+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 21:09:58 on 11-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009lsh069 in I4(1)cd CELL 0.71073 16.2982 16.2982 17.0833 90.000 90.000 90.000 ZERR 16.00 0.0006 0.0006 0.0006 0.000 0.000 0.000 LATT -2 SYMM 1/2 - X, 1/2 - Y, 1/2 + Z SYMM - Y, 1/2 + X, 1/4 + Z SYMM 1/2 + Y, - X, 3/4 + Z SYMM X, - Y, 1/2 + Z SYMM 1/2 - X, 1/2 + Y, Z SYMM - Y, 1/2 - X, 3/4 + Z SYMM 1/2 + Y, X, 1/4 + Z SFAC C H N O UNIT 192 272 16 16 V = 4537.86 F(000) = 1664.0 Mu = 0.07 mm-1 Cell Wt = 3060.26 Rho = 1.120 MERG 2 OMIT -3.00 55.00 OMIT 0 0 -4 TWIN EQIV $1 y+1, -x+5/2, z+1/4 HTAB N1 O1_$1 HTAB DFIX 0.88 0.02 N1 H1N FMAP 2 PLAN 5 SIZE 0.02 0.04 0.90 ACTA BOND $H L.S. 6 TEMP -153.00 WGHT 0.0520 1.7854 EXTI 0.006769 BASF 1.96970 FVAR 0.42875 C1 1 1.699512 0.770326 1.770329 11.00000 0.02716 0.02826 = 0.02836 0.00056 -0.00016 0.00065 C2 1 1.625873 0.738313 1.740009 11.00000 0.02625 0.02702 = 0.03147 0.00118 0.00392 0.00182 C3 1 1.572706 0.796378 1.704591 11.00000 0.02600 0.03569 = 0.03496 -0.00017 -0.00166 0.00199 AFIX 43 H3 2 1.522023 0.777978 1.683466 11.00000 -1.20000 AFIX 0 C4 1 1.592011 0.878542 1.699758 11.00000 0.03534 0.03081 = 0.04237 0.00512 -0.00064 0.00695 AFIX 43 H4 2 1.554207 0.915579 1.676454 11.00000 -1.20000 AFIX 0 C5 1 1.665486 0.907546 1.728330 11.00000 0.03940 0.02886 = 0.04265 0.00281 0.00023 -0.00166 AFIX 43 H5 2 1.679397 0.963931 1.723583 11.00000 -1.20000 AFIX 0 C6 1 1.718676 0.853029 1.764086 11.00000 0.02857 0.03101 = 0.03306 -0.00043 0.00014 -0.00372 AFIX 43 H6 2 1.769169 0.872539 1.784711 11.00000 -1.20000 AFIX 0 C7 1 1.833865 0.707572 1.779838 11.00000 0.02495 0.02584 = 0.03412 -0.00304 0.00005 -0.00235 C8 1 1.893553 0.661072 1.829825 11.00000 0.03389 0.03895 = 0.03153 0.00644 0.00027 0.00251 AFIX 137 H8A 2 1.943601 0.693637 1.836591 11.00000 -1.50000 H8B 2 1.907186 0.608908 1.804429 11.00000 -1.50000 H8C 2 1.868870 0.650292 1.881114 11.00000 -1.50000 AFIX 0 C9 1 1.601029 0.647337 1.744181 11.00000 0.02720 0.02757 = 0.03632 -0.00144 0.00226 -0.00185 C10 1 1.582886 0.623708 1.829447 11.00000 0.04623 0.03520 = 0.04157 0.00294 0.00461 -0.00966 AFIX 137 H10A 2 1.540831 0.660443 1.850724 11.00000 -1.50000 H10B 2 1.633149 0.628631 1.860580 11.00000 -1.50000 H10C 2 1.563097 0.566967 1.831458 11.00000 -1.50000 AFIX 0 C11 1 1.522416 0.631030 1.696900 11.00000 0.03730 0.03257 = 0.05476 -0.00238 -0.00520 -0.00270 AFIX 137 H11A 2 1.530831 0.647965 1.642445 11.00000 -1.50000 H11B 2 1.476912 0.662380 1.719519 11.00000 -1.50000 H11C 2 1.509407 0.572352 1.698605 11.00000 -1.50000 AFIX 0 C12 1 1.667537 0.590848 1.709587 11.00000 0.03650 0.03103 = 0.05337 -0.00679 0.00549 -0.00145 AFIX 137 H12A 2 1.718438 0.597097 1.739538 11.00000 -1.50000 H12B 2 1.677423 0.605801 1.654830 11.00000 -1.50000 H12C 2 1.649070 0.533699 1.712381 11.00000 -1.50000 AFIX 0 N1 3 1.759111 0.719860 1.809587 11.00000 0.02587 0.03201 = 0.03072 0.00378 0.00078 -0.00198 O1 4 1.853945 0.732655 1.713977 11.00000 0.02848 0.04004 = 0.03024 0.00487 0.00102 -0.00111 H1N 2 1.745819 0.699305 1.854948 11.00000 0.04213 HKLF 4 Covalent radii and connectivity table for 2009lsh069 in I4(1)cd C 0.770 H 0.320 N 0.700 O 0.660 C1 - C6 C2 N1 C2 - C1 C3 C9 C3 - C4 C2 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 C9 - C10 C11 C2 C12 C10 - C9 C11 - C9 C12 - C9 N1 - C7 C1 O1 - C7 Operators for generating equivalent atoms: $1 y+1, -x+5/2, z+1/4 Floating origin restraints generated 16398 Reflections read, of which 1031 rejected -21 =< h =< 20, -21 =< k =< 19, -20 =< l =< 21, Max. 2-theta = 54.91 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 3 13 12 18.17 7.81 6 57.48 6 11 13 19.36 6.64 5 90.77 2 Inconsistent equivalents 2520 Unique reflections, of which 0 suppressed R(int) = 0.1300 R(sigma) = 0.1026 Friedel opposites not merged Maximum memory for data reduction = 1767 / 33784 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 = 2171 / 172736 wR2 = 0.1393 before cycle 1 for 2520 data and 137 / 137 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.020; Restrained GooF = 1.019 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0520 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.42868 0.00152 -0.043 OSF 2 1.97563 2.47663 0.002 BASF 1 3 0.00674 0.00080 -0.031 EXTI Mean shift/esd = 0.010 Maximum = -0.043 for OSF Max. shift = 0.001 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 2171 / 172736 wR2 = 0.1392 before cycle 2 for 2520 data and 137 / 137 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.020; Restrained GooF = 1.019 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0520 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.42865 0.00152 -0.023 OSF 2 1.97878 2.47621 0.001 BASF 1 3 0.00673 0.00080 -0.014 EXTI Mean shift/esd = 0.004 Maximum = -0.023 for OSF Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 3 Maximum vector length = 511 Memory required = 2171 / 172736 wR2 = 0.1393 before cycle 3 for 2520 data and 137 / 137 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.020; Restrained GooF = 1.019 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0520 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.42865 0.00152 -0.001 OSF 2 1.97933 2.47617 0.000 BASF 1 3 0.00673 0.00080 -0.002 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for U12 C3 Max. shift = 0.000 A for H8C Max. dU = 0.000 for C10 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2171 / 172736 wR2 = 0.1393 before cycle 4 for 2520 data and 137 / 137 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.020; Restrained GooF = 1.019 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0520 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.42865 