+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 11:20:22 on 23-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009lsh070 in P2(1)/c CELL 0.71073 10.5164 9.8032 10.9034 90.000 95.691 90.000 ZERR 4.00 0.0003 0.0003 0.0002 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 48 68 4 8 V = 1118.54 F(000) = 448.0 Mu = 0.08 mm-1 Cell Wt = 829.06 Rho = 1.231 MERG 2 OMIT -3.00 55.00 OMIT 1 2 1 OMIT 2 1 2 DFIX 0.88 0.02 N1 H1N EQIV $1 -x, y-1/2, -z+5/2 HTAB N1 O1_$1 FMAP 2 PLAN 5 SIZE 0.28 0.38 0.44 ACTA HTAB 2.00000 BOND $H WGHT 0.04510 0.35470 L.S. 8 TEMP -153.00 FVAR 1.30568 C1 1 0.112702 0.074651 1.106903 11.00000 0.01701 0.01459 = 0.01990 -0.00274 0.00209 -0.00224 C2 1 0.102773 0.189480 1.031744 11.00000 0.01718 0.01694 = 0.02456 -0.00045 0.00079 0.00216 AFIX 43 H2 2 0.032243 0.249602 1.034349 11.00000 -1.20000 AFIX 0 C3 1 0.196091 0.216821 0.952398 11.00000 0.02001 0.01531 = 0.02369 0.00348 0.00003 -0.00033 AFIX 43 H3 2 0.189006 0.295488 0.901298 11.00000 -1.20000 AFIX 0 C4 1 0.299205 0.129033 0.948208 11.00000 0.01713 0.01660 = 0.01890 -0.00084 0.00175 -0.00237 C5 1 0.308046 0.012649 1.022022 11.00000 0.02001 0.01505 = 0.02443 0.00010 0.00378 0.00201 AFIX 43 H5 2 0.377956 -0.048153 1.018660 11.00000 -1.20000 AFIX 0 C6 1 0.215376 -0.014487 1.100062 11.00000 0.02349 0.01234 = 0.02251 0.00215 0.00325 0.00076 AFIX 43 H6 2 0.221545 -0.094464 1.149495 11.00000 -1.20000 AFIX 0 C7 1 -0.057633 0.125485 1.242787 11.00000 0.01815 0.01812 = 0.02364 -0.00409 0.00157 0.00003 C8 1 -0.145806 0.057242 1.324804 11.00000 0.02694 0.02568 = 0.03323 -0.00201 0.01235 0.00053 AFIX 137 H8A 2 -0.144012 0.107171 1.402824 11.00000 -1.50000 H8B 2 -0.117684 -0.036900 1.341115 11.00000 -1.50000 H8C 2 -0.233056 0.057083 1.283803 11.00000 -1.50000 AFIX 0 C9 1 0.391924 0.263179 0.795147 11.00000 0.02538 0.01324 = 0.02272 0.00335 0.00423 0.00024 AFIX 23 H9A 2 0.387879 0.348179 0.843633 11.00000 -1.20000 H9B 2 0.314998 0.258388 0.735114 11.00000 -1.20000 AFIX 0 C10 1 0.511585 0.261751 0.728506 11.00000 0.02411 0.01631 = 0.01934 0.00041 0.00382 -0.00284 AFIX 23 H10A 2 0.587296 0.260910 0.790185 11.00000 -1.20000 H10B 2 0.514767 0.346553 0.679602 11.00000 -1.20000 AFIX 0 C11 1 0.518494 0.139784 0.643244 11.00000 0.02860 0.01690 = 0.02548 -0.00232 0.00423 -0.00138 AFIX 23 H11A 2 0.442167 0.139953 0.582298 11.00000 -1.20000 H11B 2 0.516436 0.055019 0.692362 11.00000 -1.20000 AFIX 0 C12 1 0.637952 0.139048 0.574807 11.00000 0.03607 0.02022 = 0.02155 -0.00048 0.00778 -0.00119 AFIX 137 H12A 2 0.638717 0.220606 0.522910 11.00000 -1.50000 H12B 2 0.637949 0.057362 0.522995 11.00000 -1.50000 H12C 2 0.714032 0.138704 0.634493 11.00000 -1.50000 AFIX 0 N1 3 0.021368 0.039828 1.189518 11.00000 0.02050 0.01332 = 0.02486 -0.00036 0.00595 -0.00019 O1 4 -0.059466 0.250064 1.226225 11.00000 0.02907 0.01643 = 0.03315 -0.00336 0.00644 0.00291 O2 4 0.397456 0.146504 0.875416 11.00000 0.02055 0.01838 = 0.02480 0.00732 0.00648 0.00197 H1N 2 0.018841 -0.047039 1.209385 