+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007ncs0623 started at 13:36:38 on 09-Jul-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007NCS0623 in P2(1)/c CELL 0.71073 11.9613 6.6856 13.4450 90.000 106.263 90.000 ZERR 4.00 0.0005 0.0002 0.0004 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 44 56 8 4 V = 1032.15 F(000) = 408.0 Mu = 0.08 mm-1 Cell Wt = 760.97 Rho = 1.224 MERG 2 ACTA OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.10 0.14 0.16 BOND $H WGHT 0.03960 1.21770 L.S. 20 TEMP -153.00 FVAR 0.87504 C1 1 0.450139 -0.017849 0.353286 11.00000 0.02246 0.02487 = 0.02920 0.00445 -0.00261 0.00052 AFIX 43 H1 2 0.520847 -0.060000 0.401011 11.00000 -1.20000 AFIX 0 C2 1 0.435207 -0.059348 0.248930 11.00000 0.02167 0.02173 = 0.03272 0.00151 0.00340 0.00154 AFIX 43 H2 2 0.493494 -0.124874 0.225335 11.00000 -1.20000 AFIX 0 C3 1 0.330321 0.000550 0.181502 11.00000 0.02281 0.01758 = 0.02176 0.00151 0.00342 -0.00293 C4 1 0.245907 0.096396 0.218490 11.00000 0.02050 0.01814 = 0.02135 0.00232 0.00190 -0.00118 C5 1 0.271008 0.131640 0.323471 11.00000 0.02468 0.02631 = 0.02299 0.00300 0.00351 0.00155 AFIX 43 H5 2 0.214321 0.197438 0.349074 11.00000 -1.20000 AFIX 0 C6 1 0.140017 0.135534 0.128517 11.00000 0.01897 0.02231 = 0.01706 0.00177 0.00184 -0.00094 AFIX 13 H6 2 0.074197 0.051516 0.137149 11.00000 -1.20000 AFIX 0 C7 1 0.178830 0.054724 0.037405 11.00000 0.02402 0.02025 = 0.01945 0.00015 0.00494 -0.00504 C8 1 0.352721 -0.108891 0.007049 11.00000 0.03113 0.03671 = 0.03200 -0.00560 0.01333 0.00354 AFIX 137 H8A 2 0.298995 -0.189118 -0.046536 11.00000 -1.50000 H8B 2 0.415211 -0.194620 0.048061 11.00000 -1.50000 H8C 2 0.386300 -0.002543 -0.025743 11.00000 -1.50000 AFIX 0 C9 1 0.096935 0.352865 0.106122 11.00000 0.02354 0.02425 = 0.02093 0.00344 0.00177 0.00277 AFIX 13 H9 2 0.041617 0.353764 0.034897 11.00000 -1.20000 AFIX 0 C10 1 0.196025 0.495135 0.104055 11.00000 0.03423 0.02293 = 0.04356 0.00475 0.00449 -0.00185 AFIX 137 H10A 2 0.164069 0.627495 0.080726 11.00000 -1.50000 H10B 2 0.237801 0.443477 0.056325 11.00000 -1.50000 H10C 2 0.249839 0.505798 0.173787 11.00000 -1.50000 AFIX 0 C11 1 0.028846 0.424537 0.179424 11.00000 0.03988 0.03742 = 0.02651 0.00460 0.00874 0.01488 AFIX 137 H11A 2 0.080238 0.427347 0.250405 11.00000 -1.50000 H11B 2 -0.036236 0.333152 0.175795 11.00000 -1.50000 H11C 2 -0.001331 0.559287 0.159299 11.00000 -1.50000 AFIX 0 N1 3 0.372757 0.076756 0.391733 11.00000 0.02835 0.02998 = 0.02141 0.00466 -0.00169 0.00063 N2 3 0.289926 -0.020489 0.074327 11.00000 0.02287 0.02288 = 0.02212 -0.00173 0.00552 -0.00064 O1 4 0.123911 0.056016 -0.053667 11.00000 0.02988 0.03508 = 0.01827 -0.00072 0.00300 -0.00498 HKLF 4 Covalent radii and connectivity table for 2007NCS0623 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - N1 C2 C2 - C3 C1 C3 - C2 N2 C4 C4 - C5 C3 C6 C5 - N1 C4 C6 - C4 C7 C9 C7 - O1 N2 C6 C8 - N2 C9 - C11 C10 C6 C10 - C9 C11 - C9 N1 - C1 C5 N2 - C7 C3 C8 O1 - C7 9511 Reflections read, of which 528 rejected -15 =< h =< 15, -8 =< k =< 8, -17 =< l =< 17, Max. 2-theta = 54.93 0 Systematic absence violations 0 Inconsistent equivalents 2357 Unique reflections, of which 0 suppressed R(int) = 0.0448 R(sigma) = 0.0440 Friedel opposites merged Maximum memory for data reduction = 1537 / 23490 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 = 1919 / 164630 wR2 = 0.1460 before cycle 1 for 2357 data and 130 / 130 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0396 * P )^2 + 1.