+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 23:41:28 on 13-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh060 in P2(1)2(1)2(1) CELL 0.71073 4.7667 18.4984 18.6318 90.000 90.000 90.000 ZERR 8.00 0.0001 0.0004 0.0004 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O CL UNIT 64 64 8 8 8 V = 1642.88 F(000) = 704.0 Mu = 0.40 mm-1 Cell Wt = 1356.83 Rho = 1.371 MERG 2 OMIT -3.00 55.00 OMIT 0 1 3 OMIT 1 0 3 OMIT 0 2 2 FMAP 2 PLAN 5 ACTA EQIV $1 -x-1, y-1/2, -z+5/2 HTAB N1 O11_$1 HTAB N11 O1 HTAB BOND $H DFIX 0.88 0.02 N1 H1N N11 H11N L.S. 6 SIZE 0.24 0.24 0.1 TEMP -153.00 WGHT 0.0495 0.3236 FVAR 0.82786 MOLE 1 C1 1 -0.270642 -0.324166 1.320705 11.00000 0.02755 0.03198 = 0.02917 0.00427 0.00335 -0.00130 C2 1 -0.295464 -0.249499 1.332314 11.00000 0.03215 0.03000 = 0.02878 0.00249 0.00298 -0.00350 AFIX 43 H2 2 -0.425360 -0.221404 1.305530 11.00000 -1.20000 AFIX 0 C3 1 -0.126281 -0.217856 1.383670 11.00000 0.03525 0.04285 = 0.03168 -0.00332 0.00912 -0.01047 C4 1 0.066843 -0.256163 1.423629 11.00000 0.03146 0.07265 = 0.03068 -0.00374 -0.00043 -0.00632 AFIX 43 H4 2 0.181385 -0.232737 1.458271 11.00000 -1.20000 AFIX 0 C5 1 0.088513 -0.330102 1.411599 11.00000 0.03741 0.06545 = 0.04049 0.00415 -0.00335 0.01142 AFIX 43 H5 2 0.219605 -0.357785 1.438424 11.00000 -1.20000 AFIX 0 C6 1 -0.078913 -0.363868 1.360932 11.00000 0.03705 0.04263 = 0.03953 0.00782 0.00074 0.00614 AFIX 43 H6 2 -0.062738 -0.414517 1.353586 11.00000 -1.20000 AFIX 0 C7 1 -0.589719 -0.334834 1.216208 11.00000 0.03083 0.02452 = 0.03114 0.00290 0.00246 -0.00503 C8 1 -0.761397 -0.389151 1.174948 11.00000 0.04170 0.03042 = 0.03909 0.00058 -0.00283 -0.00644 AFIX 137 H8A 2 -0.959806 -0.375390 1.176763 11.00000 -1.50000 H8B 2 -0.737523 -0.437146 1.196364 11.00000 -1.50000 H8C 2 -0.698524 -0.390246 1.124882 11.00000 -1.50000 AFIX 0 N1 3 -0.439948 -0.361951 1.271387 11.00000 0.03436 0.02053 = 0.03446 0.00550 0.00068 -0.00076 O1 4 -0.587238 -0.270673 1.198582 11.00000 0.05248 0.02560 = 0.04273 0.01178 -0.01081 -0.00524 CL1 5 0.192999 -0.000948 0.968980 11.00000 0.05762 0.03646 = 0.04614 0.01429 0.01071 -0.00530 H1N 2 -0.455352 -0.407781 1.280753 11.00000 0.04466 MOLE 2 C11 1 -0.198466 -0.126621 1.111388 11.00000 0.02464 0.02287 = 0.02579 -0.00239 -0.00270 -0.00261 C12 1 -0.121836 -0.066568 1.070049 11.00000 0.03207 0.02151 = 0.03148 0.00048 -0.00271 -0.00079 AFIX 43 H12 2 -0.210782 -0.021068 1.076472 11.00000 -1.20000 AFIX 0 C13 1 0.088701 -0.075810 1.019328 11.00000 0.03359 0.02904 = 0.02784 0.00463 -0.00291 -0.00662 C14 1 0.220256 -0.141398 1.007425 11.00000 0.02874 0.03606 = 0.02749 -0.00214 0.00161 -0.00248 AFIX 43 H14 2 0.361448 -0.146135 0.971748 11.00000 -1.20000 AFIX 0 C15 1 0.140217 -0.200008 1.049032 11.00000 0.02917 0.02723 = 0.03429 -0.00538 -0.00081 0.00118 AFIX 43 H15 2 0.228212 -0.245546 1.042041 11.00000 -1.20000 AFIX 0 C16 1 -0.066166 -0.192822 1.100531 11.00000 0.02791 0.02192 = 0.03038 -0.00044 -0.00114 -0.00116 