+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0348 started at 17:16:10 on 14-Mar-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0348 in P2(1)/n CELL 0.71073 15.5139 5.6320 18.7366 90.000 93.038 90.000 ZERR 4.00 0.0003 0.0001 0.0004 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H O UNIT 88 72 8 V = 1634.80 F(000) = 664.0 Mu = 0.08 mm-1 Cell Wt = 1257.46 Rho = 1.277 MERG 2 OMIT -3.00 55.00 OMIT 4 0 0 OMIT 0 1 15 OMIT -12 2 2 OMIT 11 2 1 FMAP 2 PLAN 20 SIZE 0.20 0.20 0.50 ACTA BOND WGHT 0.05710 1.12030 L.S. 4 TEMP -153.00 FVAR 0.73502 C1 1 0.100562 0.194899 0.937336 11.00000 0.01847 0.01519 = 0.02315 0.00153 0.00330 0.00097 AFIX 13 H1 2 0.119275 0.025155 0.940552 11.00000 -1.20000 AFIX 0 C2 1 0.155358 0.341543 0.993850 11.00000 0.02290 0.01409 = 0.02195 -0.00017 0.00220 0.00116 C3 1 0.109678 0.280283 0.861633 11.00000 0.01804 0.01783 = 0.01978 0.00062 -0.00069 -0.00275 C4 1 0.160053 0.150932 0.816267 11.00000 0.02271 0.02278 = 0.02290 0.00116 -0.00116 0.00201 AFIX 43 H4 2 0.187903 0.009893 0.833085 11.00000 -1.20000 AFIX 0 C5 1 0.170011 0.226279 0.746485 11.00000 0.02946 0.03562 = 0.02181 -0.00153 0.00424 0.00328 AFIX 43 H5 2 0.204808 0.137239 0.715970 11.00000 -1.20000 AFIX 0 C6 1 0.129368 0.430338 0.721538 11.00000 0.02995 0.03618 = 0.02141 0.00718 0.00100 -0.00523 AFIX 43 H6 2 0.136292 0.481881 0.673905 11.00000 -1.20000 AFIX 0 C7 1 0.078305 0.560391 0.766138 11.00000 0.02637 0.02349 = 0.02754 0.00734 -0.00376 -0.00153 AFIX 43 H7 2 0.050020 0.700231 0.748866 11.00000 -1.20000 AFIX 0 C8 1 0.068614 0.486033 0.835914 11.00000 0.02388 0.01865 = 0.02490 0.00016 0.00115 0.00038 AFIX 43 H8 2 0.033854 0.575664 0.866308 11.00000 -1.20000 AFIX 0 C9 1 0.250509 0.320740 0.977499 11.00000 0.02142 0.01940 = 0.01632 -0.00110 -0.00071 -0.00113 C10 1 0.296208 0.115579 0.996472 11.00000 0.02756 0.02179 = 0.02148 0.00187 0.00029 0.00252 AFIX 43 H10 2 0.268269 -0.010205 1.019896 11.00000 -1.20000 AFIX 0 C11 1 0.382580 0.094132 0.981261 11.00000 0.02716 0.02830 = 0.03019 0.00327 -0.00274 0.00665 AFIX 43 H11 2 0.413592 -0.045459 0.994980 11.00000 -1.20000 AFIX 0 C12 1 0.423697 0.274481 0.946308 11.00000 0.02033 0.03522 = 0.02927 -0.00245 -0.00123 -0.00052 AFIX 43 H12 2 0.482728 0.258943 0.935990 11.00000 -1.20000 AFIX 0 C13 1 0.378485 0.477389 0.926468 11.00000 0.02375 0.02933 = 0.03079 0.00437 0.00128 -0.00529 AFIX 43 H13 2 0.406422 0.601469 0.902275 11.00000 -1.20000 AFIX 0 C14 1 0.292128 0.500413 0.941841 11.00000 0.02447 0.01997 = 0.02723 0.00330 -0.00092 -0.00022 AFIX 43 H14 2 0.261336 0.640096 0.927854 11.00000 -1.20000 AFIX 0 C15 1 0.142042 0.250749 1.066588 11.00000 0.02443 0.02156 = 0.02380 -0.00209 0.00177 0.00163 C16 1 0.135508 0.191219 1.127660 11.00000 0.02173 0.02263 = 0.02347 -0.00208 0.00101 0.00241 C17 1 0.132487 0.138348 1.202671 