11.00000 0.02791 HKLF 4 Covalent radii and connectivity table for 2009lsh070 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - C2 C6 N1 C2 - C1 C3 C3 - C4 C2 C4 - O2 C3 C5 C5 - C6 C4 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 C9 - O2 C10 C10 - C9 C11 C11 - C10 C12 C12 - C11 N1 - C7 C1 O1 - C7 O2 - C4 C9 Operators for generating equivalent atoms: $1 -x, y-1/2, -z+5/2 17135 Reflections read, of which 546 rejected -13 =< h =< 13, -12 =< k =< 11, -13 =< l =< 14, Max. 2-theta = 55.00 0 Systematic absence violations 0 Inconsistent equivalents 2552 Unique reflections, of which 0 suppressed R(int) = 0.0407 R(sigma) = 0.0280 Friedel opposites merged Maximum memory for data reduction = 1742 / 25371 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 = 2160 / 178556 wR2 = 0.1017 before cycle 1 for 2552 data and 142 / 142 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 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.060 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0451 * P )^2 + 0.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.30565 0.00285 -0.009 OSF Mean shift/esd = 0.007 Maximum = -0.026 for U33 O2 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 2160 / 178556 wR2 = 0.1017 before cycle 2 for 2552 data and 142 / 142 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 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.061 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0451 * P )^2 + 0.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.30562 0.00285 -0.011 OSF Mean shift/esd = 0.003 Maximum = -0.011 for OSF Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 3 Maximum vector length = 511 Memory required = 2160 / 178556 wR2 = 0.1017 before cycle 3 for 2552 data and 142 / 142 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 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.061 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0451 * P )^2 + 0.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.30562 0.00285 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 H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 2160 / 178556 wR2 = 0.1017 before cycle 4 for 2552 data and 142 / 142 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 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.061 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0451 * P )^2 + 0.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.30562 0.00285 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for tors H8A Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 5 Maximum vector length = 511 Memory required = 2160 / 178556 wR2 = 0.1017 before cycle 5 for 2552 data and 142 / 142 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 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.060 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0451 * P )^2 + 0.