AFIX 43 H16 2 -0.118342 -0.233394 1.128798 11.00000 -1.20000 AFIX 0 C17 1 -0.519088 -0.065937 1.197575 11.00000 0.02709 0.02479 = 0.03279 -0.00343 -0.00314 0.00115 C18 1 -0.745448 -0.080610 1.251893 11.00000 0.03443 0.03279 = 0.03469 -0.00590 0.00161 0.00056 AFIX 137 H18A 2 -0.670484 -0.073333 1.300334 11.00000 -1.50000 H18B 2 -0.810627 -0.130599 1.246859 11.00000 -1.50000 H18C 2 -0.902725 -0.047460 1.243877 11.00000 -1.50000 AFIX 0 N11 3 -0.412120 -0.124636 1.163830 11.00000 0.02859 0.01723 = 0.02973 -0.00184 0.00069 -0.00135 O11 4 -0.432762 -0.004068 1.185842 11.00000 0.04731 0.02053 = 0.04877 -0.00632 0.00761 -0.00151 CL2 5 -0.170070 -0.125059 1.399580 11.00000 0.06391 0.04326 = 0.04081 -0.01249 0.00539 -0.01667 H11N 2 -0.476930 -0.166139 1.176873 11.00000 0.02370 HKLF 4 Covalent radii and connectivity table for 2008lsh060 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 CL 0.990 C1 - C6 C2 N1 C2 - C3 C1 C3 - C4 C2 Cl2 C4 - C3 C5 C5 - C6 C4 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 N1 - C7 C1 O1 - C7 Cl1 - C13 C11 - C16 C12 N11 C12 - C13 C11 C13 - C14 C12 Cl1 C14 - C13 C15 C15 - C16 C14 C16 - C15 C11 C17 - O11 N11 C18 C18 - C17 N11 - C17 C11 O11 - C17 Cl2 - C3 Operators for generating equivalent atoms: $1 -x-1, y-1/2, -z+5/2 61277 Reflections read, of which 244 rejected -6 =< h =< 6, -24 =< k =< 24, -24 =< l =< 23, Max. 2-theta = 54.98 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -2 11 18 -1.49 0.56 8 4.81 1 Inconsistent equivalents 3760 Unique reflections, of which 0 suppressed R(int) = 0.0532 R(sigma) = 0.0218 Friedel opposites not merged Maximum memory for data reduction = 2083 / 37926 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 = 2643 / 259978 wR2 = 0.0877 before cycle 1 for 3760 data and 209 / 209 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. 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 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.069; Restrained GooF = 1.069 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0495 * P )^2 + 0.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.82786 0.00131 0.003 OSF Mean shift/esd = 0.091 Maximum = 0.303 for z Cl2 Max. shift = 0.005 A for H1N Max. dU = 0.000 for H11N Least-squares cycle 2 Maximum vector length = 511 Memory required = 2643 / 259978 wR2 = 0.0876 before cycle 2 for 3760 data and 209 / 209 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. 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 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.069; Restrained GooF = 1.069 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0495 * P )^2 + 0.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.82767 0.00131 -0.146 OSF Mean shift/esd = 0.029 Maximum = -0.146 for OSF Max. shift = 0.002 A for H1N Max. dU = 0.000 for H11N Least-squares cycle 3 Maximum vector length = 511 Memory required = 2643 / 259978 wR2 = 0.0876 before cycle 3 for 3760 data and 209 / 209 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. 