11.00000 0.01871 0.02182 = 0.01934 -0.00065 0.00097 0.00345 C18 1 0.169515 0.299042 1.252195 11.00000 0.02815 0.02338 = 0.02631 -0.00308 0.00203 -0.00229 AFIX 43 H18 2 0.195178 0.441116 1.236095 11.00000 -1.20000 AFIX 0 C19 1 0.168867 0.251598 1.324641 11.00000 0.03871 0.03572 = 0.02302 -0.00728 -0.00097 -0.00024 AFIX 43 H19 2 0.194392 0.361208 1.358007 11.00000 -1.20000 AFIX 0 C20 1 0.131396 0.046062 1.348893 11.00000 0.03323 0.04334 = 0.01987 0.00585 0.00473 0.00912 AFIX 43 H20 2 0.131075 0.014620 1.398692 11.00000 -1.20000 AFIX 0 C21 1 0.094243 -0.114096 1.300025 11.00000 0.03083 0.03211 = 0.03633 0.00952 0.00735 0.00178 AFIX 43 H21 2 0.068037 -0.254880 1.316495 11.00000 -1.20000 AFIX 0 C22 1 0.095223 -0.069482 1.227349 11.00000 0.02657 0.02736 = 0.02822 -0.00105 -0.00115 -0.00251 AFIX 43 H22 2 0.070417 -0.180879 1.194184 11.00000 -1.20000 AFIX 0 O1 3 0.012058 0.210250 0.956797 11.00000 0.02113 0.02052 = 0.02991 0.00025 0.00675 -0.00479 AFIX 147 H1A 2 -0.013410 0.082139 0.946540 11.00000 -1.50000 AFIX 0 O2 3 0.132570 0.586468 0.989608 11.00000 0.02488 0.01530 = 0.03186 -0.00123 0.00494 0.00178 AFIX 147 H2 2 0.082854 0.605320 1.004399 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 2007src0348 in P2(1)/n C 0.770 H 0.320 O 0.660 C1 - O1 C3 C2 C2 - O2 C15 C9 C1 C3 - C4 C8 C1 C4 - C3 C5 C5 - C6 C4 C6 - C5 C7 C7 - C8 C6 C8 - C7 C3 C9 - C14 C10 C2 C10 - C11 C9 C11 - C12 C10 C12 - C13 C11 C13 - C12 C14 C14 - C9 C13 C15 - C16 C2 C16 - C15 C17 C17 - C22 C18 C16 C18 - C19 C17 C19 - C20 C18 C20 - C19 C21 C21 - C22 C20 C22 - C21 C17 O1 - C1 O2 - C2 h k l Fo^2 Sigma Why rejected 13 0 0 35.17 8.70 observed but should be systematically absent -14 0 1 47.02 10.99 observed but should be systematically absent -13 0 2 54.29 8.43 observed but should be systematically absent -13 0 2 30.13 6.15 observed but should be systematically absent -12 0 3 268.07 47.55 observed but should be systematically absent -12 0 3 347.20 40.71 observed but should be systematically absent -1 0 14 43.92 10.54 observed but should be systematically absent -1 0 14 40.76 9.35 observed but should be systematically absent 1 0 14 33.42 5.98 observed but should be systematically absent 0 0 15 23.66 5.66 observed but should be systematically absent -1 0 16 44.00 7.65 observed but should be systematically absent 1 0 16 185.17 34.13 observed but should be systematically absent 1 0 16 189.03 44.57 observed but should be systematically absent 0 0 19 75.41 11.40 observed but should be systematically absent 0 0 19 91.33 8.68 observed but should be systematically absent 20110 Reflections read, of which 1158 rejected -18 =< h =< 20, -7 =< k =< 7, -24 =< l =< 21, Max. 2-theta = 54.98 15 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -8 1 5 51.73 3.45 7 29.06 6 2 21 -1.93 8.22 2 41.26 2 Inconsistent equivalents 3754 Unique reflections, of which 0 suppressed R(int) = 0.0757 R(sigma) = 0.0572 Friedel opposites merged Maximum memory for data reduction = 2027 / 37966 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 = 2630 / 270319 wR2 = 0.1548 before cycle 1 for 3754 data and 219 / 219 parameters GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0571 * P )^2 + 1.