+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0002r started at 17:54:19 on 20-Feb-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0002r in P2(1)/c CELL 0.71073 6.4630 12.9251 20.8621 90.000 93.690 90.000 ZERR 4.00 0.0008 0.0014 0.0023 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H B N O UNIT 68 104 4 4 12 V = 1739.10 F(000) = 656.0 Mu = 0.08 mm-1 Cell Wt = 1212.79 Rho = 1.158 MERG 2 OMIT -3.00 50.00 SHEL 7 0.84 FMAP 2 PLAN 10 SIZE 0.02 0.06 0.10 ACTA 50.00 BOND $H WGHT 0.00000 6.29740 L.S. 4 TEMP -153.00 FVAR 0.64349 MOLE 1 C14 1 -0.040511 -0.079039 0.096918 11.00000 0.04112 0.03860 = 0.03129 -0.00448 0.00135 0.00388 AFIX 43 H14 2 -0.182571 -0.098013 0.096658 11.00000 -1.20000 AFIX 0 C11 1 0.369288 -0.021188 0.098937 11.00000 0.04667 0.04429 = 0.03116 -0.00237 0.00022 0.00624 AFIX 43 H11 2 0.511044 -0.001814 0.098769 11.00000 -1.20000 AFIX 0 C15 1 0.046815 -0.020944 0.148114 11.00000 0.04950 0.04095 = 0.02540 0.00354 0.00739 0.00235 AFIX 43 H15 2 -0.036332 -0.001707 0.182105 11.00000 -1.20000 AFIX 0 C10 1 0.254135 0.009336 0.150197 11.00000 0.04099 0.04279 = 0.02383 0.00065 0.00010 0.00114 C13 1 0.073547 -0.109591 0.046802 11.00000 0.05389 0.03104 = 0.02551 -0.00003 -0.00377 0.00429 C3 1 0.384990 0.182736 0.291577 11.00000 0.03768 0.03689 = 0.02415 -0.00636 0.00152 -0.00528 C12 1 0.280911 -0.079182 0.048302 11.00000 0.05310 0.04794 = 0.02177 -0.00295 0.00789 0.01084 AFIX 43 H12 2 0.363031 -0.098499 0.014081 11.00000 -1.20000 AFIX 0 C16 1 -0.024111 -0.168040 -0.010194 11.00000 0.05668 0.04108 = 0.02753 0.00105 -0.00304 0.00186 AFIX 23 H16A 2 -0.156192 -0.199162 0.001760 11.00000 -1.20000 H16B 2 -0.056326 -0.118946 -0.045874 11.00000 -1.20000 AFIX 0 C7 1 0.340945 0.290242 0.264294 11.00000 0.05187 0.04589 = 0.03034 -0.00452 0.00347 -0.00179 AFIX 137 H7B 2 0.372847 0.291789 0.219012 11.00000 -1.50000 H7C 2 0.427311 0.341067 0.288426 11.00000 -1.50000 H7A 2 0.194308 0.307116 0.267870 11.00000 -1.50000 AFIX 0 C4 1 0.599777 0.141791 0.276608 11.00000 0.04521 0.05191 = 0.02312 -0.00834 -0.00137 -0.00126 C22 1 0.034300 -0.289972 -0.095177 11.00000 0.08614 0.04730 = 0.02011 -0.00576 -0.00199 0.00435 AFIX 23 H22B 2 0.025813 -0.233403 -0.127232 11.00000 -1.20000 H22A 2 -0.105984 -0.319741 -0.092417 11.00000 -1.20000 AFIX 0 C9 1 0.674016 0.050842 0.318521 11.00000 0.06525 0.04321 = 0.03602 -0.01058 -0.00727 0.01415 AFIX 137 H9C 2 0.563725 -0.001118 0.319105 11.00000 -1.50000 H9A 2 0.709131 0.075183 0.362366 11.00000 -1.50000 H9B 2 0.796930 0.019979 0.301045 11.00000 -1.50000 AFIX 0 C6 1 0.337972 0.179529 0.361918 11.00000 0.04953 0.04588 = 0.02881 -0.00491 0.01090 -0.00214 AFIX 137 H6B 2 0.198628 0.207107 0.366818 11.00000 -1.50000 H6A 2 0.439936 0.221542 0.387092 11.00000 -1.50000 H6C 2 0.345003 0.107868 