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 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.069; Restrained GooF = 1.069 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0495 * P )^2 + 0.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.82767 0.00131 -0.001 OSF Mean shift/esd = 0.001 Maximum = 0.018 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for H11N Least-squares cycle 4 Maximum vector length = 511 Memory required = 2643 / 259978 wR2 = 0.0876 before cycle 4 for 3760 data and 209 / 209 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. 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 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.069; Restrained GooF = 1.069 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0495 * P )^2 + 0.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.82767 0.00131 0.001 OSF Mean shift/esd = 0.001 Maximum = 0.006 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 5 Maximum vector length = 511 Memory required = 2643 / 259978 wR2 = 0.0876 before cycle 5 for 3760 data and 209 / 209 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. 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 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.069; Restrained GooF = 1.069 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0495 * P )^2 + 0.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.82767 0.00131 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.002 for tors H8A Max. shift = 0.000 A for H8A Max. dU = 0.000 for H11N Least-squares cycle 6 Maximum vector length = 511 Memory required = 2643 / 259978 wR2 = 0.0876 before cycle 6 for 3760 data and 209 / 209 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. 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 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.069; Restrained GooF = 1.069 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0495 * P )^2 + 0.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.82767 0.00131 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z C2 Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 -0.4254 -0.2214 1.3055 43 0.950 0.000 C2 C3 C1 H4 0.1814 -0.2327 1.4583 43 0.950 0.000 C4 C3 C5 H5 0.2196 -0.3578 1.4384 43 0.950 0.000 C5 C6 C4 H6 -0.0626 -0.4145 1.3536 43 0.950 0.000 C6 C5 C1 H8A -0.9597 -0.3753 1.1767 137 0.980 0.000 C8 C7 H8A H8B -0.7377 -0.4371 1.1964 137 0.980 0.000 C8 C7 H8A H8C -0.6983 -0.3903 1.1249 137 0.980 0.000 C8 C7 H8A H12 -0.2107 -0.0211 1.0765 43 0.950 0.000 C12 C13 C11 H14 0.3614 -0.1462 0.9717 43 0.950 0.000 C14 C13 C15 H15 0.2282 -0.2455 1.0420 43 0.950 0.000 C15 C16 C14 H16 -0.1184 -0.2334 1.1288 43 0.950 0.000 C16 C15 C11 H18A -0.6705 -0.0731 1.3003 137 0.980 0.000 C18 C17 H18A H18B -0.8099 -0.1307 1.2470 137 0.980 0.000 C18 C17 H18A H18C -0.9029 -0.0476 1.2437 137 0.980 0.000 C18 C17 H18A 2008lsh060 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.27065 -0.32415 1.32073 1.00000 0.02765 0.03193 0.02898 0.00423 0.00335 -0.00126 0.02952 0.00303 0.00036 0.00009 0.00009 0.00000 0.00087 0.00083 0.00080 0.00065 0.00066 0.00067 0.00037 C2 -0.29547 -0.24950 1.33233 1.00000 0.03215 0.02991 0.02861 0.00258 0.00298 -0.00348 0.03022 0.00313 0.00042 0.00009 0.00009 0.00000 0.00085 0.00080 0.00076 0.00064 0.00070 0.00072 0.00035 H2 -0.42536 -0.22141 1.30554 1.00000 0.03627 0.00000 0.00000 C3 -0.12625 -0.21786 1.38369 1.00000 0.03524 0.04252 0.03142 -0.00322 0.00913 -0.01043 0.03640 0.00320 0.00041 0.00010 0.00010 0.00000 0.00099 0.00099 0.00088 0.00074 0.00074 0.00081 0.00042 C4 0.06684 -0.25616 1.42363 1.00000 0.03121 0.07276 0.03052 -0.00391 -0.00045 -0.00624 0.04483 0.00369 0.00044 0.00013 0.00010 0.00000 0.00094 0.00144 0.00091 0.00093 0.00079 0.00101 0.00049 H4 0.18140 -0.23274 1.45827 1.00000 0.05379 0.00000 0.00000 C5 0.08850 -0.33008 1.41159 1.00000 0.03725 0.06527 0.04034 0.00422 -0.00321 0.01140 0.04762 0.00410 0.00046 0.00013 0.00012 0.00000 0.00102 0.00136 0.00105 0.00097 0.00089 0.00100 0.00050 H5 0.21959 -0.35776 1.43841 1.00000 0.05715 0.00000 0.00000 C6 -0.07888 -0.36386 1.36092 1.00000 0.03707 0.04236 0.03927 0.00763 0.00080 0.00619 0.03957 0.00375 0.00043 0.00011 0.00010 0.00000 0.00097 0.00101 0.00098 0.00082 0.00081 0.00088 0.00043 H6 -0.06263 -0.41450 1.35355 1.00000 0.04748 0.00000 0.00000 C7 -0.58979 -0.33485 1.21619 1.00000 0.03066 0.02471 0.03106 0.00295 0.00257 -0.00490 0.02881 0.00300 0.00038 0.00009 0.00009 0.00000 0.00084 0.00076 0.00081 0.00064 0.00067 0.00068 0.00035 C8 -0.76134 -0.38914 1.17495 1.00000 0.04160 0.03045 0.03900 0.00065 -0.00274 -0.00632 0.03702 0.00313 0.00042 0.00010 0.00010 0.00000 0.00109 0.00089 0.00093 0.00071 0.00079 0.00076 0.00043 H8A -0.95972 -0.37534 1.17670 1.00000 0.05553 0.00000 0.00000 H8B -0.73768 -0.43712 1.19641 1.00000 0.05553 0.00000 0.00000 H8C -0.69826 -0.39029 1.12490 1.00000 0.05553 0.00000 0.00000 N1 -0.43996 -0.36195 1.27140 1.00000 0.03420 0.02047 0.03434 0.00550 0.00066 -0.00083 0.02967 0.00261 0.00033 0.00008 0.00008 0.00000 0.00078 0.00064 0.00075 0.00056 0.00062 0.00058 0.00031 O1 -0.58725 -0.27067 1.19859 1.00000 0.05238 0.02548 0.04255 0.01180 -0.01074 -0.00527 0.04014 0.00232 0.00032 0.00006 0.00007 0.00000 0.00083 0.00059 0.00072 0.00054 0.00067 0.00060 0.00033 Cl1 0.19298 -0.00095 0.96898 1.00000 0.05761 0.03642 0.04608 0.01433 0.01070 -0.00535 0.04670 0.00097 0.00012 0.00003 0.00003 0.00000 0.00030 0.00023 0.00026 0.00020 0.00023 0.00023 0.00014 H1N -0.45596 -0.40788 1.28043 1.00000 0.04420 0.03689 0.00507 0.00087 0.00117 0.00000 0.00628 C11 -0.19842 -0.12663 1.11138 1.00000 0.02448 0.02296 0.02560 -0.00255 -0.00270 -0.00264 0.02435 0.00259 0.00035 0.00008 0.00008 0.00000 0.00071 0.00070 0.00071 0.00058 0.00063 0.00066 0.00030 C12 -0.12180 -0.06658 1.07006 1.00000 0.03193 0.02159 0.03137 0.00045 -0.00285 -0.00065 0.02830 0.00286 0.00037 0.00009 