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87504 0.00253 0.000 OSF Mean shift/esd = 0.007 Maximum = -0.032 for tors H8A Max. shift = 0.001 A for H8B Max. dU = 0.000 for C9 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1919 / 164630 wR2 = 0.1460 before cycle 2 for 2357 data and 130 / 130 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0396 * P )^2 + 1.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87503 0.00253 -0.003 OSF Mean shift/esd = 0.003 Maximum = -0.037 for tors H8A Max. shift = 0.001 A for H8B Max. dU = 0.000 for C9 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1919 / 164630 wR2 = 0.1460 before cycle 3 for 2357 data and 130 / 130 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0396 * P )^2 + 1.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87503 0.00253 0.000 OSF Mean shift/esd = 0.001 Maximum = -0.032 for tors H8A Max. shift = 0.001 A for H8B Max. dU = 0.000 for C8 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1919 / 164630 wR2 = 0.1460 before cycle 4 for 2357 data and 130 / 130 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0396 * P )^2 + 1.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87503 0.00253 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.027 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for C8 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1919 / 164630 wR2 = 0.1460 before cycle 5 for 2357 data and 130 / 130 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0396 * P )^2 + 1.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87503 0.00253 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.023 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for C2 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1919 / 164630 wR2 = 0.1460 before cycle 6 for 2357 data and 130 / 130 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0396 * P )^2 + 1.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87503 0.00253 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.020 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for C2 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1919 / 164630 wR2 = 0.1460 before cycle 7 for 2357 data and 130 / 130 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0396 * P )^2 + 1.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87503 0.00253 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.017 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for C2 Least-squares cycle 8 Maximum vector length = 511 Memory required = 1919 / 164630 wR2 = 0.1460 before cycle 8 for 2357 data and 130 / 130 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0396 * P )^2 + 1.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87503 0.00253 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.015 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for C2 Least-squares cycle 9 Maximum vector length = 511 Memory required = 1919 / 164630 wR2 = 0.1460 before cycle 9 for 2357 data and 130 / 130 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0396 * P )^2 + 1.