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.73442 0.00192 -0.312 OSF Mean shift/esd = 0.048 Maximum = -0.312 for OSF Max. shift = 0.002 A for H2 Max. dU = 0.000 for C6 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2630 / 270319 wR2 = 0.1548 before cycle 2 for 3754 data and 219 / 219 parameters GooF = S = 1.123; Restrained GooF = 1.123 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0571 * P )^2 + 1.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.73418 0.00191 -0.125 OSF Mean shift/esd = 0.016 Maximum = -0.125 for OSF Max. shift = 0.001 A for H2 Max. dU = 0.000 for C6 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2630 / 270319 wR2 = 0.1548 before cycle 3 for 3754 data and 219 / 219 parameters GooF = S = 1.124; Restrained GooF = 1.124 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0571 * P )^2 + 1.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.73418 0.00191 -0.001 OSF Mean shift/esd = 0.001 Maximum = 0.009 for tors H2 Max. shift = 0.000 A for H2 Max. dU = 0.000 for C5 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2630 / 270319 wR2 = 0.1548 before cycle 4 for 3754 data and 219 / 219 parameters GooF = S = 1.124; Restrained GooF = 1.124 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0571 * P )^2 + 1.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.73418 0.00191 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.002 for tors H2 Max. shift = 0.000 A for H2 Max. dU = 0.000 for C16 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 H1 0.1193 0.0252 0.9406 13 1.000 0.000 C1 O1 C3 C2 H4 0.1879 0.0099 0.8331 43 0.950 0.000 C4 C3 C5 H5 0.2048 0.1372 0.7160 43 0.950 0.000 C5 C6 C4 H6 0.1363 0.4819 0.6739 43 0.950 0.000 C6 C5 C7 H7 0.0500 0.7002 0.7489 43 0.950 0.000 C7 C8 C6 H8 0.0338 0.5756 0.8663 43 0.950 0.000 C8 C7 C3 H10 0.2683 -0.0102 1.0199 43 0.950 0.000 C10 C11 C9 H11 0.4136 -0.0455 0.9950 43 0.950 0.000 C11 C12 C10 H12 0.4827 0.2590 0.9360 43 0.950 0.000 C12 C13 C11 H13 0.4064 0.6015 0.9023 43 0.950 0.000 C13 C12 C14 H14 0.2613 0.6401 0.9279 43 0.950 0.000 C14 C9 C13 H18 0.1952 0.4411 1.2361 43 0.950 0.000 C18 C19 C17 H19 0.1944 0.3612 1.3580 43 0.950 0.000 C19 C20 C18 H20 0.1311 0.0146 1.3987 43 0.950 0.000 C20 C19 C21 H21 0.0680 -0.2549 1.3165 43 0.950 0.000 C21 C22 C20 H22 0.0704 -0.1809 1.1942 43 0.950 0.000 C22 C21 C17 H1A -0.0134 0.0822 0.9465 147 0.840 0.000 O1 C1 H1A H2 0.0829 0.6054 