 0.0299 0.0216 C17 0.0276 0.0243 0.0184 C18 0.0299 0.0285 0.0210 N3 0.0342 0.0232 0.0223 N4 0.0447 0.0248 0.0192 O3 0.0500 0.0237 0.0183 O4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.005 0.011 0.016 0.021 0.028 0.036 0.047 0.063 0.089 1.000 Number in group 291. 326. 293. 247. 283. 273. 299. 273. 277. 287. GooF 1.138 1.231 1.176 1.123 1.161 1.067 1.082 1.027 0.933 1.047 K 10.795 2.422 1.306 1.152 1.074 1.074 0.992 0.990 1.005 1.000 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.26 1.44 1.81 inf Number in group 290. 293. 271. 286. 284. 284. 288. 284. 283. 286. GooF 1.243 1.227 1.219 1.027 1.123 1.069 1.010 0.956 0.956 1.164 K 1.105 1.112 1.028 1.023 0.996 0.996 1.013 1.023 1.034 0.988 R1 0.263 0.256 0.235 0.157 0.111 0.093 0.088 0.088 0.054 0.050 Recommended weighting scheme: WGHT 0.0000 4.4838 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) 6 3 0 184.00 38.14 4.56 0.021 1.20 -5 6 12 131.40 5.88 3.63 0.008 0.92 2 7 14 93.39 7.97 3.46 0.010 0.90 0 0 4 4863.14 5651.50 3.46 0.260 3.69 1 14 2 47.11 141.66 3.45 0.041 1.03 1 6 9 39.24 0.08 3.37 0.001 1.33 -5 12 6 117.81 36.01 3.18 0.021 0.90 1 4 15 227.61 387.04 2.97 0.068 0.93 6 3 2 76.30 19.86 2.94 0.015 1.17 -1 0 7 474.94 330.82 2.90 0.063 2.08 6 9 2 131.40 51.93 2.88 0.025 0.97 6 3 6 353.52 227.02 2.84 0.052 1.05 2 9 9 89.46 30.43 2.83 0.019 1.09 -1 1 1 93.66 179.87 2.79 0.046 6.23 -1 13 11 93.86 14.80 2.78 0.013 0.87 -2 9 10 147.39 248.17 2.74 0.054 1.07 -1 1 9 32.36 0.55 2.70 0.003 1.62 -8 6 4 94.51 25.54 2.69 0.017 0.86 -6 4 11 -17.15 38.67 2.69 0.021 0.92 -7 9 4 191.53 83.86 2.68 0.032 0.88 -5 0 15 66.39 6.95 2.67 0.009 0.85 4 10 9 24.37 87.87 2.66 0.032 0.92 7 8 4 -22.75 61.43 2.65 0.027 0.88 -3 7 14 87.67 20.38 2.62 0.016 0.90 6 3 10 86.94 10.48 2.60 0.011 0.90 0 11 6 41.42 2.57 2.58 0.006 1.18 4 2 11 -15.14 19.29 2.58 0.015 1.04 -7 8 8 92.07 11.89 2.58 0.012 0.85 -1 7 12 -5.04 24.77 2.56 0.017 1.06 -6 7 2 27.69 99.80 2.55 0.035 1.07 -5 6 5 -14.01 17.97 2.55 0.015 1.20 6 4 11 -7.84 41.02 2.55 0.022 0.85 -2 11 9 126.54 55.85 2.55 0.026 1.01 -1 0 1 57.33 119.64 2.52 0.038 6.87 -7 2 3 54.97 123.32 2.51 0.038 1.05 -3 14 5 92.10 4.03 2.50 0.007 0.93 0 15 4 -7.12 46.82 2.49 0.024 0.95 6 10 5 45.78 0.67 2.47 0.003 0.89 -4 2 15 47.11 7.15 2.46 0.009 0.90 -1 15 4 43.78 120.22 2.46 0.038 0.95 -2 14 9 142.07 54.01 2.44 0.025 0.87 -3 4 12 -2.89 38.30 2.43 0.021 1.09 6 8 3 177.23 78.76 2.43 0.031 0.99 -5 6 9 62.16 3.75 2.42 0.007 1.04 0 6 4 1038.97 846.35 2.42 0.100 2.05 7 7 0 124.12 47.03 2.41 0.024 0.95 -6 4 6 37.63 3.10 2.41 0.006 1.09 -2 0 2 654.14 831.14 2.41 0.100 3.44 6 12 2 371.87 241.24 2.40 0.054 0.86 -4 5 7 46.88 0.11 2.40 0.001 1.31 Bond lengths and angles C1 - Distance Angles N1 1.3814 (0.0049) C6 1.3976 (0.0052) 106.07 (0.31) C2 1.3996 (0.0053) 130.34 (0.35) 123.59 (0.36) C1 - N1 C6 C2 - Distance Angles C3 1.3752 (0.0058) C1 1.3996 (0.0053) 115.76 (0.36) H2 0.9500 122.12 122.12 C2 - C3 C1 C3 - Distance Angles C2 1.3752 (0.0058) C4 1.4039 (0.0056) 122.16 (0.37) H3 0.9500 118.92 118.92 C3 - C2 C4 C4 - Distance Angles C5 1.3848 (0.0054) C3 1.4039 (0.0056) 121.58 (0.37) H4 0.9500 119.21 119.21 C4 - C5 C3 C5 - Distance Angles C4 1.3848 (0.0054) C6 1.4058 (0.0053) 117.58 (0.36) H5 0.9500 121.21 121.21 C5 - C4 C6 C6 - Distance Angles C1 1.3976 (0.0052) C5 1.4058 (0.0053) 119.33 (0.35) C7 1.4282 (0.0051) 104.63 (0.33) 136.04 (0.36) C6 - C1 C5 C7 - Distance Angles N2 1.3410 (0.0046) C6 1.4282 (0.0051) 110.79 (0.32) C9 1.4574 (0.0051) 