+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 17:09:38 on 30-Mar-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh115 in C2/c CELL 0.71073 20.7183 12.6104 9.1726 90.000 109.300 90.000 ZERR 8.00 0.0007 0.0005 0.0003 0.000 0.002 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O F UNIT 104 80 16 8 16 V = 2261.81 F(000) = 1024.0 Mu = 0.12 mm-1 Cell Wt = 1985.84 Rho = 1.458 MERG 2 OMIT -3.00 55.00 OMIT -4 2 3 DFIX 0.88 0.02 N1 H1N N2 H2N EADP C1A C1B EADP C2A C2B EADP C3A C3B EADP C4A C4B EADP C5A C5B EADP C6A C6B FMAP 2 PLAN 5 SIZE 0.02 0.08 0.26 ACTA EQIV $1 x, -y+2, z+1/2 HTAB N2 O1_$1 HTAB N1 O1_$1 HTAB 2.00000 BOND $H LIST 6 L.S. 6 TEMP -153.00 WGHT 0.023700 5.065800 FVAR 0.40194 0.80020 C7 1 0.125749 0.986485 0.225277 11.00000 0.02252 0.02634 = 0.01793 0.00074 0.00615 -0.00410 C8 1 0.072393 1.163645 0.184530 11.00000 0.02533 0.02565 = 0.02285 0.00425 0.00938 0.00069 C9 1 0.088518 1.263241 0.250760 11.00000 0.03140 0.03034 = 0.02412 -0.00051 0.00496 0.00032 AFIX 43 H9 2 0.119429 1.271060 0.353012 11.00000 -1.20000 AFIX 0 C10 1 0.058612 1.350442 0.164623 11.00000 0.04284 0.02318 = 0.04032 -0.00163 0.01056 -0.00077 C11 1 0.013797 1.343904 0.015868 11.00000 0.03884 0.03018 = 0.03611 0.01040 0.00411 0.00438 AFIX 43 H11 2 -0.006033 1.405693 -0.040453 11.00000 -1.20000 AFIX 0 C12 1 -0.001216 1.244446 -0.048254 11.00000 0.02998 0.03794 = 0.02664 0.00628 0.00367 -0.00187 AFIX 43 H12 2 -0.031724 1.237509 -0.151067 11.00000 -1.20000 AFIX 0 C13 1 0.027338 1.154149 0.034349 11.00000 0.02845 0.02874 = 0.02574 0.00214 0.00571 -0.00421 AFIX 43 H13 2 0.016156 1.086102 -0.011505 11.00000 -1.20000 AFIX 0 N1 3 0.148306 0.909548 0.334699 11.00000 0.03455 0.02700 = 0.01608 0.00119 0.00993 0.00515 N2 3 0.100277 1.073414 0.275873 11.00000 0.03643 0.02801 = 0.01587 0.00256 0.01029 0.00479 O1 4 0.127574 0.978570 0.092584 11.00000 0.03706 0.02851 = 0.01614 -0.00045 0.01012 -0.00219 PART 1 C1A 1 0.172322 0.806181 0.316366 21.00000 0.01395 0.02626 = 0.01730 -0.00111 -0.00050 0.00131 C2A 1 0.199124 0.778666 0.200814 21.00000 0.02454 0.03415 = 0.02374 0.00177 0.00861 0.00799 AFIX 43 H2A 2 0.206151 0.830182 0.131991 21.00000 -1.20000 AFIX 0 C3A 1 0.215215 0.671853 0.190677 21.00000 0.02840 0.03198 = 0.02688 -0.00647 0.01284 0.00369 C4A 1 0.208856 0.594787 0.289866 21.00000 0.02628 0.02486 = 0.03595 -0.00100 0.00890 0.00209 AFIX 43 H4A 2 0.221768 0.523476 0.280596 21.00000 -1.20000 AFIX 0 C5A 1 0.182548 0.625399 0.405478 21.00000 0.02402 0.03254 = 0.02729 0.00581 0.00692 0.00143 AFIX 43 H5A 2 0.176460 0.573834 0.475315 21.00000 -1.20000 AFIX 0 C6A 1 0.165408 0.729177 0.419214 21.00000 0.02470 0.02806 = 0.01711 0.00002 0.00227 0.00103 AFIX 43 H6A 2 0.148587 0.748803 0.499999 21.00000 -1.20000 AFIX 0 F1A 5 0.241168 0.647243 0.075940 21.00000 0.05496 0.04580 = 0.04094 -0.00405 0.02991 0.01361 PART 2 SAME C1A > F1A C1B 1 0.160713 0.805398 0.301656 -21.00000 0.01395 0.02626 = 0.01730 -0.00111 -0.00050 0.00131 C2B 1 0.159316 0.724352 0.402942 -21.00000 0.02454 0.03415 = 0.02374 0.00177 0.00861 0.00799 AFIX 43 H2B 2 0.137246 0.734031 0.477768 -21.00000 -1.20000 AFIX 0 C3B 1 0.191553 0.626704 0.392377 -21.00000 0.02840 0.03198 = 0.02688 -0.00647 0.01284 0.00369 C4B 1 0.219351 0.608041 0.280628 -21.00000 0.02628 0.02486 = 0.03595 -0.00100 0.00890 0.00209 AFIX 43 H4B 2 0.235796 0.539805 0.266497 -21.00000 -1.20000 AFIX 0 C5B 1 0.222764 0.693309 0.187332 -21.00000 0.02402 0.03254 = 0.02729 0.00581 0.00692 0.00143 AFIX 43 H5B 2 0.247892 0.685152 0.118164 -21.00000 -1.20000 AFIX 0 C6B 1 0.191823 0.787557 0.190705 -21.00000 0.02470 0.02806 = 0.01711 0.00002 0.00227 0.00103 AFIX 43 H6B 2 0.191385 0.841179 0.117638 -21.00000 -1.20000 AFIX 0 F1B 5 0.181900 0.555835 0.495415 -21.00000 0.06244 0.03048 = 0.05117 0.01573 0.01581 0.01072 PART 0 F2 5 0.073876 1.447407 0.231174 11.00000 0.07142 0.02620 = 0.05459 -0.00207 -0.00044 0.00028 H2N 2 0.107243 1.079033 0.374064 11.00000 0.03270 H1N 2 0.143582 0.924213 0.423871 11.00000 0.04396 HKLF 4 Covalent radii and connectivity table for 2008lsh115 in C2/c C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 C7 - O1 N1 N2 C8 - C9 C13 N2 C9 - C10 C8 C10 - F2 C11 C9 C11 - C10 C12 C12 - C11 C13 C13 - C12 C8 N1 - C7 C1B_b C1A_a N2 - C7 C8 O1 - C7 C1A_a - C2A_a C6A_a N1 C2A_a - C1A_a C3A_a C3A_a - F1A_a C4A_a C2A_a C4A_a - C3A_a C5A_a C5A_a - C6A_a C4A_a C6A_a - C5A_a C1A_a F1A_a - C3A_a C1B_b - C2B_b N1 C6B_b C2B_b - C1B_b C3B_b C3B_b - C4B_b F1B_b C2B_b C4B_b - C3B_b C5B_b C5B_b - C6B_b C4B_b C6B_b - C5B_b C1B_b F1B_b - C3B_b F2 - C10 Operators for generating equivalent atoms: $1 x, -y+2, z+1/2 13699 Reflections read, of which 400 rejected -25 =< h =< 26, -16 =< k =< 16, -11 =< l =< 11, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 2586 Unique reflections, of which 0 suppressed R(int) = 0.0516 R(sigma) = 0.0416 Friedel opposites merged Maximum memory for data reduction = 2259 / 30745 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 = 2839 / 247693 wR2 = 0.1270 before cycle 1 for 2586 data and 199 / 199 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 15. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.010 0.000 0.029 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.106; Restrained GooF = 1.105 for 17 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0237 * P )^2 + 5.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40194 0.00097 0.002 OSF 2 0.80019 0.00420 -0.002 FVAR 2 Mean shift/esd = 0.003 Maximum = -0.017 for y C3B_b Max. shift = 0.001 A for C3B_b Max. dU = 0.000 for C5A_a Least-squares cycle 2 Maximum vector length = 511 Memory required = 2839 / 247693 wR2 = 0.1270 before cycle 2 for 2586 data and 199 / 199 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 15. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.010 0.000 0.029 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.106; Restrained GooF = 1.105 for 17 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0237 * P )^2 + 5.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40194 0.00097 0.000 OSF 2 0.80019 0.00420 -0.002 FVAR 2 Mean shift/esd = 0.003 Maximum = -0.021 for y C3B_b Max. shift = 0.001 A for C3B_b Max. dU = 0.000 for C5A_a Least-squares cycle 3 Maximum vector length = 511 Memory required = 2839 / 247693 wR2 = 0.1270 before cycle 3 for 2586 data and 199 / 199 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 15. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.010 0.000 0.029 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.107; Restrained GooF = 1.105 for 17 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0237 * P )^2 + 5.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40194 0.00097 -0.001 OSF 2 0.80018 0.00420 -0.001 FVAR 2 Mean shift/esd = 0.002 Maximum = -0.018 for y C3B_b Max. shift = 0.001 A for C3B_b Max. dU = 0.000 for C5A_a Least-squares cycle 4 Maximum vector length = 511 Memory required = 2839 / 247693 wR2 = 0.1270 before cycle 4 for 2586 data and 199 / 199 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 15. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.010 0.000 0.029 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.107; Restrained GooF = 1.105 for 17 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0237 * P )^2 + 5.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40194 0.00097 0.000 OSF 2 0.80018 0.00420 -0.001 FVAR 2 Mean shift/esd = 0.002 Maximum = -0.015 for y C3B_b Max. shift = 0.001 A for C3B_b Max. dU = 0.000 for C5A_a Least-squares cycle 5 Maximum vector length = 511 Memory required = 2839 / 247693 wR2 = 0.1270 before cycle 5 for 2586 data and 199 / 199 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 15. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.010 0.000 0.029 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.107; Restrained GooF = 1.105 for 17 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0237 * P )^2 + 5.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40194 0.00097 0.000 OSF 2 0.80017 0.00420 -0.001 FVAR 2 Mean shift/esd = 0.002 Maximum = -0.013 for y C3B_b Max. shift = 0.001 A for C3B_b Max. dU = 0.000 for C5A_a Least-squares cycle 6 Maximum vector length = 511 Memory required = 2839 / 247693 wR2 = 0.1270 before cycle 6 for 2586 data and 199 / 199 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 15. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.010 0.000 0.029 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.106; Restrained GooF = 1.105 for 17 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0237 * P )^2 + 5.