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.30562 0.00285 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z O1 Max. shift = 0.000 A for H8C Max. dU = 0.000 for C1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2160 / 178556 wR2 = 0.1017 before cycle 6 for 2552 data and 142 / 142 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 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.061 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0451 * P )^2 + 0.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.30562 0.00285 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z O1 Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 7 Maximum vector length = 511 Memory required = 2160 / 178556 wR2 = 0.1017 before cycle 7 for 2552 data and 142 / 142 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 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.061 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0451 * P )^2 + 0.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.30562 0.00285 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z O1 Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 8 Maximum vector length = 511 Memory required = 2160 / 178556 wR2 = 0.1017 before cycle 8 for 2552 data and 142 / 142 parameters Summary of restraints applied in cycle 8 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 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.061 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0451 * P )^2 + 0.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.30562 0.00285 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z O1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C6 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.0322 0.2496 1.0343 43 0.950 0.000 C2 C1 C3 H3 0.1890 0.2955 0.9013 43 0.950 0.000 C3 C4 C2 H5 0.3780 -0.0482 1.0187 43 0.950 0.000 C5 C6 C4 H6 0.2215 -0.0945 1.1495 43 0.950 0.000 C6 C5 C1 H8A -0.1440 0.1072 1.4028 137 0.980 0.000 C8 C7 H8A H8B -0.1177 -0.0369 1.3411 137 0.980 0.000 C8 C7 H8A H8C -0.2331 0.0571 1.2838 137 0.980 0.000 C8 C7 H8A H9A 0.3879 0.3482 0.8436 23 0.990 0.000 C9 O2 C10 H9B 0.3150 0.2584 0.7351 23 0.990 0.000 C9 O2 C10 H10A 0.5873 0.2609 0.7902 23 0.990 0.000 C10 C9 C11 H10B 0.5148 0.3466 0.6796 23 0.990 0.000 C10 C9 C11 H11A 0.4422 0.1400 0.5823 23 0.990 0.000 C11 C10 C12 H11B 0.5164 0.0550 0.6924 23 0.990 0.000 C11 C10 C12 H12A 0.6387 0.2206 0.5229 137 0.980 0.000 C12 C11 H12A H12B 0.6379 0.0574 0.5230 137 0.980 0.000 C12 C11 H12A H12C 0.7140 0.1387 0.6345 137 0.980 0.000 C12 C11 H12A 2009lsh070 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.11270 0.07465 1.10690 1.00000 0.01700 0.01458 0.01990 -0.00274 0.00209 -0.00224 0.01714 0.00186 0.00010 0.00011 0.00010 0.00000 0.00052 0.00053 0.00053 0.00041 0.00039 0.00040 0.00024 C2 0.10277 0.18948 1.03174 1.00000 0.01717 0.01693 0.02456 -0.00044 0.00079 0.00216 0.01964 0.00198 0.00011 0.00012 0.00010 0.00000 0.00053 0.00056 0.00057 0.00044 0.00042 0.00041 0.00025 H2 0.03224 0.24960 1.03435 1.00000 0.02357 0.00000 0.00000 C3 0.19609 0.21682 0.95240 1.00000 0.02000 