0.00152 0.000 OSF 2 1.97963 2.47616 0.000 BASF 1 3 0.00673 0.00080 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for x C1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C3 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2171 / 172736 wR2 = 0.1393 before cycle 5 for 2520 data and 137 / 137 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.020; Restrained GooF = 1.019 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0520 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.42865 0.00152 0.000 OSF 2 1.97895 2.47622 0.000 BASF 1 3 0.00673 0.00080 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x C7 Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 6 Maximum vector length = 511 Memory required = 2171 / 172736 wR2 = 0.1393 before cycle 6 for 2520 data and 137 / 137 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.020; Restrained GooF = 1.019 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0520 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.42865 0.00152 0.000 OSF 2 1.97925 2.47621 0.000 BASF 1 3 0.00673 0.00080 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x C7 Max. shift = 0.000 A for H12A Max. dU = 0.000 for H1N Largest correlation matrix elements 0.615 EXTI / OSF Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 1.5220 0.7780 1.6835 43 0.950 0.000 C3 C4 C2 H4 1.5542 0.9156 1.6765 43 0.950 0.000 C4 C5 C3 H5 1.6794 0.9639 1.7236 43 0.950 0.000 C5 C4 C6 H6 1.7692 0.8725 1.7847 43 0.950 0.000 C6 C5 C1 H8A 1.9436 0.6936 1.8366 137 0.980 0.000 C8 C7 H8A H8B 1.9072 0.6089 1.8044 137 0.980 0.000 C8 C7 H8A H8C 1.8689 0.6503 1.8811 137 0.980 0.000 C8 C7 H8A H10A 1.5408 0.6605 1.8507 137 0.980 0.000 C10 C9 H10A H10B 1.6332 0.6286 1.8606 137 0.980 0.000 C10 C9 H10A H10C 1.5631 0.5670 1.8315 137 0.980 0.000 C10 C9 H10A H11A 1.5308 0.6479 1.6424 137 0.980 0.000 C11 C9 H11A H11B 1.4769 0.6624 1.7195 137 0.980 0.000 C11 C9 H11A H11C 1.5094 0.5724 1.6986 137 0.980 0.000 C11 C9 H11A H12A 1.7184 0.5971 1.7395 137 0.980 0.000 C12 C9 H12A H12B 1.6774 0.6058 1.6548 137 0.980 0.000 C12 C9 H12A H12C 1.6491 0.5337 1.7124 137 0.980 0.000 C12 C9 H12A 2009lsh069 in I4(1)cd ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 1.69951 0.77032 1.77033 1.00000 0.02713 0.02821 0.02831 0.00056 -0.00017 0.00065 0.02788 0.00482 0.00018 0.00017 0.00016 0.00000 0.00157 0.00168 0.00148 0.00133 0.00119 0.00130 0.00069 C2 1.62588 0.73831 1.74001 1.00000 0.02622 0.02700 0.03150 0.00117 0.00391 0.00183 0.02824 0.00488 0.00017 0.00017 0.00016 0.00000 0.00149 0.00161 0.00157 0.00128 0.00124 0.00125 0.00065 C3 1.57271 0.79637 1.70460 1.00000 0.02599 0.03568 0.03490 -0.00018 -0.00166 0.00198 0.03219 0.00536 0.00018 0.00018 0.00017 0.00000 0.00152 0.00177 0.00156 0.00142 0.00129 0.00139 0.00070 H3 1.52203 0.77797 1.68348 1.00000 0.03862 0.00000 