0.377251 11.00000 -1.50000 AFIX 0 C21 1 0.182245 -0.372160 -0.115198 11.00000 0.10587 0.05489 = 0.03055 -0.01053 0.00913 0.01048 AFIX 23 H21B 2 0.132471 -0.400094 -0.157611 11.00000 -1.20000 H21A 2 0.320300 -0.340787 -0.119694 11.00000 -1.20000 AFIX 0 C18 1 0.125795 -0.334226 0.013777 11.00000 0.09499 0.04595 = 0.02210 -0.00101 -0.00127 0.01254 AFIX 23 H18B 2 -0.013012 -0.364985 0.017883 11.00000 -1.20000 H18A 2 0.176859 -0.307840 0.056455 11.00000 -1.20000 AFIX 0 C8 1 0.766948 0.223021 0.273986 11.00000 0.04584 0.06548 = 0.04037 -0.00590 0.00250 -0.00502 AFIX 137 H8B 2 0.897006 0.190189 0.263305 11.00000 -1.50000 H8A 2 0.786708 0.257171 0.315874 11.00000 -1.50000 H8C 2 0.725622 0.274421 0.241079 11.00000 -1.50000 AFIX 0 C19 1 0.270765 -0.414752 -0.008184 11.00000 0.13135 0.05982 = 0.03356 -0.00930 -0.00628 0.03084 AFIX 23 H19B 2 0.410787 -0.384453 -0.010456 11.00000 -1.20000 H19A 2 0.280381 -0.472138 0.023298 11.00000 -1.20000 AFIX 0 B1 3 0.353910 0.073916 0.206633 11.00000 0.04499 0.03878 = 0.02234 0.00904 -0.00164 0.00283 N17 4 0.110725 -0.249477 -0.032100 11.00000 0.06080 0.04597 = 0.01666 0.00008 0.00434 0.01241 O20 5 0.201183 -0.454307 -0.070046 11.00000 0.14400 0.04805 = 0.03851 -0.00461 0.00565 0.02349 O2 5 0.244894 0.111161 0.255718 11.00000 0.04646 0.04545 = 0.02775 -0.00696 0.00794 -0.00551 O5 5 0.558718 0.098558 0.211527 11.00000 0.04335 0.06291 = 0.02588 -0.00716 0.00216 0.00073 HKLF 4 Covalent radii and connectivity table for 2009src0002r in P2(1)/c C 0.770 H 0.320 B 0.820 N 0.700 O 0.660 C14 - C13 C15 C11 - C12 C10 C15 - C10 C14 C10 - C15 C11 B1 C13 - C14 C12 C16 C3 - O2 C6 C7 C4 C12 - C11 C13 C16 - N17 C13 C7 - C3 C4 - O5 C8 C9 C3 C22 - N17 C21 C9 - C4 C6 - C3 C21 - O20 C22 C18 - N17 C19 C8 - C4 C19 - O20 C18 B1 - O5 O2 C10 N17 - C18 C16 C22 O20 - C21 C19 O2 - B1 C3 O5 - B1 C4 13697 Reflections read, of which 2169 rejected -7 =< h =< 7, -14 =< k =< 15, -24 =< l =< 22, Max. 2-theta = 49.99 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) -1 13 2 2.88 1.99 2 14.50 1 Inconsistent equivalents 3017 Unique reflections, of which 0 suppressed R(int) = 0.1001 R(sigma) = 0.1062 Friedel opposites merged Maximum memory for data reduction = 2419 / 29949 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 = 3042 / 252595 wR2 = 0.2227 before cycle 1 for 3017 data and 203 / 203 parameters GooF = S = 1.081; Restrained GooF = 1.081 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.64352 0.00224 0.015 OSF Mean shift/su = 0.014 Maximum = -0.054 for U23 C8 Max. shift = 0.001 A for H9A Max. dU = 0.000 for C19 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3042 / 252595 wR2 = 0.2227 before cycle 2 for 3017 data and 203 / 203 parameters GooF = S = 1.081; Restrained GooF = 1.081 