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40194 0.00097 0.000 OSF 2 0.80017 0.00420 -0.001 FVAR 2 Mean shift/esd = 0.001 Maximum = -0.011 for y C3B_b Max. shift = 0.000 A for C3B_b Max. dU = 0.000 for C5A_a Largest correlation matrix elements -0.958 z C6B_b / z C2A_a -0.920 z C3B_b / z C5A_a -0.885 y C3B_b / y C5A_a -0.946 z C1B_b / z C1A_a -0.914 z C2B_b / z C6A_a -0.884 U11 C1A_a / x C1A_a -0.946 x C6B_b / x C2A_a -0.913 x C3B_b / x C5A_a 0.884 x C6B_b / U11 C2A_a 0.941 x C1B_b / U11 C1A_a -0.913 x C4B_b / x C4A_a -0.882 x C3B_b / U11 C5A_a -0.940 z C4B_b / z C4A_a -0.910 x C4B_b / U11 C4A_a 0.881 z C1B_b / U33 C1A_a -0.939 x C2B_b / x C6A_a -0.904 x C1B_b / x C1A_a 0.876 z C1B_b / U13 C1A_a -0.923 y C6B_b / y C2A_a -0.893 y C2B_b / y C6A_a -0.868 x C5B_b / x C3A_a -0.920 y C1B_b / y C1A_a -0.885 z C5B_b / z C3A_a 0.859 U11 C4A_a / x C4A_a Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H9 0.1194 1.2711 0.3530 43 0.950 0.000 C9 C10 C8 H11 -0.0060 1.4057 -0.0405 43 0.950 0.000 C11 C10 C12 H12 -0.0317 1.2375 -0.1511 43 0.950 0.000 C12 C11 C13 H13 0.0162 1.0861 -0.0115 43 0.950 0.000 C13 C12 C8 H2A 0.2061 0.8302 0.1319 43 0.950 0.000 C2A_a C1A_a C3A_a H4A 0.2217 0.5235 0.2806 43 0.950 0.000 C4A_a C3A_a C5A_a H5A 0.1765 0.5739 0.4754 43 0.950 0.000 C5A_a C6A_a C4A_a H6A 0.1486 0.7488 0.5000 43 0.950 0.000 C6A_a C5A_a C1A_a H2B 0.1374 0.7338 0.4780 43 0.950 0.000 C2B_b C1B_b C3B_b H4B 0.2359 0.5398 0.2665 43 0.950 0.000 C4B_b C3B_b C5B_b H5B 0.2478 0.6852 0.1178 43 0.950 0.000 C5B_b C6B_b C4B_b H6B 0.1915 0.8413 0.1179 43 0.950 0.000 C6B_b C5B_b C1B_b 2008lsh115 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C7 0.12575 0.98648 0.22528 1.00000 0.02252 0.02634 0.01793 0.00074 0.00615 -0.00410 0.02239 0.00392 0.00010 0.00017 0.00022 0.00000 0.00100 0.00107 0.00094 0.00081 0.00075 0.00082 0.00043 C8 0.07239 1.16365 0.18453 1.00000 0.02533 0.02565 0.02285 0.00425 0.00938 0.00069 0.02426 0.00420 0.00010 0.00017 0.00023 0.00000 0.00103 0.00109 0.00100 0.00085 0.00081 0.00086 0.00044 C9 0.08852 1.26324 0.25076 1.00000 0.03140 0.03034 0.02412 -0.00051 0.00496 0.00032 0.02966 0.00442 0.00012 0.00018 0.00025 0.00000 0.00114 0.00122 0.00106 0.00090 0.00087 0.00094 0.00049 H9 0.11943 1.27106 0.35301 1.00000 0.03560 0.00000 0.00000 C10 0.05861 1.35044 0.16462 1.00000 0.04284 0.02318 0.04032 -0.00163 0.01056 -0.00077 0.03623 0.00483 0.00013 0.00018 0.00029 0.00000 0.00138 0.00118 0.00135 0.00099 0.00108 0.00101 0.00056 C11 0.01380 1.34390 0.01587 1.00000 0.03884 0.03018 0.03611 0.01040 0.00411 0.00438 0.03709 0.00494 0.00013 0.00020 0.00028 0.00000 0.00132 0.00128 0.00130 0.00101 0.00104 0.00103 0.00057 H11 -0.00603 1.40569 -0.04045 1.00000 0.04451 0.00000 0.00000 C12 -0.00122 1.24445 -0.04825 1.00000 0.02998 0.03794 0.02664 0.00628 0.00367 -0.00187 0.03292 0.00465 0.00012 0.00019 0.00026 0.00000 0.00116 0.00133 0.00111 0.00098 0.00090 0.00099 0.00053 H12 -0.03172 1.23751 -0.15107 1.00000 0.03951 0.00000 0.00000 C13 0.02734 1.15415 0.03435 1.00000 0.02845 0.02874 