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87503 0.00253 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.013 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for C8 Least-squares cycle 10 Maximum vector length = 511 Memory required = 1919 / 164630 wR2 = 0.1460 before cycle 10 for 2357 data and 130 / 130 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0396 * P )^2 + 1.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87503 0.00253 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.011 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for C2 Least-squares cycle 11 Maximum vector length = 511 Memory required = 1919 / 164630 wR2 = 0.1460 before cycle 11 for 2357 data and 130 / 130 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0396 * P )^2 + 1.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87503 0.00253 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.009 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for C2 Least-squares cycle 12 Maximum vector length = 511 Memory required = 1919 / 164630 wR2 = 0.1460 before cycle 12 for 2357 data and 130 / 130 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0396 * P )^2 + 1.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87503 0.00253 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.008 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for C2 Least-squares cycle 13 Maximum vector length = 511 Memory required = 1919 / 164630 wR2 = 0.1460 before cycle 13 for 2357 data and 130 / 130 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0396 * P )^2 + 1.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87503 0.00253 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.007 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for C2 Least-squares cycle 14 Maximum vector length = 511 Memory required = 1919 / 164630 wR2 = 0.1460 before cycle 14 for 2357 data and 130 / 130 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0396 * P )^2 + 1.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87503 0.00253 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.006 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for C6 Least-squares cycle 15 Maximum vector length = 511 Memory required = 1919 / 164630 wR2 = 0.1460 before cycle 15 for 2357 data and 130 / 130 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0396 * P )^2 + 1.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87503 0.00253 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.005 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for C11 Least-squares cycle 16 Maximum vector length = 511 Memory required = 1919 / 164630 wR2 = 0.1460 before cycle 16 for 2357 data and 130 / 130 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0396 * P )^2 + 1.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87503 0.00253 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.004 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for C2 Least-squares cycle 17 Maximum vector length = 511 Memory required = 1919 / 164630 wR2 = 0.1460 before cycle 17 for 2357 data and 130 / 130 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0396 * P )^2 + 1.