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.64356 0.00224 0.016 OSF Mean shift/su = 0.006 Maximum = 0.022 for U33 C18 Max. shift = 0.000 A for H9A Max. dU = 0.000 for C19 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3042 / 252595 wR2 = 0.2227 before cycle 3 for 3017 data and 203 / 203 parameters GooF = S = 1.081; Restrained GooF = 1.081 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.64357 0.00224 0.004 OSF Mean shift/su = 0.001 Maximum = 0.004 for OSF Max. shift = 0.000 A for H6B Max. dU = 0.000 for C8 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3042 / 252595 wR2 = 0.2227 before cycle 4 for 3017 data and 203 / 203 parameters GooF = S = 1.081; Restrained GooF = 1.081 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.64357 0.00224 0.001 OSF Mean shift/su = 0.000 Maximum = 0.001 for x C19 Max. shift = 0.000 A for H19A Max. dU = 0.000 for C15 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H14 -0.1826 -0.0980 0.0967 43 0.950 0.000 C14 C13 C15 H11 0.5110 -0.0018 0.0988 43 0.950 0.000 C11 C12 C10 H15 -0.0364 -0.0017 0.1821 43 0.950 0.000 C15 C10 C14 H12 0.3630 -0.0985 0.0141 43 0.950 0.000 C12 C11 C13 H16A -0.1562 -0.1992 0.0018 23 0.990 0.000 C16 N17 C13 H16B -0.0563 -0.1190 -0.0459 23 0.990 0.000 C16 N17 C13 H7B 0.3728 0.2918 0.2190 137 0.980 0.000 C7 C3 H7B H7C 0.4273 0.3411 0.2884 137 0.980 0.000 C7 C3 H7B H7A 0.1943 0.3071 0.2679 137 0.980 0.000 C7 C3 H7B H22B 0.0259 -0.2334 -0.1272 23 0.990 0.000 C22 N17 C21 H22A -0.1060 -0.3197 -0.0924 23 0.990 0.000 C22 N17 C21 H9C 0.5638 -0.0012 0.3191 137 0.980 0.000 C9 C4 H9C H9A 0.7090 0.0752 0.3624 137 0.980 0.000 C9 C4 H9C H9B 0.7970 0.0200 0.3011 137 0.980 0.000 C9 C4 H9C H6B 0.1986 0.2071 0.3668 137 0.980 0.000 C6 C3 H6B H6A 0.4399 0.2216 0.3871 137 0.980 0.000 C6 C3 H6B H6C 0.3451 0.1079 0.3772 137 0.980 0.000 C6 C3 H6B H21B 0.1324 -0.4001 -0.1576 23 0.990 0.000 C21 O20 C22 H21A 0.3203 -0.3408 -0.1197 23 0.990 0.000 C21 O20 C22 H18B -0.0130 -0.3650 0.0179 23 0.990 0.000 C18 N17 C19 H18A 0.1768 -0.3078 0.0564 23 0.990 0.000 C18 N17 C19 H8B 0.8970 0.1902 0.2633 137 0.980 0.000 C8 C4 H8B H8A 0.7867 0.2572 0.3159 137 0.980 0.000 C8 C4 H8B H8C 0.7256 0.2744 0.2411 137 0.980 0.000 C8 C4 H8B H19B 0.4108 -0.3845 -0.0104 23 0.990 0.000 C19 O20 C18 H19A 0.2803 -0.4721 0.0233 23 0.990 0.000 C19 O20 C18 2009src0002r in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C14 -0.04050 -0.07905 0.09692 1.00000 0.04124 0.03864 0.03125 -0.00437 0.00129 0.00388 0.03709 0.00892 0.00081 0.00039 0.00023 0.00000 0.00301 0.00325 0.00304 0.00253 0.00243 0.00246 0.00130 H14 -0.18255 -0.09804 0.09667 1.00000 0.04451 0.00000 0.00000 C11 0.36927 -0.02119 0.09894 1.00000 0.04662 0.04424 0.03117 -0.00250 0.00020 0.00618 0.04078 0.00938 0.00085 0.00042 0.00024 0.00000 0.00326 0.00345 