0.00009 0.00000 0.00087 0.00071 0.00081 0.00061 0.00067 0.00067 0.00035 H12 -0.21070 -0.02108 1.07650 1.00000 0.03396 0.00000 0.00000 C13 0.08869 -0.07581 1.01931 1.00000 0.03343 0.02891 0.02770 0.00467 -0.00291 -0.00666 0.03001 0.00293 0.00038 0.00009 0.00009 0.00000 0.00086 0.00083 0.00081 0.00064 0.00068 0.00069 0.00036 C14 0.22020 -0.14142 1.00742 1.00000 0.02862 0.03603 0.02750 -0.00225 0.00161 -0.00252 0.03072 0.00295 0.00038 0.00010 0.00009 0.00000 0.00084 0.00090 0.00077 0.00067 0.00066 0.00070 0.00036 H14 0.36139 -0.14616 0.97175 1.00000 0.03686 0.00000 0.00000 C15 0.14019 -0.20000 1.04902 1.00000 0.02909 0.02718 0.03410 -0.00530 -0.00089 0.00126 0.03012 0.00292 0.00038 0.00009 0.00009 0.00000 0.00089 0.00076 0.00084 0.00066 0.00067 0.00070 0.00036 H15 0.22819 -0.24554 1.04202 1.00000 0.03615 0.00000 0.00000 C16 -0.06621 -0.19282 1.10053 1.00000 0.02781 0.02183 0.03035 -0.00046 -0.00116 -0.00122 0.02666 0.00283 0.00036 0.00009 0.00009 0.00000 0.00079 0.00071 0.00081 0.00062 0.00068 0.00063 0.00032 H16 -0.11841 -0.23339 1.12879 1.00000 0.03199 0.00000 0.00000 C17 -0.51907 -0.06593 1.19756 1.00000 0.02710 0.02474 0.03265 -0.00341 -0.00337 0.00105 0.02816 0.00287 0.00035 0.00009 0.00009 0.00000 0.00081 0.00075 0.00085 0.00068 0.00067 0.00066 0.00035 C18 -0.74530 -0.08061 1.25188 1.00000 0.03436 0.03274 0.03461 -0.00583 0.00150 0.00071 0.03390 0.00308 0.00038 0.00010 0.00010 0.00000 0.00097 0.00087 0.00089 0.00072 0.00072 0.00070 0.00039 H18A -0.67052 -0.07313 1.30031 1.00000 0.05086 0.00000 0.00000 H18B -0.80991 -0.13066 1.24698 1.00000 0.05086 0.00000 0.00000 H18C -0.90294 -0.04760 1.24374 1.00000 0.05086 0.00000 0.00000 N11 -0.41213 -0.12462 1.16384 1.00000 0.02856 0.01712 0.02967 -0.00176 0.00076 -0.00139 0.02512 0.00236 0.00030 0.00007 0.00007 0.00000 0.00069 0.00061 0.00068 0.00052 0.00056 0.00055 0.00028 O11 -0.43282 -0.00406 1.18585 1.00000 0.04703 0.02045 0.04887 -0.00625 0.00759 -0.00154 0.03878 0.00232 0.00030 0.00007 0.00007 0.00000 0.00075 0.00056 0.00073 0.00054 0.00063 0.00057 0.00030 Cl2 -0.17004 -0.12507 1.39959 1.00000 0.06390 0.04321 0.04079 -0.01249 0.00538 -0.01668 0.04930 0.00086 0.00013 0.00003 0.00003 0.00000 0.00033 0.00026 0.00025 0.00020 0.00024 0.00026 0.00015 H11N -0.47760 -0.16598 1.17702 1.00000 0.02445 0.03065 0.00400 0.00085 0.00097 0.00000 0.00470 Final Structure Factor Calculation for 2008lsh060 in P2(1)2(1)2(1) Total number of l.s. parameters = 209 Maximum vector length = 511 Memory required = 2436 / 26068 wR2 = 0.0876 before cycle 7 for 3760 data and 2 / 209 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. 