0.02574 0.00214 0.00571 -0.00421 0.02845 0.00432 0.00011 0.00018 0.00025 0.00000 0.00111 0.00117 0.00106 0.00089 0.00086 0.00092 0.00048 H13 0.01616 1.08610 -0.01151 1.00000 0.03414 0.00000 0.00000 N1 0.14831 0.90955 0.33470 1.00000 0.03455 0.02700 0.01608 0.00119 0.00993 0.00516 0.02549 0.00368 0.00010 0.00015 0.00020 0.00000 0.00099 0.00097 0.00083 0.00071 0.00072 0.00077 0.00040 N2 0.10028 1.07341 0.27587 1.00000 0.03643 0.02801 0.01587 0.00256 0.01029 0.00479 0.02636 0.00370 0.00010 0.00015 0.00020 0.00000 0.00104 0.00098 0.00084 0.00073 0.00075 0.00079 0.00041 O1 0.12757 0.97857 0.09258 1.00000 0.03706 0.02851 0.01614 -0.00045 0.01012 -0.00219 0.02691 0.00288 0.00008 0.00012 0.00015 0.00000 0.00086 0.00079 0.00070 0.00059 0.00060 0.00066 0.00035 C1A_a 0.17232 0.80620 0.31636 0.80017 0.01393 0.02626 0.01732 -0.00114 -0.00049 0.00125 0.02057 0.01440 0.00032 0.00052 0.00093 0.00420 0.00301 0.00110 0.00205 0.00108 0.00216 0.00150 0.00111 C2A_a 0.19912 0.77866 0.20080 0.80017 0.02456 0.03416 0.02375 0.00178 0.00864 0.00799 0.02733 0.02397 0.00047 0.00070 0.00112 0.00420 0.00302 0.00260 0.00218 0.00154 0.00226 0.00164 0.00111 H2A_a 0.20613 0.83016 0.13194 0.80017 0.03279 0.00420 0.00000 C3A_a 0.21523 0.67185 0.19071 0.80017 0.02846 0.03195 0.02689 -0.00638 0.01287 0.00375 0.02818 0.01075 0.00031 0.00032 0.00069 0.00420 0.00218 0.00256 0.00148 0.00201 0.00135 0.00186 0.00102 C4A_a 0.20885 0.59480 0.28989 0.80017 0.02626 0.02490 0.03591 -0.00099 0.00894 0.00210 0.02935 0.01661 0.00037 0.00042 0.00098 0.00420 0.00303 0.00193 0.00172 0.00146 0.00147 0.00176 0.00099 H4A_a 0.22174 0.52348 0.28060 0.80017 0.03522 0.00420 0.00000 C5A_a 0.18256 0.62544 0.40554 0.80017 0.02412 0.03257 0.02712 0.00573 0.00698 0.00152 0.02830 0.01786 0.00036 0.00050 0.00084 0.00420 0.00281 0.00155 0.00220 0.00144 0.00127 0.00149 0.00099 H5A_a 0.17651 0.57390 0.47545 0.80017 0.03396 0.00420 0.00000 C6A_a 0.16540 0.72921 0.41921 0.80017 0.02473 0.02799 0.01713 -0.00005 0.00230 0.00099 0.02442 0.01414 0.00043 0.00050 0.00079 0.00420 0.00234 0.00172 0.00214 0.00137 0.00183 0.00142 0.00109 H6A_a 0.14855 0.74885 0.49995 0.80017 0.02931 0.00420 0.00000 F1A_a 0.24117 0.64724 0.07594 0.80017 0.05497 0.04579 0.04095 -0.00404 0.02992 0.01361 0.04376 0.00394 0.00010 0.00015 0.00021 0.00420 0.00121 0.00119 0.00109 0.00083 0.00090 0.00089 0.00062 C1B_b 0.16070 0.80529 0.30170 0.19983 0.01393 0.02626 0.01732 -0.00114 -0.00049 0.00125 0.02057 0.07681 0.00180 0.00225 0.00436 0.00420 0.00301 0.00110 0.00205 0.00108 0.00216 0.00150 0.00111 C2B_b 0.15935 0.72418 0.40295 0.19983 0.02456 0.03416 0.02375 0.00178 0.00864 0.00799 0.02733 0.07896 0.00205 0.00222 0.00403 0.00420 0.00302 0.00260 0.00218 0.00154 0.00226 0.00164 0.00111 H2B_b 0.13737 0.73384 0.47796 0.19983 0.03279 0.00420 0.00000 C3B_b 0.19148 0.62650 0.39206 0.19983 0.02846 0.03195 0.02689 -0.00638 0.01287 0.00375 0.02818 