0.00306 0.00265 0.00248 0.00265 0.00136 H11 0.51103 -0.00183 0.09878 1.00000 0.04893 0.00000 0.00000 C15 0.04681 -0.02095 0.14810 1.00000 0.04965 0.04095 0.02531 0.00341 0.00736 0.00228 0.03842 0.00913 0.00082 0.00040 0.00024 0.00000 0.00338 0.00329 0.00287 0.00251 0.00237 0.00262 0.00131 H15 -0.03636 -0.00170 0.18209 1.00000 0.04611 0.00000 0.00000 C10 0.25413 0.00934 0.15020 1.00000 0.04096 0.04278 0.02375 0.00071 0.00011 0.00115 0.03591 0.00874 0.00078 0.00041 0.00023 0.00000 0.00308 0.00336 0.00278 0.00245 0.00227 0.00251 0.00127 C13 0.07358 -0.10959 0.04680 1.00000 0.05389 0.03106 0.02546 -0.00003 -0.00375 0.00433 0.03708 0.00888 0.00084 0.00039 0.00023 0.00000 0.00343 0.00304 0.00283 0.00237 0.00245 0.00253 0.00128 C3 0.38499 0.18275 0.29158 1.00000 0.03772 0.03690 0.02419 -0.00642 0.00147 -0.00526 0.03296 0.00815 0.00074 0.00039 0.00023 0.00000 0.00282 0.00302 0.00266 0.00239 0.00214 0.00236 0.00119 C12 0.28091 -0.07919 0.04830 1.00000 0.05309 0.04779 0.02182 -0.00294 0.00792 0.01075 0.04066 0.00936 0.00084 0.00042 0.00024 0.00000 0.00348 0.00352 0.00281 0.00254 0.00248 0.00276 0.00137 H12 0.36305 -0.09850 0.01409 1.00000 0.04879 0.00000 0.00000 C16 -0.02409 -0.16805 -0.01019 1.00000 0.05675 0.04107 0.02752 0.00103 -0.00303 0.00196 0.04203 0.00895 0.00085 0.00042 0.00024 0.00000 0.00346 0.00342 0.00295 0.00254 0.00251 0.00277 0.00138 H16A -0.15617 -0.19916 0.00177 1.00000 0.05043 0.00000 0.00000 H16B -0.05631 -0.11896 -0.04587 1.00000 0.05043 0.00000 0.00000 C7 0.34092 0.29024 0.26428 1.00000 0.05187 0.04596 0.03044 -0.00456 0.00330 -0.00181 0.04273 0.00922 0.00084 0.00041 0.00024 0.00000 0.00339 0.00359 0.00296 0.00266 0.00253 0.00272 0.00140 H7B 0.37278 0.29176 0.21900 1.00000 0.06410 0.00000 0.00000 H7C 0.42731 0.34107 0.28840 1.00000 0.06410 0.00000 0.00000 H7A 0.19429 0.30711 0.26787 1.00000 0.06410 0.00000 0.00000 C4 0.59976 0.14178 0.27661 1.00000 0.04519 0.05171 0.02316 -0.00831 -0.00141 -0.00121 0.04018 0.00878 0.00080 0.00044 0.00023 0.00000 0.00316 0.00362 0.00280 0.00255 0.00233 0.00265 0.00136 C22 0.03433 -0.28998 -0.09517 1.00000 0.08618 0.04744 0.02009 -0.00580 -0.00200 0.00433 0.05147 0.00985 0.00099 0.00045 0.00024 0.00000 0.00455 0.00377 0.00284 0.00266 0.00282 0.00321 0.00162 H22B 0.02589 -0.23340 -0.12722 1.00000 0.06177 0.00000 0.00000 H22A -0.10597 -0.31973 -0.09242 1.00000 0.06177 0.00000 0.00000 C9 0.67401 0.05083 0.31852 1.00000 0.06513 0.04329 0.03608 -0.01061 -0.00731 0.01409 0.04862 0.00982 0.00092 0.00043 0.00025 0.00000 0.00389 0.00353 0.00330 0.00274 0.00282 0.00290 0.00154 H9C 0.56377 -0.00116 0.31907 1.00000 0.07293 0.00000 0.00000 H9A 0.70896 0.07516 0.36238 1.00000 0.07293 0.00000 0.00000 H9B 0.79702 0.02002 0.30108 1.00000 0.07293 0.00000 0.00000 C6 0.33799 0.17952 0.36191 