120.75 (0.33) 128.43 (0.34) C7 - N2 C6 C8 - Distance Angles N1 1.4565 (0.0047) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - N1 H8A H8B C9 - Distance Angles O1 1.2625 (0.0043) O2 1.2834 (0.0044) 124.36 (0.34) C7 1.4574 (0.0051) 117.93 (0.33) 117.71 (0.33) C9 - O1 O2 N1 - Distance Angles N2 1.3378 (0.0042) C1 1.3814 (0.0049) 112.37 (0.28) C8 1.4565 (0.0047) 121.06 (0.32) 126.53 (0.33) N1 - N2 C1 N2 - Distance Angles N1 1.3378 (0.0042) C7 1.3410 (0.0046) 106.14 (0.29) N2 - N1 O1 - Distance Angles C9 1.2625 (0.0044) O1 - O2 - Distance Angles C9 1.2834 (0.0044) H2O 0.8400 109.47 O2 - C9 C10 - Distance Angles N3 1.3713 (0.0048) C11 1.4042 (0.0053) 131.05 (0.35) C15 1.4152 (0.0052) 106.67 (0.32) 122.29 (0.36) C10 - N3 C11 C11 - Distance Angles C12 1.3739 (0.0057) C10 1.4042 (0.0053) 116.44 (0.36) H11 0.9500 121.78 121.78 C11 - C12 C10 C12 - Distance Angles C11 1.3739 (0.0057) C13 1.4002 (0.0056) 121.75 (0.37) H12 0.9500 119.13 119.13 C12 - C11 C13 C13 - Distance Angles C14 1.3717 (0.0052) C12 1.4002 (0.0056) 122.32 (0.37) H13 0.9500 118.84 118.84 C13 - C14 C12 C14 - Distance Angles C13 1.3717 (0.0052) C15 1.4022 (0.0053) 117.67 (0.36) H14 0.9500 121.16 121.16 C14 - C13 C15 C15 - Distance Angles C14 1.4022 (0.0053) C10 1.4152 (0.0052) 119.53 (0.35) C16 1.4204 (0.0052) 136.80 (0.36) 103.64 (0.33) C15 - C14 C10 C16 - Distance Angles N4 1.3467 (0.0048) C15 1.4204 (0.0052) 111.64 (0.33) C18 1.4715 (0.0051) 119.16 (0.32) 129.18 (0.35) C16 - N4 C15 C17 - Distance Angles N3 1.4497 (0.0048) H17A 0.9800 109.47 H17B 0.9800 109.47 109.47 H17C 0.9800 109.47 109.47 109.47 C17 - N3 H17A H17B C18 - Distance Angles O4 1.2231 (0.0043) O3 1.3165 (0.0044) 123.97 (0.34) C16 1.4715 (0.0051) 123.14 (0.35) 112.89 (0.31) C18 - O4 O3 N3 - Distance Angles N4 1.3429 (0.0043) C10 1.3713 (0.0048) 112.30 (0.30) C17 1.4497 (0.0048) 120.16 (0.33) 127.43 (0.33) N3 - N4 C10 N4 - Distance Angles N3 1.3429 (0.0043) C16 1.3467 (0.0048) 105.75 (0.30) N4 - N3 O3 - Distance Angles C18 1.3165 (0.0044) H3O 0.8400 109.47 O3 - C18 O4 - Distance Angles C18 1.2231 (0.0043) O4 - FMAP and GRID set by program FMAP 2 1 11 GRID -3.125 -2 -2 3.125 2 2 R1 = 0.1186 for 2849 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.25 at 0.0673 0.5796 0.4840 [ 0.87 A from O1 ] Deepest hole -0.30 at 0.1024 0.1926 0.2011 [ 1.05 A from C1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2816 / 19267 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0673 0.4204 0.5160 1.00000 0.05 0.25 0.87 O1 0.97 H2O 1.79 O2 1.91 C9 Q2 1 0.4171 0.3551 0.1186 1.00000 0.05 0.24 1.18 H8A 1.30 H8C 1.49 C8 2.31 H8B Q3 1 0.7216 0.5199 0.4821 1.00000 0.05 0.24 1.35 H3O 1.73 O3 2.03 H2O 2.07 O4 Q4 1 0.4632 0.2722 0.4182 1.00000 0.05 0.23 0.86 N4 1.24 C16 1.91 C18 2.07 N3 Q5 1 0.2256 0.4238 0.2367 1.00000 0.05 0.23 0.93 N2 1.81 H3 1.83 N1 2.11 H8A Shortest distances between peaks (including symmetry equivalents) 1 3 2.18 2 5 2.56 1 1 2.61 1 3 2.72 Time profile in seconds ----------------------- 0.04: 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. 0.69: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.88: Structure factors and derivatives 1.44: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.19: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.10: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.01: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007jmw0006 finished at 11:49:36 Total CPU time: 3.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++