0.01530 0.02368 0.00348 0.00003 -0.00033 0.01981 0.00198 0.00011 0.00011 0.00010 0.00000 0.00056 0.00053 0.00057 0.00043 0.00043 0.00042 0.00025 H3 0.18901 0.29549 0.90130 1.00000 0.02377 0.00000 0.00000 C4 0.29920 0.12903 0.94821 1.00000 0.01712 0.01659 0.01889 -0.00084 0.00174 -0.00237 0.01754 0.00189 0.00010 0.00011 0.00010 0.00000 0.00053 0.00054 0.00052 0.00042 0.00040 0.00041 0.00024 C5 0.30804 0.01265 1.02202 1.00000 0.02000 0.01505 0.02442 0.00010 0.00378 0.00201 0.01972 0.00203 0.00011 0.00011 0.00010 0.00000 0.00054 0.00054 0.00056 0.00044 0.00043 0.00042 0.00025 H5 0.37795 -0.04815 1.01866 1.00000 0.02366 0.00000 0.00000 C6 0.21538 -0.01449 1.10006 1.00000 0.02349 0.01233 0.02250 0.00214 0.00324 0.00076 0.01937 0.00199 0.00011 0.00011 0.00010 0.00000 0.00058 0.00052 0.00056 0.00042 0.00044 0.00041 0.00025 H6 0.22154 -0.09446 1.14949 1.00000 0.02325 0.00000 0.00000 C7 -0.05763 0.12548 1.24279 1.00000 0.01815 0.01812 0.02363 -0.00409 0.00156 0.00003 0.02000 0.00198 0.00010 0.00012 0.00010 0.00000 0.00054 0.00057 0.00056 0.00044 0.00042 0.00042 0.00025 C8 -0.14581 0.05724 1.32481 1.00000 0.02693 0.02567 0.03323 -0.00201 0.01234 0.00054 0.02799 0.00240 0.00012 0.00013 0.00012 0.00000 0.00064 0.00065 0.00067 0.00052 0.00051 0.00050 0.00029 H8A -0.14403 0.10719 1.40282 1.00000 0.04198 0.00000 0.00000 H8B -0.11767 -0.03689 1.34113 1.00000 0.04198 0.00000 0.00000 H8C -0.23305 0.05706 1.28380 1.00000 0.04198 0.00000 0.00000 C9 0.39192 0.26318 0.79514 1.00000 0.02538 0.01323 0.02270 0.00335 0.00423 0.00024 0.02032 0.00209 0.00011 0.00011 0.00010 0.00000 0.00058 0.00053 0.00056 0.00043 0.00044 0.00043 0.00025 H9A 0.38788 0.34818 0.84363 1.00000 0.02438 0.00000 0.00000 H9B 0.31500 0.25838 0.73511 1.00000 0.02438 0.00000 0.00000 C10 0.51158 0.26175 0.72851 1.00000 0.02411 0.01630 0.01933 0.00042 0.00382 -0.00284 0.01980 0.00200 0.00011 0.00012 0.00010 0.00000 0.00057 0.00056 0.00055 0.00043 0.00043 0.00043 0.00025 H10A 0.58730 0.26091 0.79019 1.00000 0.02376 0.00000 0.00000 H10B 0.51477 0.34655 0.67960 1.00000 0.02376 0.00000 0.00000 C11 0.51849 0.13978 0.64324 1.00000 0.02860 0.01690 0.02547 -0.00232 0.00422 -0.00138 0.02355 0.00211 0.00012 0.00012 0.00011 0.00000 0.00063 0.00058 0.00060 0.00045 0.00047 0.00046 0.00027 H11A 0.44217 0.13995 0.58230 1.00000 0.02826 0.00000 0.00000 H11B 0.51644 0.05502 0.69236 1.00000 0.02826 0.00000 0.00000 C12 0.63795 0.13905 0.57481 1.00000 0.03607 0.02021 0.02154 -0.00048 0.00778 -0.00119 0.02562 0.00225 0.00012 0.00013 0.00011 0.00000 0.00069 0.00060 0.00057 0.00047 0.00049 0.00050 0.00028 H12A 0.63872 0.22061 0.52291 1.00000 0.03842 0.00000 0.00000 H12B 0.63795 0.05737 0.52299 1.00000 0.03842 0.00000 0.00000 H12C 0.71403 0.13870 0.63449 1.00000 0.03842 0.00000 0.00000 N1 0.02137 0.03983 1.18952 1.00000 0.02050 0.01331 0.02485 -0.00036 0.00595 -0.00019 0.01931 0.00172 0.00009 0.00010 0.00009 0.00000 0.00049 0.00048 0.00050 0.00038 0.00037 0.00037 0.00022 O1 -0.05947 0.25006 1.22622 1.00000 