0.08409 0.00193 0.00211 0.00376 0.00420 0.00218 0.00256 0.00148 0.00201 0.00135 0.00186 0.00102 C4B_b 0.21937 0.60800 0.28051 0.19983 0.02626 0.02490 0.03591 -0.00099 0.00894 0.00210 0.02935 0.08133 0.00189 0.00200 0.00429 0.00420 0.00303 0.00193 0.00172 0.00146 0.00147 0.00176 0.00099 H4B_b 0.23593 0.53983 0.26646 0.19983 0.03522 0.00420 0.00000 C5B_b 0.22271 0.69331 0.18719 0.19983 0.02412 0.03257 0.02712 0.00573 0.00698 0.00152 0.02830 0.05644 0.00151 0.00191 0.00328 0.00420 0.00281 0.00155 0.00220 0.00144 0.00127 0.00149 0.00099 H5B_b 0.24775 0.68516 0.11785 0.19983 0.03396 0.00420 0.00000 C6B_b 0.19184 0.78758 0.19078 0.19983 0.02473 0.02799 0.01713 -0.00005 0.00230 0.00099 0.02442 0.09840 0.00217 0.00279 0.00470 0.00420 0.00234 0.00172 0.00214 0.00137 0.00183 0.00142 0.00109 H6B_b 0.19147 0.84129 0.11788 0.19983 0.02931 0.00420 0.00000 F1B_b 0.18189 0.55581 0.49539 0.19983 0.06251 0.03043 0.05125 0.01574 0.01586 0.01070 0.04879 0.01685 0.00042 0.00058 0.00091 0.00420 0.00536 0.00421 0.00496 0.00348 0.00394 0.00352 0.00259 F2 0.07388 1.44741 0.23117 1.00000 0.07142 0.02620 0.05458 -0.00207 -0.00044 0.00028 0.05600 0.00309 0.00009 0.00012 0.00019 0.00000 0.00116 0.00080 0.00100 0.00068 0.00083 0.00073 0.00048 H2N 0.10724 1.07903 0.37406 1.00000 0.03269 0.04318 0.00124 0.00194 0.00197 0.00000 0.00655 H1N 0.14358 0.92421 0.42387 1.00000 0.04394 0.04941 0.00138 0.00211 0.00228 0.00000 0.00761 Final Structure Factor Calculation for 2008lsh115 in C2/c Total number of l.s. parameters = 199 Maximum vector length = 511 Memory required = 2640 / 24017 wR2 = 0.1270 before cycle 7 for 2586 data and 0 / 199 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 15. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.010 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.107; Restrained GooF = 1.105 for 17 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0237 * P )^2 + 5.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0595 for 1993 Fo > 4sig(Fo) and 0.0835 for all 2586 data wR2 = 0.1270, GooF = S = 1.107, Restrained GooF = 1.105 for all data Occupancy sum of asymmetric unit = 18.00 for non-hydrogen and 10.00 for hydrogen atoms Principal mean square atomic displacements U 0.0296 0.0199 0.0177 C7 0.0288 0.0250 0.0190 C8 0.0355 0.0303 0.0232 C9 0.0466 0.0391 0.0230 C10 0.0512 0.0393 0.0208 C11 0.0445 0.0316 0.0227 C12 0.0364 0.0247 0.0243 C13 0.0373 0.0244 0.0148 N1 0.0387 0.0261 0.0143 N2 0.0378 0.0280 0.0149 O1 0.0276 0.0230 0.0111 C1A_a 0.0387 0.0235 0.0198 C2A_a 0.0372 0.0305 0.0168 C3A_a 0.0372 0.0277 0.0232 C4A_a 0.0364 0.0260 0.0225 C5A_a 0.0298 0.0274 0.0161 C6A_a 0.0656 0.0476 0.0181 F1A_a 0.0276 0.0230 0.0111 C1B_b 0.0387 0.0235 0.0198 C2B_b 0.0372 0.0305 0.0168 C3B_b 0.0372 0.0277 0.0232 C4B_b 0.0364 0.0260 0.0225 C5B_b 0.0298 0.0274 0.0161 C6B_b 0.0659 0.0592 0.0212 F1B_b 0.0964 0.0455 0.0260 F2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.017 0.026 0.035 0.045 0.059 0.076 0.103 0.149 1.000 Number in group 275. 