0.00000 C4 1.59201 0.87854 1.69976 1.00000 0.03532 0.03081 0.04232 0.00513 -0.00064 0.00693 0.03615 0.00565 0.00019 0.00019 0.00019 0.00000 0.00182 0.00176 0.00173 0.00146 0.00142 0.00146 0.00075 H4 1.55421 0.91558 1.67645 1.00000 0.04338 0.00000 0.00000 C5 1.66549 0.90754 1.72833 1.00000 0.03939 0.02883 0.04262 0.00283 0.00021 -0.00166 0.03695 0.00567 0.00021 0.00018 0.00018 0.00000 0.00189 0.00172 0.00195 0.00145 0.00145 0.00148 0.00076 H5 1.67940 0.96393 1.72358 1.00000 0.04434 0.00000 0.00000 C6 1.71868 0.85303 1.76409 1.00000 0.02856 0.03100 0.03302 -0.00043 0.00014 -0.00374 0.03086 0.00496 0.00018 0.00018 0.00016 0.00000 0.00165 0.00168 0.00166 0.00130 0.00129 0.00127 0.00070 H6 1.76917 0.87254 1.78472 1.00000 0.03703 0.00000 0.00000 C7 1.83387 0.70757 1.77983 1.00000 0.02493 0.02584 0.03410 -0.00305 0.00003 -0.00234 0.02829 0.00482 0.00018 0.00017 0.00017 0.00000 0.00159 0.00158 0.00159 0.00128 0.00127 0.00119 0.00065 C8 1.89355 0.66107 1.82983 1.00000 0.03385 0.03896 0.03148 0.00641 0.00025 0.00253 0.03476 0.00552 0.00019 0.00021 0.00017 0.00000 0.00178 0.00183 0.00153 0.00132 0.00132 0.00140 0.00074 H8A 1.94361 0.69362 1.83658 1.00000 0.05215 0.00000 0.00000 H8B 1.90717 0.60889 1.80444 1.00000 0.05215 0.00000 0.00000 H8C 1.86887 0.65031 1.88112 1.00000 0.05215 0.00000 0.00000 C9 1.60103 0.64733 1.74418 1.00000 0.02718 0.02758 0.03625 -0.00143 0.00226 -0.00183 0.03034 0.00510 0.00017 0.00018 0.00018 0.00000 0.00160 0.00153 0.00153 0.00132 0.00131 0.00120 0.00069 C10 1.58289 0.62371 1.82944 1.00000 0.04623 0.03518 0.04150 0.00294 0.00460 -0.00969 0.04097 0.00559 0.00021 0.00021 0.00018 0.00000 0.00195 0.00183 0.00168 0.00142 0.00151 0.00159 0.00080 H10A 1.54085 0.66046 1.85072 1.00000 0.06146 0.00000 0.00000 H10B 1.63316 0.62862 1.86057 1.00000 0.06146 0.00000 0.00000 H10C 1.56309 0.56697 1.83145 1.00000 0.06146 0.00000 0.00000 C11 1.52241 0.63103 1.69690 1.00000 0.03726 0.03258 0.05472 -0.00241 -0.00519 -0.00273 0.04152 0.00539 0.00019 0.00019 0.00020 0.00000 0.00189 0.00175 0.00194 0.00162 0.00161 0.00138 0.00080 H11A 1.53084 0.64794 1.64244 1.00000 0.06227 0.00000 0.00000 H11B 1.47691 0.66239 1.71950 1.00000 0.06227 0.00000 0.00000 H11C 1.50940 0.57235 1.69861 1.00000 0.06227 0.00000 0.00000 C12 1.66754 0.59085 1.70959 1.00000 0.03650 0.03101 0.05332 -0.00678 0.00551 -0.00143 0.04028 0.00593 0.00020 0.00018 0.00022 0.00000 0.00182 0.00170 0.00199 0.00153 0.00155 0.00142 0.00080 H12A 1.71844 0.59709 1.73954 1.00000 0.06042 0.00000 0.00000 H12B 1.67743 0.60581 1.65483 1.00000 0.06042 0.00000 0.00000 H12C 1.64907 0.53370 1.71237 1.00000 0.06042 0.00000 0.00000 N1 1.75911 0.71986 1.80959 1.00000 0.02583 0.03201 0.03069 0.00378 0.00078 -0.00198 0.02951 0.00401 0.00015 0.00015 0.00014 0.00000 0.00135 0.00142 0.00131 0.00114 0.00106 0.00111 0.00059 O1 1.85395 0.73266 1.71398 