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 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.069; Restrained GooF = 1.069 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0495 * P )^2 + 0.32 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0349 for 3449 Fo > 4sig(Fo) and 0.0401 for all 3760 data wR2 = 0.0876, GooF = S = 1.069, Restrained GooF = 1.069 for all data Flack x parameter = 0.0224 with esd 0.0532 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 22.00 for non-hydrogen and 16.00 for hydrogen atoms Principal mean square atomic displacements U 0.0351 0.0303 0.0232 C1 0.0349 0.0317 0.0241 C2 0.0530 0.0333 0.0229 C3 0.0740 0.0312 0.0292 C4 0.0696 0.0422 0.0310 C5 0.0508 0.0372 0.0307 C6 0.0338 0.0321 0.0206 C7 0.0456 0.0379 0.0276 C8 0.0363 0.0342 0.0185 N1 0.0626 0.0384 0.0194 O1 0.0644 0.0529 0.0228 Cl1 0.0278 0.0263 0.0189 C11 0.0346 0.0288 0.0215 C12 0.0403 0.0270 0.0228 C13 0.0375 0.0283 0.0263 C14 0.0372 0.0290 0.0242 C15 0.0308 0.0277 0.0215 C16 0.0354 0.0256 0.0235 C17 0.0397 0.0346 0.0274 C18 0.0304 0.0282 0.0167 N11 0.0565 0.0407 0.0191 O11 0.0766 0.0438 0.0275 Cl2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.024 0.038 0.049 0.063 0.077 0.095 0.118 0.151 0.213 1.000 Number in group 404. 360. 367. 376. 380. 379. 368. 371. 380. 375. GooF 1.099 1.091 1.223 1.054 0.999 1.033 0.959 0.949 1.061 1.193 K 1.184 0.975 0.943 0.972 0.976 0.992 0.998 1.011 1.033 0.982 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.63 inf Number in group 384. 373. 372. 389. 376. 368. 376. 369. 374. 379. GooF 1.018 0.985 1.035 1.051 0.975 1.111 0.983 0.899 1.120 1.426 K 1.033 1.025 1.020 0.987 0.996 1.018 1.021 1.032 1.028 0.964 R1 0.103 0.078 0.067 0.055 0.039 0.039 0.029 0.024 0.025 0.030 Recommended weighting scheme: WGHT 0.0477 0.3385 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 0 8 730.24 961.28 4.67 0.254 2.09 3 3 0 45.65 25.19 4.60 0.041 1.54 2 7 1 11.90 2.81 4.39 0.014 1.76 0 2 9 -1.52 4.67 4.16 0.018 2.02 2 0 5 5.44 0.16 3.96 0.003 2.01 0 2 3 9709.17 12134.25 3.92 0.902 5.16 0 10 0 200.34 261.23 3.76 0.132 1.85 0 4 2 1980.09 2434.02 3.66 0.404 4.14 0 10 8 22.34 12.45 3.59 0.029 1.45 0 7 2 7.65 16.74 3.52 0.033 2.54 0 8 2 134.91 175.56 3.48 0.108 2.24 0 7 3 148.32 114.63 3.47 0.088 2.43 0 6 10 43.04 28.79 3.46 0.044 1.59 1 3 10 527.56 432.11 3.42 0.170 1.67 4 0 8 0.38 8.11 3.37 0.023 1.06 2 11 0 25.31 39.21 3.32 0.051 1.37 -1 3 10 527.54 436.28 3.26 0.171 1.67 0 8 8 153.48 121.08 3.24 0.090 1.64 0 4 0 2671.95 3203.54 3.18 0.463 4.62 0 21 2 7.60 21.12 3.16 0.038 0.88 -4 11 6 15.68 28.41 3.13 0.044 0.93 2 0 10 114.35 89.12 3.13 0.077 1.47 1 20 3 71.77 96.40 3.11 0.080 0.90 0 1 9 91.69 118.40 3.09 0.089 2.06 1 10 2 289.27 238.34 3.06 0.126 1.70 0 11 2 490.44 410.64 3.01 0.166 1.65 3 4 0 5.50 0.24 2.94 0.004 1.50 1 5 8 696.53 589.65 2.94 0.199 1.82 -4 9 3 428.16 356.28 2.94 0.154 1.02 0 15 18 99.62 69.59 2.93 0.068 0.79 -2 7 1 9.17 3.50 2.91 0.015 1.76 -3 18 3 22.24 37.59 2.91 0.050 0.85 4 9 2 13.71 6.08 2.91 0.020 1.02 3 16 10 292.80 233.71 2.91 0.125 0.84 1 19 14 65.51 43.88 2.90 0.054 0.78 -1 10 2 276.18 229.18 2.90 0.124 1.70 2 9 1 334.42 279.81 2.87 0.137 1.55 0 9 7 658.64 559.63 2.86 0.194 1.63 0 6 11 165.00 202.30 2.84 0.116 1.48 1 9 0 874.73 746.41 2.83 0.224 1.89 6 2 4 16.13 