249. 259. 266. 247. 266. 255. 250. 260. 259. GooF 1.256 1.168 1.200 1.049 1.083 1.179 1.110 0.963 0.906 1.092 K 6.311 1.319 1.101 1.043 0.989 0.992 0.993 0.997 1.009 0.999 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.66 inf Number in group 265. 256. 257. 260. 256. 258. 261. 254. 259. 260. GooF 1.212 1.328 1.199 1.215 0.968 0.980 0.901 0.847 0.980 1.302 K 1.123 1.132 1.042 1.008 1.008 0.986 0.993 1.003 1.031 0.990 R1 0.234 0.249 0.173 0.156 0.092 0.071 0.045 0.040 0.044 0.035 Recommended weighting scheme: WGHT 0.0179 4.9908 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) -5 13 6 141.41 31.93 3.67 0.022 0.82 16 4 6 77.87 0.56 3.37 0.003 0.78 7 3 3 211.09 360.10 3.34 0.074 1.61 2 6 1 106.57 223.43 3.33 0.058 1.97 8 6 8 68.92 1.17 3.27 0.004 0.82 1 1 1 5942.29 6880.87 3.22 0.324 6.18 -5 7 9 129.92 35.97 3.22 0.023 0.88 3 15 2 389.13 231.10 3.00 0.059 0.81 -5 1 4 3327.49 2837.98 2.96 0.208 2.20 3 15 1 614.74 388.03 2.95 0.077 0.83 9 11 6 -30.14 51.52 2.94 0.028 0.78 -21 1 9 52.53 2.68 2.94 0.006 0.82 15 9 4 291.05 143.57 2.93 0.047 0.80 1 5 1 505.70 692.82 2.90 0.103 2.38 -23 1 7 612.01 851.27 2.88 0.114 0.84 -2 14 3 62.16 3.49 2.87 0.007 0.86 -12 0 6 395.61 254.39 2.86 0.062 1.32 0 4 0 298.84 448.07 2.85 0.083 3.15 -1 13 4 67.81 9.91 2.85 0.012 0.89 -3 1 1 5847.01 6631.90 2.84 0.318 5.64 -15 9 8 84.49 0.29 2.82 0.002 0.82 11 3 8 948.27 706.09 2.79 0.104 0.80 -20 8 3 389.50 232.42 2.78 0.060 0.87 6 8 7 149.32 51.10 2.76 0.028 0.87 -1 7 10 157.76 46.43 2.76 0.027 0.79 -3 11 8 59.67 0.24 2.75 0.002 0.80 5 5 1 3380.28 2912.98 2.75 0.211 1.98 -16 0 10 192.63 332.70 2.74 0.071 0.85 11 1 5 268.71 160.84 2.73 0.050 1.07 -3 5 3 2763.35 2367.54 2.69 0.190 1.94 -4 10 7 6.63 72.93 2.66 0.033 0.91 2 2 10 235.61 362.67 2.61 0.074 0.83 23 3 1 59.90 1.09 2.59 0.004 0.80 1 3 8 319.47 463.12 2.59 0.084 1.03 -25 1 6 168.11 5.40 2.58 0.009 0.81 0 2 2 2916.32 3348.21 2.56 0.226 3.57 -12 10 6 325.12 466.09 2.55 0.084 0.91 2 12 4 48.89 2.59 2.53 0.006 0.93 14 10 2 129.73 244.32 2.51 0.061 0.88 20 6 1 376.11 248.49 2.50 0.062 0.86 -1 7 9 178.48 76.95 2.49 0.034 0.86 -6 0 6 9605.03 8571.75 2.48 0.362 1.52 6 14 4 72.92 4.43 2.46 0.008 0.78 12 2 4 25.84 78.11 2.45 0.035 1.12 11 1 6 48.79 7.21 2.44 0.010 0.97 -4 10 1 61.95 12.20 2.43 0.014 1.22 -21 9 2 251.46 135.29 2.42 0.045 0.80 -9 13 1 65.38 148.56 2.41 0.048 0.89 -12 14 1 224.74 118.30 2.41 0.043 0.80 -5 15 2 77.62 9.49 2.41 0.012 0.82 Bond lengths and angles C7 - Distance Angles O1 1.2342 (0.0023) N1 1.3627 (0.0026) 123.64 (0.19) N2 1.3629 (0.0027) 122.85 (0.19) 113.51 (0.17) C7 - O1 N1 C8 - Distance Angles C9 1.3870 (0.0031) C13 1.3904 (0.0029) 119.84 (0.20) N2 1.4179 (0.0027) 118.41 (0.19) 121.69 (0.19) C8 - C9 C13 C9 - Distance Angles C10 1.3761 (0.0032) C8 1.3870 (0.0030) 118.33 (0.20) H9 