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87503 0.00253 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.004 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for C8 Least-squares cycle 18 Maximum vector length = 511 Memory required = 1919 / 164630 wR2 = 0.1460 before cycle 18 for 2357 data and 130 / 130 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0396 * P )^2 + 1.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87503 0.00253 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.003 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for C2 Least-squares cycle 19 Maximum vector length = 511 Memory required = 1919 / 164630 wR2 = 0.1460 before cycle 19 for 2357 data and 130 / 130 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0396 * P )^2 + 1.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87503 0.00253 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.003 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for C2 Least-squares cycle 20 Maximum vector length = 511 Memory required = 1919 / 164630 wR2 = 0.1460 before cycle 20 for 2357 data and 130 / 130 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0396 * P )^2 + 1.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87503 0.00253 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for C6 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.5208 -0.0600 0.4010 43 0.950 0.000 C1 N1 C2 H2 0.4935 -0.1249 0.2253 43 0.950 0.000 C2 C3 C1 H5 0.2143 0.1974 0.3491 43 0.950 0.000 C5 N1 C4 H6 0.0742 0.0515 0.1371 13 1.000 0.000 C6 C4 C7 C9 H8A 0.2991 -0.1897 -0.0463 137 0.980 0.000 C8 N2 H8A H8B 0.4155 -0.1941 0.0481 137 0.980 0.000 C8 N2 H8A H8C 0.3860 -0.0025 -0.0260 137 0.980 0.000 C8 N2 H8A H9 0.0416 0.3538 0.0349 13 1.000 0.000 C9 C11 C10 C6 H10A 0.1641 0.6275 0.0807 137 0.980 0.000 C10 C9 H10A H10B 0.2378 0.4435 0.0563 137 0.980 0.000 C10 C9 H10A H10C 0.2498 0.5058 0.1738 137 0.980 0.000 C10 C9 H10A H11A 0.0802 0.4274 0.2504 137 0.980 0.000 C11 C9 H11A H11B -0.0362 0.3331 0.1758 137 0.980 0.000 C11 C9 H11A H11C -0.0013 0.5593 0.1593 137 0.980 0.000 C11 C9 H11A 2007NCS0623 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.45014 -0.01785 0.35328 1.00000 0.02246 0.02486 0.02920 0.00446 -0.00261 0.00051 0.02750 0.00387 0.00017 0.00031 0.00016 0.00000 0.00097 0.00105 0.00107 0.00083 0.00082 0.00081 0.00046 H1 0.52085 -0.06000 0.40101 1.00000 0.03300 0.00000 0.00000 C2 0.43520 -0.05934 0.24893 1.00000 0.02165 0.02172 0.03274 0.00152 0.00341 0.00153 0.02622 0.00387 0.00017 0.00031 0.00016 0.00000 0.00096 0.00099 0.00107 0.00083 0.00082 0.00079 0.00044 H2 0.49349 -0.12487 0.22534 1.00000 0.03147 0.00000 0.00000 C3 0.33032 0.00055 0.18151 1.00000 0.02280 0.01756 0.02176 0.00151 0.00342 -0.00294 0.02128 0.00361 0.00016 0.00028 0.00014 0.00000 0.00092 0.00090 0.00091 0.00071 0.00074 0.00073 0.00041 C4 0.24591 0.09639 0.21849 1.00000 0.02050 0.01812 0.02134 0.00232 0.00190 -0.00119 0.02079 0.00355 0.00016 0.00028 0.00014 0.00000 0.00089 0.00093 0.00092 0.00072 0.00072 0.00073 0.00041 