1.00000 0.04952 0.04598 0.02876 -0.00505 0.01097 -0.00217 0.04106 0.00915 0.00081 0.00043 0.00023 0.00000 0.00327 0.00342 0.00300 0.00261 0.00245 0.00267 0.00135 H6B 0.19863 0.20707 0.36682 1.00000 0.06159 0.00000 0.00000 H6A 0.43993 0.22155 0.38709 1.00000 0.06159 0.00000 0.00000 H6C 0.34507 0.10786 0.37724 1.00000 0.06159 0.00000 0.00000 C21 0.18221 -0.37217 -0.11519 1.00000 0.10611 0.05491 0.03055 -0.01063 0.00900 0.01047 0.06366 0.01170 0.00112 0.00049 0.00027 0.00000 0.00554 0.00433 0.00330 0.00318 0.00336 0.00373 0.00190 H21B 0.13240 -0.40010 -0.15760 1.00000 0.07639 0.00000 0.00000 H21A 0.32027 -0.34081 -0.11970 1.00000 0.07639 0.00000 0.00000 C18 0.12578 -0.33422 0.01377 1.00000 0.09480 0.04601 0.02233 -0.00107 -0.00134 0.01259 0.05460 0.01076 0.00102 0.00044 0.00025 0.00000 0.00485 0.00375 0.00297 0.00274 0.00298 0.00340 0.00169 H18B -0.01303 -0.36498 0.01787 1.00000 0.06552 0.00000 0.00000 H18A 0.17682 -0.30784 0.05645 1.00000 0.06552 0.00000 0.00000 C8 0.76694 0.22303 0.27399 1.00000 0.04591 0.06550 0.04053 -0.00613 0.00235 -0.00499 0.05066 0.00955 0.00084 0.00047 0.00027 0.00000 0.00332 0.00422 0.00345 0.00306 0.00270 0.00304 0.00156 H8B 0.89700 0.19020 0.26331 1.00000 0.07599 0.00000 0.00000 H8A 0.78668 0.25718 0.31588 1.00000 0.07599 0.00000 0.00000 H8C 0.72561 0.27443 0.24108 1.00000 0.07599 0.00000 0.00000 C19 0.27074 -0.41476 -0.00817 1.00000 0.13153 0.05993 0.03356 -0.00933 -0.00635 0.03100 0.07551 0.01252 0.00126 0.00052 0.00028 0.00000 0.00664 0.00448 0.00366 0.00329 0.00390 0.00437 0.00229 H19B 0.41078 -0.38447 -0.01044 1.00000 0.09061 0.00000 0.00000 H19A 0.28032 -0.47214 0.02331 1.00000 0.09061 0.00000 0.00000 B1 0.35389 0.07391 0.20662 1.00000 0.04484 0.03889 0.02239 0.00907 -0.00154 0.00278 0.03553 0.01075 0.00095 0.00047 0.00028 0.00000 0.00371 0.00371 0.00321 0.00273 0.00269 0.00289 0.00147 N17 0.11070 -0.24949 -0.03210 1.00000 0.06096 0.04594 0.01659 0.00007 0.00438 0.01236 0.04108 0.00767 0.00069 0.00034 0.00019 0.00000 0.00293 0.00289 0.00215 0.00207 0.00198 0.00229 0.00114 O20 0.20117 -0.45431 -0.07005 1.00000 0.14393 0.04814 0.03852 -0.00463 0.00560 0.02361 0.07687 0.00826 0.00082 0.00033 0.00019 0.00000 0.00470 0.00276 0.00260 0.00219 0.00275 0.00276 0.00155 O2 0.24490 0.11115 0.25572 1.00000 0.04640 0.04559 0.02783 -0.00688 0.00790 -0.00561 0.03970 0.00576 0.00052 0.00027 0.00015 0.00000 0.00218 0.00228 0.00196 0.00174 0.00163 0.00175 0.00092 O5 0.55872 0.09856 0.21153 1.00000 0.04338 0.06296 0.02589 -0.00719 0.00217 0.00066 0.04408 0.00605 0.00053 0.00030 0.00016 0.00000 0.00222 0.00262 0.00197 0.00185 0.00162 0.00188 0.00098 Final Structure Factor Calculation for 2009src0002r in P2(1)/c Total number of l.s. parameters = 203 Maximum vector length = 511 Memory required = 2839 / 24017 