1.0046 147 0.840 0.000 O2 C2 H2 2007src0348 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.10057 0.19494 0.93734 1.00000 0.01829 0.01505 0.02319 0.00146 0.00333 0.00097 0.01876 0.00330 0.00012 0.00033 0.00010 0.00000 0.00092 0.00087 0.00099 0.00074 0.00073 0.00074 0.00040 H1 0.11928 0.02519 0.94056 1.00000 0.02251 0.00000 0.00000 C2 0.15536 0.34150 0.99384 1.00000 0.02282 0.01396 0.02192 -0.00015 0.00218 0.00116 0.01953 0.00333 0.00012 0.00032 0.00010 0.00000 0.00099 0.00087 0.00099 0.00073 0.00074 0.00076 0.00041 C3 0.10968 0.28026 0.86164 1.00000 0.01792 0.01772 0.01976 0.00061 -0.00075 -0.00277 0.01853 0.00322 0.00012 0.00033 0.00010 0.00000 0.00090 0.00092 0.00095 0.00073 0.00070 0.00074 0.00040 C4 0.16006 0.15095 0.81627 1.00000 0.02259 0.02267 0.02288 0.00114 -0.00118 0.00203 0.02280 0.00345 0.00013 0.00036 0.00010 0.00000 0.00100 0.00099 0.00101 0.00080 0.00076 0.00083 0.00043 H4 0.18791 0.00992 0.83309 1.00000 0.02736 0.00000 0.00000 C5 0.17002 0.22624 0.74650 1.00000 0.02923 0.03547 0.02182 -0.00152 0.00420 0.00328 0.02874 0.00384 0.00014 0.00041 0.00011 0.00000 0.00111 0.00122 0.00107 0.00089 0.00082 0.00094 0.00048 H5 0.20481 0.13718 0.71598 1.00000 0.03449 0.00000 0.00000 C6 0.12936 0.43033 0.72155 1.00000 0.02979 0.03601 0.02134 0.00721 0.00091 -0.00521 0.02906 0.00381 0.00014 0.00041 0.00011 0.00000 0.00115 0.00123 0.00106 0.00089 0.00084 0.00097 0.00049 H6 0.13628 0.48187 0.67391 1.00000 0.03488 0.00000 0.00000 C7 0.07831 0.56038 0.76614 1.00000 0.02633 0.02338 0.02742 0.00730 -0.00381 -0.00149 0.02589 0.00364 0.00013 0.00038 0.00011 0.00000 0.00107 0.00103 0.00111 0.00083 0.00083 0.00085 0.00046 H7 0.05004 0.70023 0.74887 1.00000 0.03107 0.00000 0.00000 C8 0.06861 0.48603 0.83590 1.00000 0.02369 0.01856 0.02490 0.00018 0.00109 0.00041 0.02239 0.00345 0.00013 0.00035 0.00011 0.00000 0.00100 0.00096 0.00106 0.00078 0.00078 0.00080 0.00043 H8 0.03384 0.57565 0.86628 1.00000 0.02687 0.00000 0.00000 C9 0.25051 0.32072 0.97750 1.00000 0.02132 0.01924 0.01623 -0.00111 -0.00077 -0.00112 0.01899 0.00323 0.00012 0.00034 0.00010 0.00000 0.00094 0.00092 0.00090 0.00073 0.00070 0.00078 0.00040 C10 0.29621 0.11560 0.99648 1.00000 0.02750 0.02164 0.02139 0.00192 0.00027 0.00250 0.02355 0.00355 0.00013 0.00036 0.00010 0.00000 0.00106 0.00098 0.00101 0.00080 0.00079 0.00084 0.00044 H10 0.26828 -0.01016 1.01992 1.00000 0.02826 0.00000 0.00000 C11 0.38258 0.09414 0.98126 1.00000 0.02703 0.02818 0.03016 0.00332 -0.00274 0.00666 0.02861 0.00385 0.00014 0.00039 0.00011 0.00000 0.00111 0.00110 0.00114 0.00090 0.00086 0.00092 0.00048 H11 0.41359 -0.04547 0.99498 1.00000 0.03433 0.00000 0.00000 C12 0.42369 0.27449 0.94631 1.00000 0.02016 0.03507 0.02923 -0.00236 -0.00125 -0.00054 0.02824 0.00364 0.00013 0.00040 0.00011 0.00000 0.00099 0.00120 0.00115 