C5 0.27101 0.13164 0.32347 1.00000 0.02468 0.02629 0.02301 0.00300 0.00352 0.00155 0.02530 0.00385 0.00017 0.00031 0.00015 0.00000 0.00098 0.00104 0.00097 0.00079 0.00078 0.00080 0.00044 H5 0.21433 0.19745 0.34907 1.00000 0.03036 0.00000 0.00000 C6 0.14002 0.13553 0.12852 1.00000 0.01896 0.02231 0.01707 0.00177 0.00184 -0.00096 0.02009 0.00355 0.00016 0.00029 0.00014 0.00000 0.00088 0.00095 0.00086 0.00071 0.00069 0.00073 0.00040 H6 0.07420 0.05152 0.13715 1.00000 0.02411 0.00000 0.00000 C7 0.17883 0.05472 0.03741 1.00000 0.02402 0.02024 0.01946 0.00015 0.00493 -0.00506 0.02147 0.00358 0.00017 0.00029 0.00014 0.00000 0.00093 0.00094 0.00090 0.00073 0.00073 0.00077 0.00041 C8 0.35272 -0.10888 0.00705 1.00000 0.03114 0.03673 0.03200 -0.00560 0.01335 0.00353 0.03238 0.00445 0.00019 0.00036 0.00017 0.00000 0.00110 0.00126 0.00113 0.00093 0.00091 0.00096 0.00051 H8A 0.29908 -0.18965 -0.04633 1.00000 0.04857 0.00000 0.00000 H8B 0.41546 -0.19408 0.04812 1.00000 0.04857 0.00000 0.00000 H8C 0.38597 -0.00252 -0.02601 1.00000 0.04857 0.00000 0.00000 C9 0.09694 0.35285 0.10612 1.00000 0.02353 0.02424 0.02091 0.00344 0.00177 0.00277 0.02379 0.00385 0.00017 0.00030 0.00015 0.00000 0.00095 0.00103 0.00093 0.00076 0.00075 0.00078 0.00043 H9 0.04162 0.35375 0.03490 1.00000 0.02855 0.00000 0.00000 C10 0.19602 0.49514 0.10406 1.00000 0.03422 0.02293 0.04357 0.00475 0.00448 -0.00184 0.03487 0.00440 0.00020 0.00033 0.00019 0.00000 0.00119 0.00107 0.00131 0.00095 0.00101 0.00091 0.00053 H10A 0.16406 0.62750 0.08074 1.00000 0.05231 0.00000 0.00000 H10B 0.23779 0.44350 0.05632 1.00000 0.05231 0.00000 0.00000 H10C 0.24984 0.50579 0.17378 1.00000 0.05231 0.00000 0.00000 C11 0.02885 0.42454 0.17943 1.00000 0.03989 0.03740 0.02650 0.00459 0.00873 0.01487 0.03471 0.00476 0.00020 0.00037 0.00017 0.00000 0.00126 0.00128 0.00107 0.00092 0.00093 0.00103 0.00053 H11A 0.08024 0.42739 0.25040 1.00000 0.05206 0.00000 0.00000 H11B -0.03622 0.33313 0.17581 1.00000 0.05206 0.00000 0.00000 H11C -0.00135 0.55927 0.15929 1.00000 0.05206 0.00000 0.00000 N1 0.37276 0.07675 0.39173 1.00000 0.02836 0.02998 0.02141 0.00465 -0.00169 0.00062 0.02833 0.00329 0.00015 0.00027 0.00013 0.00000 0.00090 0.00097 0.00084 0.00071 0.00069 0.00075 0.00041 N2 0.28992 -0.02049 0.07433 1.00000 0.02287 0.02286 0.02211 -0.00174 0.00554 -0.00064 0.02277 0.00309 0.00014 0.00025 0.00012 0.00000 0.00082 0.00086 0.00081 0.00065 0.00066 0.00066 0.00038 O1 0.12391 0.05601 -0.05367 1.00000 0.02989 0.03508 0.01828 -0.00072 0.00300 -0.00499 0.02851 0.00265 0.00012 0.00023 0.00010 0.00000 0.00077 0.00085 0.00069 0.00059 0.00057 0.00064 0.00036 Final Structure Factor Calculation for 2007NCS0623 in P2(1)/c Total number of l.s. parameters = 130 Maximum vector length = 511 Memory required = 1789 / 22995 wR2 = 0.1460 before cycle 21 for 2357 data and 0 / 130 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0396 * P )^2 + 1.