0.02907 0.01642 0.03315 -0.00335 0.00644 0.00290 0.02599 0.00152 0.00008 0.00008 0.00008 0.00000 0.00047 0.00043 0.00048 0.00034 0.00036 0.00034 0.00022 O2 0.39746 0.14650 0.87542 1.00000 0.02055 0.01837 0.02479 0.00732 0.00648 0.00197 0.02095 0.00149 0.00007 0.00008 0.00007 0.00000 0.00041 0.00042 0.00042 0.00032 0.00032 0.00031 0.00020 H1N 0.01884 -0.04702 1.20939 1.00000 0.02793 0.02476 0.00134 0.00130 0.00128 0.00000 0.00372 Final Structure Factor Calculation for 2009lsh070 in P2(1)/c Total number of l.s. parameters = 142 Maximum vector length = 511 Memory required = 2018 / 22995 wR2 = 0.1017 before cycle 9 for 2552 data and 0 / 142 parameters Summary of restraints applied in cycle 9 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 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.061 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0451 * P )^2 + 0.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0392 for 2149 Fo > 4sig(Fo) and 0.0487 for all 2552 data wR2 = 0.1017, GooF = S = 1.061, Restrained GooF = 1.061 for all data Occupancy sum of asymmetric unit = 15.00 for non-hydrogen and 17.00 for hydrogen atoms Principal mean square atomic displacements U 0.0213 0.0175 0.0127 C1 0.0250 0.0190 0.0149 C2 0.0260 0.0194 0.0140 C3 0.0196 0.0186 0.0144 C4 0.0248 0.0200 0.0143 C5 0.0242 0.0220 0.0119 C6 0.0259 0.0181 0.0159 C7 0.0392 0.0260 0.0188 C8 0.0264 0.0224 0.0121 C9 0.0253 0.0191 0.0151 C10 0.0294 0.0250 0.0163 C11 0.0372 0.0201 0.0195 C12 0.0266 0.0180 0.0133 N1 0.0349 0.0284 0.0147 O1 0.0310 0.0185 0.0133 O2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.014 0.028 0.043 0.059 0.078 0.101 0.127 0.177 0.248 1.000 Number in group 256. 264. 249. 254. 261. 246. 257. 260. 249. 256. GooF 0.868 1.059 0.976 1.186 1.124 1.138 1.023 1.129 0.961 1.098 K 2.487 1.063 0.999 0.983 0.994 0.973 0.994 1.015 1.012 1.008 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.65 inf Number in group 263. 254. 252. 258. 248. 257. 257. 252. 255. 256. GooF 0.934 0.916 0.923 0.987 0.922 1.093 0.995 1.035 1.258 1.421 K 1.029 1.044 1.012 1.005 1.012 0.995 1.015 1.014 1.023 0.994 R1 0.108 0.087 0.076 0.062 0.048 0.050 0.034 0.030 0.039 0.033 Recommended weighting scheme: WGHT 0.0449 0.3562 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 5 2 53.89 33.83 4.36 0.077 1.84 -1 2 1 3.09 10.97 4.18 0.044 4.17 4 4 1 10.24 3.99 3.70 0.027 1.75 -6 0 6 23.06 12.00 3.65 0.046 1.32 -8 1 7 75.74 104.00 3.61 0.135 1.05 -7 2 8 14.65 26.53 3.60 0.068 1.03 -3 6 2 95.74 71.48 3.48 0.112 1.44 1 2 0 1492.53 1782.63 3.45 0.560 4.44 1 8 8 17.64 30.57 3.43 0.073 0.90 1 8 7 23.89 40.34 3.43 0.084 0.95 3 0 0 114.30 148.49 3.40 0.162 3.49 4 5 0 29.69 44.46 3.35 0.088 1.57 -3 5 3 188.29 150.74 3.29 0.163 1.58 -8 2 7 69.12 93.00 3.28 0.128 1.03 6 3 1 7.60 2.64 3.27 0.022 1.51 -7 4 3 18.45 9.66 3.24 0.041 1.24 8 6 0 1.04 7.10 3.18 0.035 1.02 6 2 1 117.51 91.63 3.14 0.127 1.60 -8 6 2 39.51 56.32 3.14 0.100 1.02 2 0 8 219.50 167.19 3.13 0.172 1.28 1 5 