3.94 2.80 0.016 0.78 -1 13 9 17.05 27.05 2.80 0.043 1.14 0 3 6 516.76 610.68 2.79 0.202 2.77 -1 5 8 688.17 587.91 2.78 0.198 1.82 0 3 2 827.36 973.13 2.76 0.255 5.14 -3 6 9 72.05 92.89 2.76 0.079 1.17 3 13 15 191.11 151.40 2.74 0.101 0.81 2 12 0 1.91 7.70 2.73 0.023 1.29 1 22 3 10.79 1.10 2.73 0.009 0.82 -2 9 1 321.89 270.78 2.72 0.135 1.55 Bond lengths and angles C1 - Distance Angles C6 1.3912 (0.0026) C2 1.4027 (0.0024) 119.49 (0.18) N1 1.4089 (0.0023) 117.75 (0.16) 122.73 (0.16) C1 - C6 C2 C2 - Distance Angles C3 1.3817 (0.0026) C1 1.4027 (0.0024) 118.32 (0.18) H2 0.9500 120.84 120.84 C2 - C3 C1 C3 - Distance Angles C4 1.3793 (0.0030) C2 1.3817 (0.0026) 123.07 (0.19) Cl2 1.7544 (0.0020) 119.40 (0.16) 117.51 (0.16) C3 - C4 C2 C4 - Distance Angles C3 1.3793 (0.0030) C5 1.3895 (0.0033) 117.90 (0.19) H4 0.9500 121.05 121.05 C4 - C3 C5 C5 - Distance Angles C6 1.3850 (0.0031) C4 1.3895 (0.0033) 120.74 (0.19) H5 0.9500 119.63 119.63 C5 - C6 C4 C6 - Distance Angles C5 1.3850 (0.0031) C1 1.3912 (0.0026) 120.48 (0.20) H6 0.9500 119.76 119.76 C6 - C5 C1 C7 - Distance Angles O1 1.2317 (0.0020) N1 1.3489 (0.0023) 123.77 (0.16) C8 1.5059 (0.0024) 120.82 (0.16) 115.39 (0.15) C7 - O1 N1 C8 - Distance Angles C7 1.5059 (0.0024) 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 N1 - Distance Angles C7 1.3489 (0.0023) C1 1.4089 (0.0023) 128.06 (0.14) H1N 0.8696 (0.0155) 117.66 (1.56) 114.14 (1.52) N1 - C7 C1 O1 - Distance Angles C7 1.2317 (0.0020) O1 - Cl1 - Distance Angles C13 1.7447 (0.0017) Cl1 - C11 - Distance Angles C16 1.3919 (0.0022) C12 1.3999 (0.0023) 120.00 (0.15) N11 1.4123 (0.0021) 116.75 (0.14) 123.23 (0.15) C11 - C16 C12 C12 - Distance Angles C13 1.3892 (0.0025) C11 1.3999 (0.0023) 117.72 (0.16) H12 0.9500 121.14 121.14 C12 - C13 C11 C13 - Distance Angles C14 1.3838 (0.0026) C12 1.3892 (0.0025) 122.95 (0.16) Cl1 1.7447 (0.0017) 118.75 (0.14) 118.30 (0.13) C13 - C14 C12 C14 - Distance Angles C13 1.3838 (0.0026) C15 1.3858 (0.0025) 118.14 (0.16) H14 0.9500 120.93 120.93 C14 - C13 C15 C15 - Distance Angles C16 1.3808 (0.0025) C14 1.3858 (0.0025) 120.63 (0.16) H15 0.9500 119.68 119.68 C15 - C16 C14 C16 - Distance Angles C15 1.3808 (0.0025) C11 1.3919 (0.0022) 120.54 (0.15) H16 0.9500 119.73 119.73 C16 - C15 C11 C17 - Distance Angles O11 1.2356 (0.0021) N11 1.3540 (0.0021) 122.38 (0.16) C18 1.5036 (0.0024) 121.65 (0.15) 115.95 (0.15) C17 - O11 N11 C18 - Distance Angles C17 1.5036 (0.0024) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - C17 H18A H18B N11 - Distance Angles C17 1.3540 (0.0021) C11 1.4123 (0.0022) 127.86 (0.14) H11N 0.8619 (0.0144) 116.30 (1.29) 115.79 (1.29) N11 - C17 C11 O11 - Distance Angles C17 1.2356 (0.0021) O11 - Cl2 - Distance Angles C3 1.7544 (0.0020) Cl2 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.870(16) 1.960(16) 2.8129(19) 167(2) N1-H1N...O11_$1 0.862(14) 2.046(15) 2.9008(18) 171.4(18) N11-H11N...O1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)