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0617 for 1877 Fo > 4sig(Fo) and 0.0804 for all 2357 data wR2 = 0.1460, GooF = S = 1.049, Restrained GooF = 1.049 for all data Occupancy sum of asymmetric unit = 14.00 for non-hydrogen and 14.00 for hydrogen atoms Principal mean square atomic displacements U 0.0409 0.0248 0.0167 C1 0.0359 0.0231 0.0197 C2 0.0277 0.0201 0.0161 C3 0.0274 0.0181 0.0169 C4 0.0289 0.0272 0.0199 C5 0.0247 0.0203 0.0153 C6 0.0283 0.0194 0.0167 C7 0.0409 0.0348 0.0215 C8 0.0286 0.0262 0.0166 C9 0.0505 0.0324 0.0217 C10 0.0537 0.0278 0.0227 C11 0.0385 0.0302 0.0163 N1 0.0244 0.0234 0.0206 N2 0.0388 0.0289 0.0178 O1 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 0.026 0.036 0.047 0.059 0.075 0.102 0.150 1.000 Number in group 242. 230. 250. 235. 245. 224. 231. 233. 233. 234. GooF 1.043 1.140 1.076 1.043 1.108 0.974 1.022 1.012 0.984 1.067 K 3.912 1.619 1.124 1.007 1.029 1.007 1.005 1.003 1.007 0.998 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.65 inf Number in group 244. 231. 236. 233. 239. 236. 233. 234. 236. 235. GooF 0.985 1.140 1.110 1.067 0.971 0.901 0.916 0.941 1.102 1.294 K 1.032 1.077 1.054 1.042 1.021 1.002 0.983 0.986 1.028 0.995 R1 0.159 0.167 0.163 0.120 0.101 0.068 0.063 0.052 0.052 0.041 Recommended weighting scheme: WGHT 0.0391 1.2225 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 6 0 34.08 1.06 3.83 0.009 1.11 3 2 4 127.26 186.38 3.61 0.118 1.83 -13 4 5 41.92 15.40 3.56 0.034 0.80 -6 0 4 251.19 181.17 3.53 0.117 1.90 -1 4 1 7.33 24.46 3.41 0.043 1.65 -4 2 3 384.79 300.43 3.28 0.150 2.13 0 4 5 23.53 46.73 3.19 0.059 1.40 4 2 4 145.29 103.07 3.12 0.088 1.65 10 5 4 17.90 2.04 3.10 0.012 0.80 5 3 2 34.10 16.34 3.05 0.035 1.49 -6 6 10 7.01 23.41 3.05 0.042 0.83 6 0 2 448.83 358.04 3.01 0.164 1.71 10 5 1 15.25 0.13 2.91 0.003 0.86 -1 0 12 66.37 102.85 2.87 0.088 1.10 -8 7 3 3.02 17.85 2.87 0.037 0.80 0 1 7 898.30 759.60 2.86 0.239 1.78 7 3 9 76.68 45.36 2.85 0.058 0.88 9 0 8 31.41 12.64 2.76 0.031 0.89 -3 3 15 11.48 1.70 2.75 0.011 0.83 -13 2 6 52.40 29.15 2.75 0.047 0.88 -1 0 4 108.91 77.31 2.73 0.076 3.36 -5 7 2 18.49 5.34 2.69 0.020 0.89 -9 3 9 16.64 3.18 2.67 0.015 1.00 -11 3 8 13.08 2.89 2.67 0.015 0.92 -14 3 2 4.32 18.13 2.66 0.037 0.79 -6 3 3 81.88 51.68 2.66 0.062 1.47 2 1 7 6.75 0.87 2.65 0.008 1.58 1 0 6 96.81 67.84 2.63 0.071 2.01 0 3 1 287.27 231.53 2.61 0.132 2.20 -9 2 8 7.31 0.20 2.58 0.004 1.11 -10 1 13 12.98 28.45 2.56 0.046 0.88 -8 4 9 2.31 12.90 2.56 0.031 0.97 -14 0 6 49.47 20.00 2.56 0.039 0.85 2 3 6 44.10 26.54 2.54 0.045 1.42 0 2 6 159.25 122.26 2.54 0.096 1.81 3 5 2 29.82 51.37 2.52 0.062 1.22 0 2 8 195.17 153.26 2.50 0.107 1.45 8 2 0 175.88 136.44 2.48 0.101 1.32 -3 7 5 -3.72 4.07 2.48 0.017 0.89 4 1 11 9.94 0.03 2.46 0.002 0.98 -5 1 4 591.00 502.80 2.46 0.194 2.07 9 5 4 15.41 0.00 2.45 0.000 0.84 2 1 9 13.74 27.32 2.45 0.045 1.28 -7 1 5 685.57 585.13 2.44 0.210 1.56 1 8 1 -1.53 11.94 2.43 0.030 0.83 -11 6 3 82.00 54.71 2.43 0.064 0.78 10 3 5 15.09 4.40 2.41 0.018 0.88 3 1 12 96.39 68.14 2.40 0.072 0.96 -1 1 16 -2.95 3.33 2.40 0.016 0.81 4 1 1 371.68 441.69 2.39 0.182 2.46 Bond lengths and angles C1 - Distance Angles N1 1.3386 (0.0028) C2 1.3917 (0.0029) 125.18 (0.18) H1 0.9500 117.41 117.41 C1 - N1 C2 C2 - Distance Angles C3 1.3853 (0.0027) C1 1.3917 (0.0029) 116.05 (0.19) H2 0.9500 121.98 121.98 C2 - C3 C1 C3 - Distance Angles C2 1.3853 (0.0027) N2 1.3928 (0.0024) 129.50 (0.19) C4 1.3995 (0.0027) 120.74 (0.18) 