0.9500 120.84 120.84 C9 - C10 C8 C10 - Distance Angles F2 1.3565 (0.0027) C11 1.3759 (0.0034) 118.74 (0.21) C9 1.3761 (0.0032) 117.91 (0.21) 123.35 (0.22) C10 - F2 C11 C11 - Distance Angles C10 1.3759 (0.0034) C12 1.3765 (0.0034) 117.48 (0.21) H11 0.9500 121.26 121.26 C11 - C10 C12 C12 - Distance Angles C11 1.3765 (0.0034) C13 1.3872 (0.0032) 121.28 (0.21) H12 0.9500 119.36 119.36 C12 - C11 C13 C13 - Distance Angles C12 1.3872 (0.0032) C8 1.3904 (0.0029) 119.73 (0.21) H13 0.9500 120.14 120.14 C13 - C12 C8 N1 - Distance Angles C7 1.3627 (0.0026) C1B_b 1.3919 (0.0279) 123.73 (1.51) C1A_a 1.4247 (0.0065) 127.77 (0.37) 9.44 (1.77) H1N 0.8750 (0.0168) 114.89 (1.80) 119.24 (2.35) 117.07 (1.83) N1 - C7 C1B_b C1A_a N2 - Distance Angles C7 1.3629 (0.0027) C8 1.4179 (0.0027) 124.91 (0.17) H2N 0.8667 (0.0162) 118.00 (1.66) 116.35 (1.66) N2 - C7 C8 O1 - Distance Angles C7 1.2342 (0.0023) O1 - C1A_a - Distance Angles C2A_a 1.3934 (0.0064) C6A_a 1.3938 (0.0061) 119.82 (0.48) N1 1.4247 (0.0065) 124.09 (0.57) 116.05 (0.58) C1A_a - C2A_a C6A_a C2A_a - Distance Angles C1A_a 1.3934 (0.0064) C3A_a 1.3980 (0.0070) 117.02 (0.58) H2A_a 0.9500 121.49 121.49 C2A_a - C1A_a C3A_a C3A_a - Distance Angles F1A_a 1.3665 (0.0057) C4A_a 1.3669 (0.0059) 120.02 (0.39) C2A_a 1.3980 (0.0070) 115.66 (0.45) 124.27 (0.50) C3A_a - F1A_a C4A_a C4A_a - Distance Angles C3A_a 1.3669 (0.0059) C5A_a 1.3977 (0.0060) 117.14 (0.39) H4A_a 0.9500 121.43 121.43 C4A_a - C3A_a C5A_a C5A_a - Distance Angles C6A_a 1.3726 (0.0062) C4A_a 1.3977 (0.0060) 120.71 (0.46) H5A_a 0.9500 119.65 119.65 C5A_a - C6A_a C4A_a C6A_a - Distance Angles C5A_a 1.3726 (0.0062) C1A_a 1.3938 (0.0062) 120.97 (0.54) H6A_a 0.9500 119.52 119.52 C6A_a - C5A_a C1A_a F1A_a - Distance Angles C3A_a 1.3665 (0.0058) F1A_a - C1B_b - Distance Angles C2B_b 1.3881 (0.0208) N1 1.3919 (0.0279) 120.30 (2.55) C6B_b 1.3911 (0.0212) 119.20 (1.90) 118.31 (2.57) C1B_b - C2B_b N1 C2B_b - Distance Angles C1B_b 1.3881 (0.0208) C3B_b 1.4194 (0.0198) 118.60 (2.15) H2B_b 0.9500 120.69 120.71 C2B_b - C1B_b C3B_b C3B_b - Distance Angles C4B_b 1.3512 (0.0191) F1B_b 1.3627 (0.0179) 127.65 (1.85) C2B_b 1.4194 (0.0198) 122.08 (1.92) 109.82 (1.86) C3B_b - C4B_b F1B_b C4B_b - Distance Angles C3B_b 1.3512 (0.0191) C5B_b 1.3907 (0.0183) 116.95 (1.73) H4B_b 0.9500 121.52 121.53 C4B_b - C3B_b C5B_b C5B_b - Distance Angles C6B_b 1.3554 (0.0193) C4B_b 1.3907 (0.0183) 122.93 (2.29) H5B_b 0.9500 118.54 118.53 C5B_b - C6B_b C4B_b C6B_b - Distance Angles C5B_b 1.3554 (0.0193) C1B_b 1.3911 (0.0212) 119.68 (2.29) H6B_b 0.9500 120.15 120.16 C6B_b - C5B_b C1B_b F1B_b - Distance Angles C3B_b 1.3627 (0.0179) F1B_b - F2 - Distance Angles C10 1.3565 (0.0027) F2 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.867(16) 2.041(18) 2.847(2) 154(2) N2-H2N...O1_$1 0.875(17) 2.085(19) 2.906(2) 156(2) N1-H1N...O1_$1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)