1.00000 0.02845 0.04003 0.03020 0.00488 0.00100 -0.00111 0.03289 0.00337 0.00011 0.00012 0.00011 0.00000 0.00113 0.00132 0.00112 0.00094 0.00087 0.00090 0.00053 H1N 1.74580 0.69934 1.85494 1.00000 0.04225 0.05657 0.00202 0.00202 0.00132 0.00000 0.00989 Final Structure Factor Calculation for 2009lsh069 in I4(1)cd Total number of l.s. parameters = 137 Maximum vector length = 511 Memory required = 2036 / 25046 wR2 = 0.1393 before cycle 7 for 2520 data and 2 / 137 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.020; Restrained GooF = 1.019 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0520 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0621 for 1726 Fo > 4sig(Fo) and 0.1070 for all 2520 data wR2 = 0.1393, GooF = S = 1.020, Restrained GooF = 1.019 for all data Occupancy sum of asymmetric unit = 14.00 for non-hydrogen and 17.00 for hydrogen atoms Principal mean square atomic displacements U 0.0289 0.0280 0.0267 C1 0.0341 0.0269 0.0237 C2 0.0363 0.0350 0.0253 C3 0.0448 0.0391 0.0246 C4 0.0432 0.0396 0.0280 C5 0.0339 0.0328 0.0258 C6 0.0352 0.0271 0.0226 C7 0.0432 0.0335 0.0276 C8 0.0371 0.0284 0.0255 C9 0.0525 0.0426 0.0278 C10 0.0563 0.0378 0.0305 C11 0.0568 0.0349 0.0291 C12 0.0353 0.0287 0.0245 N1 0.0421 0.0297 0.0269 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.024 0.034 0.043 0.054 0.066 0.080 0.099 0.131 0.181 1.000 Number in group 270. 251. 235. 263. 257. 247. 242. 249. 252. 254. GooF 0.999 0.965 1.007 0.987 1.035 1.118 1.057 1.016 0.990 1.021 K 2.478 1.310 1.095 1.082 1.003 1.000 1.009 1.014 1.009 1.026 Resolution(A) 0.77 0.80 0.84 0.88 0.92 0.98 1.06 1.17 1.33 1.67 inf Number in group 254. 254. 248. 254. 249. 262. 246. 249. 251. 253. GooF 0.841 0.946 1.224 1.068 1.000 1.105 0.985 0.895 0.905 1.160 K 1.101 1.083 1.219 1.062 1.036 0.992 1.019 1.011 1.024 1.021 R1 0.318 0.306 0.253 0.196 0.124 0.098 0.060 0.045 0.038 0.032 Recommended weighting scheme: WGHT 0.0516 1.8062 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) 1 2 1 3918.23 7651.76 6.72 0.351 6.70 1 2 -1 4059.05 7633.64 5.91 0.351 6.70 4 5 -13 166.74 324.14 3.77 0.072 1.17 4 7 17 -32.59 84.51 3.73 0.037 0.90 3 6 -17 500.95 774.59 3.49 0.112 0.93 7 11 -12 457.81 778.81 3.27 0.112 0.94 1 9 0 524.21 367.98 3.11 0.077 1.80 7 8 -15 25.28 205.51 3.05 0.058 0.91 2 6 -16 305.44 174.53 2.99 0.053 0.99 2 8 -18 -206.38 230.97 2.98 0.061 0.86 1 4 -17 164.20 57.17 2.91 0.030 0.97 0 6 -14 5829.13 4489.87 2.90 0.269 1.11 11 12 11 277.22 84.48 2.86 0.037 0.84 2 8 0 1455.97 1173.83 2.85 0.138 1.98 8 8 16 -83.49 96.72 2.82 0.039 0.86 8 12 -6 348.39 534.93 2.82 0.093 1.05 7 8 -13 159.18 315.13 2.81 0.071 1.00 8 15 -9 1424.44 774.69 2.79 0.112 0.86 1 18 7 1046.40 688.62 2.70 0.105 0.85 1 3 -18 181.75 284.26 2.66 0.068 0.93 0 2 20 1128.46 735.99 2.65 0.109 0.85 2 18 -6 331.85 52.47 2.63 0.029 0.86 5 7 