109.76 (0.16) C3 - C2 N2 C4 - Distance Angles C5 1.3786 (0.0027) C3 1.3995 (0.0027) 118.04 (0.17) C6 1.5093 (0.0024) 133.18 (0.18) 108.76 (0.16) C4 - C5 C3 C5 - Distance Angles N1 1.3537 (0.0025) C4 1.3786 (0.0027) 122.99 (0.19) H5 0.9500 118.51 118.51 C5 - N1 C4 C6 - Distance Angles C4 1.5093 (0.0024) C7 1.5253 (0.0026) 101.92 (0.15) C9 1.5428 (0.0027) 118.63 (0.16) 109.69 (0.15) H6 1.0000 108.71 108.71 108.71 C6 - C4 C7 C9 C7 - Distance Angles O1 1.2168 (0.0022) N2 1.3768 (0.0025) 124.05 (0.18) C6 1.5253 (0.0026) 127.28 (0.18) 108.66 (0.15) C7 - O1 N2 C8 - Distance Angles N2 1.4534 (0.0025) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - N2 H8A H8B C9 - Distance Angles C11 1.5212 (0.0029) C10 1.5260 (0.0029) 112.02 (0.19) C6 1.5428 (0.0027) 112.36 (0.17) 111.83 (0.16) H9 1.0000 106.73 106.73 106.73 C9 - C11 C10 C6 C10 - Distance Angles C9 1.5260 (0.0029) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - C9 H10A H10B C11 - Distance Angles C9 1.5212 (0.0029) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - C9 H11A H11B N1 - Distance Angles C1 1.3386 (0.0028) C5 1.3537 (0.0025) 116.99 (0.18) N1 - C1 N2 - Distance Angles C7 1.3768 (0.0025) C3 1.3928 (0.0024) 110.88 (0.16) C8 1.4534 (0.0025) 122.61 (0.16) 126.51 (0.17) N2 - C7 C3 O1 - Distance Angles C7 1.2168 (0.0022) O1 - FMAP and GRID set by program FMAP 2 2 11 GRID -3.125 -2 -2 3.125 2 2 R1 = 0.0804 for 2357 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.26 at 0.6577 0.2328 0.4856 [ 0.98 A from H8A ] Deepest hole -0.32 at 0.5797 0.1972 0.9407 [ 0.15 A from H8B ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2114 / 17443 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3423 -0.2672 0.0144 1.00000 0.05 0.26 0.98 H8A 0.99 H8B 1.07 C8 1.96 H8C Q2 1 0.4341 -0.0644 0.0362 1.00000 0.05 0.26 0.92 H8B 0.97 H8C 0.99 C8 1.88 H8A Q3 1 0.3057 -0.0833 -0.0856 1.00000 0.05 0.23 0.90 H8A 1.19 H8C 1.23 C8 2.05 H8B Q4 1 0.1601 0.1076 0.0850 1.00000 0.05 0.22 0.72 C6 0.82 C7 1.45 H6 1.80 C4 Q5 1 0.1197 0.2446 0.1182 1.00000 0.05 0.21 0.77 C6 0.77 C9 1.44 H9 1.45 H6 Q6 1 0.1882 0.1204 0.1807 1.00000 0.05 0.21 0.75 C4 0.78 C6 1.40 H6 1.88 C3 Q7 1 0.1356 0.4323 0.1045 1.00000 0.05 0.20 0.71 C9 0.84 C10 1.35 H9 1.41 H10A Q8 1 0.2942 0.0615 0.2035 1.00000 0.05 0.19 0.70 C4 0.72 C3 1.77 C5 1.81 N2 Q9 1 0.2804 0.4970 0.1386 1.00000 0.05 0.19 0.68 H10C 0.99 C10 1.14 H10B 1.64 H10A Q10 1 0.2397 0.0557 0.2625 1.00000 0.05 0.18 0.67 C4 0.95 C5 1.59 H5 1.78 C3 Shortest distances between peaks (including symmetry equivalents) 8 10 1.16 4 5 1.18 6 10 1.18 4 6 1.24 6 8 1.28 5 7 1.29 5 6 1.30 1 2 1.72 7 9 1.72 1 3 1.78 2 3 1.91 4 8 1.94 4 7 2.22 2 2 2.24 6 7 2.33 4 10 2.33 5 8 2.41 5 10 2.42 5 9 2.51 1 9 2.55 6 9 2.87 4 9 2.96 Time profile in seconds ----------------------- 0.08: 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. 0.94: 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 2.77: Structure factors and derivatives 3.13: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.06: Apply other restraints 0.77: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007ncs0623 finished at 13:36:55 Total CPU time: 8.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++