wR2 = 0.2227 before cycle 5 for 3017 data and 0 / 203 parameters GooF = S = 1.081; Restrained GooF = 1.081 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1050 for 1725 Fo > 4sig(Fo) and 0.1909 for all 3017 data wR2 = 0.2227, GooF = S = 1.081, Restrained GooF = 1.081 for all data Occupancy sum of asymmetric unit = 22.00 for non-hydrogen and 26.00 for hydrogen atoms Principal mean square atomic displacements U 0.0452 0.0370 0.0291 C14 0.0525 0.0392 0.0307 C11 0.0511 0.0406 0.0235 C15 0.0434 0.0408 0.0236 C10 0.0564 0.0304 0.0244 C13 0.0433 0.0343 0.0213 C3 0.0616 0.0410 0.0195 C12 0.0584 0.0410 0.0267 C16 0.0525 0.0466 0.0292 C7 0.0540 0.0460 0.0206 C4 0.0877 0.0479 0.0188 C22 0.0780 0.0394 0.0285 C9 0.0538 0.0450 0.0244 C6 0.1082 0.0577 0.0252 C21 0.0986 0.0430 0.0222 C18 0.0678 0.0453 0.0388 C8 0.1460 0.0500 0.0306 C19 0.0460 0.0427 0.0179 B1 0.0679 0.0390 0.0163 N17 0.1497 0.0461 0.0349 O20 0.0540 0.0405 0.0246 O2 0.0644 0.0434 0.0245 O5 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.014 0.021 0.029 0.038 0.049 0.065 0.090 0.131 1.000 Number in group 324. 316. 294. 287. 291. 299. 307. 296. 301. 302. GooF 1.111 1.135 1.095 1.157 1.162 1.078 1.084 0.958 0.987 1.022 K 14.957 3.602 1.697 1.453 1.102 0.984 1.025 1.018 1.011 1.007 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.15 1.26 1.44 1.80 inf Number in group 310. 300. 299. 297. 302. 307. 303. 295. 300. 304. GooF 1.198 1.217 1.202 1.155 1.172 1.002 0.997 0.942 0.842 1.009 K 1.484 1.197 1.286 1.164 1.104 1.001 1.011 0.961 0.983 1.010 R1 0.483 0.441 0.421 0.308 0.233 0.152 0.132 0.120 0.081 0.044 Recommended weighting scheme: WGHT 0.0000 6.2394 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)/su Fc/Fc(max) Resolution(A) 0 15 4 264.37 74.56 3.72 0.057 0.85 0 6 5 1173.91 1586.50 3.64 0.261 1.91 0 10 2 130.28 272.02 3.48 0.108 1.28 -5 0 16 243.69 23.22 3.42 0.032 0.95 1 0 0 823.99 1188.79 3.25 0.226 6.45 6 8 1 81.77 3.62 3.23 0.012 0.89 -1 2 1 12271.30 13874.01 3.20 0.773 4.50 -7 4 7 71.75 6.53 3.18 0.017 0.86 1 14 3 179.45 32.28 3.15 0.037 0.91 -6 5 14 70.66 2.99 3.08 0.011 0.85 5 9 5 93.77 6.79 3.06 0.017 0.93 -4 10 1 550.12 346.68 3.04 0.122 1.01 -6 0 10 504.71 270.92 3.03 0.108 0.98 0 12 6 612.66 352.03 3.00 0.123 1.03 -3 6 9 48.52 3.27 3.00 0.012 1.30 6 7 6 118.00 23.16 2.97 0.032 0.89 4 11 5 96.74 1.51 2.97 0.008 0.92 1 5 5 11608.23 10341.79 2.95 0.667 2.06 1 2 3 33.58 1.21 2.93 0.007 3.74 1 13 7 -39.04 60.98 2.89 0.051 0.93 3 5 17 1.58 93.16 2.89 0.063 0.96 0 3 10 25.05 90.58 2.84 0.062 1.87 -4 2 13 33.15 125.49 2.84 0.074 1.16 0 3 23 185.52 18.11 2.84 0.028 0.89 5 3 5 233.16 389.18 2.83 0.129 1.17 2 12 11 -2.43 97.58 2.83 0.065 0.89 6 7 9 90.09 17.46 2.82 0.027 0.85 0 6 15 20.56 119.75 2.80 0.072 1.17 -6 0 8 69.73 5.42 2.77 0.015 1.02 -3 2 17 59.19 0.74 2.76 0.006 1.08 0 11 14 97.78 4.04 2.76 0.013 0.92 5 0 4 47.61 0.07 2.76 0.002 1.23 6 5 5 96.26 25.12 2.74 0.033 0.95 -1 8 16 253.95 117.10 2.73 0.071 1.01 -4 4 9 1.61 47.40 2.72 0.045 1.26 5 9 9 -30.91 41.43 2.72 0.042 0.87 -3 6 10 -27.17 37.54 2.69 0.040 1.26 1 15 4 171.54 2.02 2.68 0.009 0.84 -4 3 21 241.47 115.01 2.66 0.070 0.85 1 11 16 145.93 11.51 2.66 0.022 0.86 2 11 4 62.26 6.62 2.64 0.017 1.08 -1 3 24 145.63 14.94 2.63 0.025 0.85 -1 9 14 87.85 0.39 2.63 0.004 1.03 -2 4 21 126.81 24.74 2.61 0.033 0.92 -1 8 21 249.71 110.84 2.60 0.069 0.84 -2 6 16 511.72 758.15 2.59 0.181 1.07 2 6 9 22.80 92.34 2.58 0.063 1.39 0 5 20 115.25 18.59 2.57 0.028 0.97 -4 7 16 -23.75 27.70 2.57 0.035 0.91 4 3 14 26.42 107.83 2.56 0.068 1.03 Bond lengths and angles C14 - Distance Angles C13 1.3756 (0.0068) C15 1.3946 (0.0068) 121.76 (0.51) H14 0.9500 119.12 119.12 C14 - C13 C15 C11 - Distance Angles C12 1.3879 (0.0070) C10 1.3983 (0.0068) 121.42 (0.52) H11 0.9500 119.29 119.29 C11 - C12 C10 C15 - Distance Angles C10 1.3939 (0.0069) C14 1.3946 (0.0068) 121.07 (0.50) H15 0.9500 119.47 119.47 C15 - C10 C14 C10 - Distance Angles C15 1.3939 (0.0069) C11 1.3983 (0.0068) 117.03 (0.47) B1 1.5493 (0.0076) 121.83 (0.48) 121.14 (0.48) C10 - C15 C11 C13 - Distance Angles C14 1.3756 (0.0068) C12 1.3948 (0.0072) 117.59 (0.47) C16 1.5120 (0.0068) 121.61 (0.49) 120.69 (0.48) C13 - C14 C12 C3 - Distance Angles O2 1.4658 (0.0055) C6 1.5181 (0.0063) 108.69 (0.39) C7 1.5214 (0.0070) 106.91 (0.38) 110.03 (0.42) C4 1.5363 (0.0070) 102.43 (0.37) 115.26 (0.41) 112.86 (0.43) C3 - O2 C6 C7 C12 - Distance Angles C11 1.3879 (0.0070) C13 1.3948 (0.0072) 121.13 (0.51) H12 0.9500 119.44 119.44 C12 - C11 C13 C16 - Distance Angles N17 1.4584 (0.0065) C13 1.5120 (0.0068) 112.30 (0.43) H16A 0.9900 109.14 109.14 H16B 0.9900 109.14 109.14 107.87 C16 - N17 C13 H16A C7 - Distance Angles C3 1.5214 (0.0070) H7B 0.9800 109.47 H7C 0.9800 109.47 109.47 H7A 0.9800 109.47 109.47 109.47 C7 - C3 H7B H7C C4 - Distance Angles O5 1.4763 (0.0057) C8 1.5102 (0.0074) 108.45 (0.42) C9 1.5241 (0.0073) 105.49 (0.42) 110.95 (0.45) C3 1.5363 (0.0070) 101.90 (0.37) 115.19 (0.47) 113.85 (0.45) C4 - O5 C8 C9 C22 - Distance Angles N17 1.4715 (0.0062) C21 1.5060 (0.0079) 108.46 (0.47) H22B 0.9900 110.00 110.00 H22A 0.9900 110.00 110.00 108.37 C22 - N17 C21 H22B C9 - Distance Angles C4 1.5241 (0.0073) H9C 0.9800 109.47 H9A 0.9800 109.47 109.47 H9B 0.9800 109.47 109.47 109.47 C9 - C4 H9C H9A C6 - Distance Angles C3 1.5181 (0.0063) H6B 0.9800 109.47 H6A 0.9800 109.47 109.47 H6C 0.9800 109.47 109.47 109.47 C6 - C3 H6B H6A C21 - Distance Angles O20 1.4193 (0.0069) C22 1.5060 (0.0079) 111.89 (0.49) H21B 0.9900 109.24 109.24 H21A 0.9900 109.24 109.24 107.92 C21 - O20 C22 H21B C18 - Distance Angles N17 1.4535 (0.0066) C19 1.4920 (0.0082) 109.91 (0.49) H18B 0.9900 109.68 109.68 H18A 0.9900 109.68 109.68 108.18 C18 - N17 C19 H18B C8 - Distance Angles C4 1.5102 (0.0074) H8B 0.9800 109.47 H8A 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C4 H8B H8A C19 - Distance Angles O20 1.4336 (0.0069) C18 1.4920 (0.0082) 110.99 (0.54) H19B 0.9900 109.44 109.44 H19A 0.9900 109.44 109.44 108.04 C19 - O20 C18 H19B B1 - Distance Angles O5 1.3590 (0.0067) O2 1.3674 (0.0067) 114.04 (0.47) C10 1.5493 (0.0076) 122.63 (0.50) 123.33 (0.49) B1 - O5 O2 N17 - Distance Angles C18 1.4535 (0.0066) C16 1.4584 (0.0065) 110.71 (0.41) C22 1.4715 (0.0062) 108.97 (0.43) 111.36 (0.41) N17 - C18 C16 O20 - Distance Angles C21 1.4193 (0.0069) C19 1.4336 (0.0069) 109.84 (0.48) O20 - C21 O2 - Distance Angles B1 1.3674 (0.0068) C3 1.4658 (0.0055) 105.87 (0.39) O2 - B1 O5 - Distance Angles B1 1.3590 (0.0067) C4 1.4763 (0.0057) 105.93 (0.41) O5 - B1 FMAP and GRID set by program FMAP 2 1 16 GRID -3.846 -2 -1 3.846 2 1 R1 = 0.1909 for 3017 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.30 at 0.4949 0.7066 0.4199 [ 2.20 A from H21A ] Deepest hole -0.31 at 0.2937 0.6037 0.2391 [ 0.92 A from C4 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 3213 / 27451 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4949 -0.2066 -0.0801 1.00000 0.05 0.30 2.20 H21A 2.60 H12 2.72 H11 2.74 H16A Q2 1 0.6175 0.0451 0.0962 1.00000 0.05 0.28 0.92 H11 1.82 C11 2.26 H14 2.41 H12 Q3 1 0.5559 -0.2138 -0.1051 1.00000 0.05 0.27 2.25 H21A 2.58 H22A 2.65 H7B 2.74 O5 Q4 1 0.2758 0.0352 0.2664 1.00000 0.05 0.27 1.02 O2 1.46 B1 2.09 C3 2.15 H9C Q5 1 0.6742 0.1157 0.1117 1.00000 0.05 0.26 1.86 H11 2.27 O5 2.47 H22B 2.63 H12 Q6 1 0.1501 -0.5293 -0.0905 1.00000 0.05 0.24 1.10 O20 1.78 H6C 2.11 C21 2.18 H21B Q7 1 0.4394 -0.0622 0.1686 1.00000 0.05 0.24 1.54 C10 1.58 C11 1.74 H7C 1.74 H11 Q8 1 -0.1546 -0.0336 0.1230 1.00000 0.05 0.24 1.01 H14 1.11 C14 1.38 C15 1.47 H15 Q9 1 0.6077 -0.0442 0.1151 1.00000 0.05 0.23 0.88 H11 1.58 C11 1.59 H14 2.37 C14 Q10 1 0.5055 -0.3190 -0.0008 1.00000 0.05 0.23 1.06 H19B 1.96 C19 2.43 H6A 2.50 C18 Shortest distances between peaks (including symmetry equivalents) 1 3 0.68 2 5 1.03 2 9 1.22 8 9 1.54 7 9 1.62 1 5 1.71 2 8 1.85 3 5 1.95 5 9 2.11 1 10 2.20 1 2 2.23 5 8 2.23 2 7 2.40 2 3 2.46 3 10 2.60 4 7 2.67 7 8 2.87 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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. 0.61: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.70: Structure factors and derivatives 0.86: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.11: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0002r finished at 17:54:22 Total CPU time: 2.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++