18 163.88 27.90 2.63 0.021 0.85 8 13 9 692.70 505.65 2.62 0.090 0.93 3 17 -6 586.41 280.25 2.61 0.067 0.90 6 17 -5 315.74 114.06 2.58 0.043 0.87 7 9 2 705.11 517.88 2.57 0.091 1.41 6 8 0 138.55 32.32 2.57 0.023 1.63 0 16 -4 746.44 1091.39 2.57 0.133 0.99 5 14 -7 -23.49 118.75 2.57 0.044 1.00 2 13 -13 627.68 338.26 2.55 0.074 0.90 6 12 10 2019.79 1637.36 2.53 0.162 0.99 10 10 -4 1151.87 1524.07 2.50 0.157 1.11 10 16 2 241.21 25.52 2.50 0.020 0.86 10 10 4 1184.67 1532.28 2.47 0.157 1.11 1 14 13 222.16 98.28 2.46 0.040 0.87 4 12 -10 -69.55 44.84 2.46 0.027 1.03 3 7 0 558.58 422.23 2.45 0.082 2.14 10 16 4 307.16 39.58 2.45 0.025 0.85 8 16 -6 707.66 417.31 2.44 0.082 0.87 14 15 5 102.03 388.80 2.44 0.079 0.77 4 13 5 326.38 202.40 2.44 0.057 1.13 6 7 -9 245.69 351.49 2.43 0.075 1.29 8 18 2 503.73 266.90 2.41 0.066 0.82 8 17 -3 377.92 136.90 2.41 0.047 0.86 10 16 10 44.08 240.15 2.39 0.062 0.77 3 17 8 392.01 109.73 2.38 0.042 0.86 9 15 -8 543.66 141.82 2.38 0.048 0.85 7 16 7 324.29 131.07 2.38 0.046 0.87 11 14 -5 922.54 598.98 2.38 0.098 0.88 Bond lengths and angles C1 - Distance Angles C6 1.3878 (0.0041) C2 1.4074 (0.0041) 121.58 (0.25) N1 1.4386 (0.0036) 116.05 (0.25) 122.37 (0.24) C1 - C6 C2 C2 - Distance Angles C1 1.4074 (0.0041) C3 1.4185 (0.0040) 115.50 (0.25) C9 1.5388 (0.0040) 124.37 (0.24) 120.12 (0.26) C2 - C1 C3 C3 - Distance Angles C4 1.3782 (0.0042) C2 1.4185 (0.0040) 122.31 (0.29) H3 0.9500 118.85 118.85 C3 - C4 C2 C4 - Distance Angles C5 1.3769 (0.0047) C3 1.3782 (0.0042) 120.72 (0.29) H4 0.9500 119.64 119.64 C4 - C5 C3 C5 - Distance Angles C4 1.3769 (0.0047) C6 1.3835 (0.0040) 118.75 (0.28) H5 0.9500 120.62 120.62 C5 - C4 C6 C6 - Distance Angles C5 1.3835 (0.0040) C1 1.3878 (0.0041) 121.11 (0.28) H6 0.9500 119.44 119.44 C6 - C5 C1 C7 - Distance Angles O1 1.2409 (0.0034) N1 1.3353 (0.0039) 122.43 (0.27) C8 1.5000 (0.0041) 120.77 (0.26) 116.79 (0.26) C7 - O1 N1 C8 - Distance Angles C7 1.5000 (0.0041) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C7 H8A H8B C9 - Distance Angles C10 1.5352 (0.0042) C11 1.5378 (0.0043) 107.13 (0.25) C2 1.5388 (0.0040) 109.65 (0.25) 111.19 (0.25) C12 1.5401 (0.0043) 110.47 (0.27) 106.35 (0.25) 111.90 (0.23) C9 - C10 C11 C2 C10 - Distance Angles C9 1.5352 (0.0042) 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 1.5378 (0.0043) 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 C12 - Distance Angles C9 1.5401 (0.0043) H12A 0.9800 109.47 H12B 0.9800 109.47 109.47 H12C 0.9800 109.47 109.47 109.47 C12 - C9 H12A H12B N1 - Distance Angles C7 1.3353 (0.0039) C1 1.4386 (0.0036) 121.62 (0.25) H1N 0.8713 (0.0182) 120.53 (2.34) 117.77 (2.35) N1 - C7 C1 O1 - Distance Angles C7 1.2409 (0.0034) O1 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.871(18) 2.066(19) 2.931(3) 171(3) 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)