5 5.03 1.29 3.09 0.015 1.43 -4 4 1 299.13 251.14 2.90 0.210 1.78 -9 0 6 87.35 113.04 2.87 0.141 1.03 7 0 4 50.77 36.67 2.86 0.080 1.26 -1 5 2 91.68 72.33 2.85 0.113 1.83 0 0 2 698.62 832.94 2.83 0.383 5.42 -11 5 7 9.25 18.55 2.80 0.057 0.78 -5 0 2 206.93 169.73 2.80 0.173 2.02 -8 0 8 8.17 15.67 2.79 0.053 0.99 2 1 12 29.19 46.75 2.78 0.091 0.87 -4 1 3 18.05 11.05 2.78 0.044 2.17 -4 3 4 163.98 135.30 2.75 0.154 1.70 -2 3 6 3.85 1.18 2.72 0.014 1.55 -8 2 6 46.14 61.20 2.72 0.104 1.09 1 7 5 18.43 11.23 2.71 0.044 1.16 -2 1 1 947.00 1095.03 2.69 0.439 4.39 -7 0 12 45.72 31.66 2.68 0.075 0.81 -4 9 2 -0.12 3.84 2.64 0.026 1.00 1 1 1 397.52 464.03 2.63 0.286 5.79 2 0 0 2029.75 2330.44 2.59 0.641 5.23 0 8 6 376.17 320.86 2.57 0.238 1.01 -1 8 5 53.55 69.28 2.57 0.110 1.07 6 1 6 31.79 22.63 2.57 0.063 1.19 1 3 0 420.67 486.72 2.56 0.293 3.12 8 3 4 23.80 33.84 2.55 0.077 1.07 -4 2 3 547.97 476.10 2.54 0.290 2.03 -2 5 2 7.49 3.67 2.53 0.025 1.76 -3 0 6 71.32 55.98 2.51 0.099 1.67 5 1 2 61.45 48.30 2.49 0.092 1.86 6 3 2 173.04 146.08 2.48 0.160 1.45 Bond lengths and angles C1 - Distance Angles C2 1.3902 (0.0016) C6 1.3968 (0.0015) 119.23 (0.10) N1 1.4220 (0.0014) 123.49 (0.10) 117.26 (0.10) C1 - C2 C6 C2 - Distance Angles C1 1.3902 (0.0016) C3 1.3971 (0.0016) 120.27 (0.10) H2 0.9500 119.87 119.87 C2 - C1 C3 C3 - Distance Angles C4 1.3887 (0.0016) C2 1.3971 (0.0016) 120.02 (0.10) H3 0.9500 119.99 119.99 C3 - C4 C2 C4 - Distance Angles O2 1.3746 (0.0013) C3 1.3887 (0.0016) 125.16 (0.10) C5 1.3940 (0.0015) 115.11 (0.10) 119.72 (0.10) C4 - O2 C3 C5 - Distance Angles C6 1.3816 (0.0015) C4 1.3940 (0.0015) 120.16 (0.10) H5 0.9500 119.92 119.92 C5 - C6 C4 C6 - Distance Angles C5 1.3816 (0.0015) C1 1.3968 (0.0015) 120.57 (0.10) H6 0.9500 119.71 119.71 C6 - C5 C1 C7 - Distance Angles O1 1.2344 (0.0014) N1 1.3522 (0.0014) 123.56 (0.11) C8 1.5072 (0.0016) 121.62 (0.10) 114.81 (0.10) C7 - O1 N1 C8 - Distance Angles C7 1.5072 (0.0016) 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 O2 1.4379 (0.0013) C10 1.5143 (0.0016) 107.42 (0.09) H9A 0.9900 110.23 110.23 H9B 0.9900 110.23 110.23 108.51 C9 - O2 C10 H9A C10 - Distance Angles C9 1.5143 (0.0016) C11 1.5207 (0.0015) 113.14 (0.09) H10A 0.9900 108.95 108.95 H10B 0.9900 108.95 108.95 107.76 C10 - C9 C11 H10A C11 - Distance Angles C10 1.5207 (0.0015) C12 1.5235 (0.0016) 113.26 (0.10) H11A 0.9900 108.92 108.92 H11B 0.9900 108.92 108.92 107.74 C11 - C10 C12 H11A C12 - Distance Angles C11 1.5235 (0.0016) H12A 0.9800 109.47 H12B 0.9800 109.47 109.47 H12C 0.9800 109.47 109.47 109.47 C12 - C11 H12A H12B N1 - Distance Angles C7 1.3522 (0.0014) C1 1.4220 (0.0014) 127.26 (0.10) H1N 0.8796 (0.0124) 117.41 (0.92) 115.29 (0.92) N1 - C7 C1 O1 - Distance Angles C7 1.2344 (0.0014) O1 - O2 - Distance Angles C4 1.3746 (0.0013) C9 1.4379 (0.0013) 117.59 (0.08) O2 - C4 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.880(12) 2.138(13) 3.0001(13) 166.3(13) 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)