0.00092 0.00082 0.00089 0.00048 H12 0.48273 0.25895 0.93600 1.00000 0.03389 0.00000 0.00000 C13 0.37847 0.47744 0.92647 1.00000 0.02365 0.02924 0.03081 0.00437 0.00128 -0.00538 0.02791 0.00371 0.00013 0.00039 0.00011 0.00000 0.00105 0.00111 0.00117 0.00090 0.00086 0.00089 0.00048 H13 0.40640 0.60153 0.90228 1.00000 0.03349 0.00000 0.00000 C14 0.29213 0.50042 0.94185 1.00000 0.02431 0.01982 0.02719 0.00329 -0.00091 -0.00027 0.02385 0.00353 0.00013 0.00036 0.00011 0.00000 0.00103 0.00096 0.00109 0.00081 0.00081 0.00082 0.00044 H14 0.26133 0.64010 0.92787 1.00000 0.02862 0.00000 0.00000 C15 0.14205 0.25073 1.06660 1.00000 0.02435 0.02138 0.02377 -0.00216 0.00176 0.00166 0.02315 0.00353 0.00013 0.00036 0.00011 0.00000 0.00101 0.00098 0.00106 0.00080 0.00077 0.00081 0.00043 C16 0.13551 0.19123 1.12766 1.00000 0.02153 0.02249 0.02349 -0.00210 0.00098 0.00239 0.02251 0.00345 0.00012 0.00035 0.00010 0.00000 0.00098 0.00099 0.00106 0.00081 0.00076 0.00082 0.00043 C17 0.13250 0.13836 1.20268 1.00000 0.01853 0.02169 0.01933 -0.00065 0.00095 0.00343 0.01985 0.00336 0.00012 0.00034 0.00010 0.00000 0.00093 0.00096 0.00096 0.00077 0.00071 0.00078 0.00041 C18 0.16952 0.29904 1.25220 1.00000 0.02802 0.02322 0.02627 -0.00305 0.00205 -0.00231 0.02581 0.00358 0.00013 0.00038 0.00011 0.00000 0.00108 0.00105 0.00108 0.00083 0.00081 0.00086 0.00046 H18 0.19519 0.44110 1.23610 1.00000 0.03098 0.00000 0.00000 C19 0.16886 0.25160 1.32463 1.00000 0.03854 0.03557 0.02301 -0.00730 -0.00102 -0.00023 0.03247 0.00397 0.00015 0.00042 0.00011 0.00000 0.00126 0.00122 0.00111 0.00092 0.00091 0.00103 0.00052 H19 0.19437 0.36123 1.35800 1.00000 0.03896 0.00000 0.00000 C20 0.13139 0.04604 1.34889 1.00000 0.03309 0.04322 0.01989 0.00583 0.00470 0.00912 0.03195 0.00426 0.00015 0.00044 0.00011 0.00000 0.00120 0.00134 0.00106 0.00093 0.00087 0.00103 0.00052 H20 0.13107 0.01458 1.39868 1.00000 0.03834 0.00000 0.00000 C21 0.09424 -0.11410 1.30002 1.00000 0.03067 0.03200 0.03629 0.00954 0.00730 0.00182 0.03279 0.00427 0.00015 0.00042 0.00012 0.00000 0.00118 0.00118 0.00126 0.00100 0.00093 0.00098 0.00052 H21 0.06802 -0.25487 1.31649 1.00000 0.03935 0.00000 0.00000 C22 0.09522 -0.06950 1.22736 1.00000 0.02640 0.02719 0.02827 -0.00109 -0.00115 -0.00248 0.02738 0.00377 0.00014 0.00039 0.00011 0.00000 0.00109 0.00110 0.00112 0.00088 0.00084 0.00090 0.00047 H22 0.07041 -0.18090 1.19420 1.00000 0.03286 0.00000 0.00000 O1 0.01206 0.21027 0.95680 1.00000 0.02102 0.02033 0.02994 0.00021 0.00672 -0.00480 0.02357 0.00244 0.00008 0.00025 0.00007 0.00000 0.00070 0.00071 0.00078 0.00059 0.00056 0.00057 0.00033 H1A -0.01341 0.08218 0.94653 1.00000 0.03536 0.00000 0.00000 O2 0.13257 0.58647 0.98961 1.00000 0.02480 0.01511 0.03184 -0.00122 0.00493 0.00181 0.02380 0.00248 0.00009 0.00023 0.00008 0.00000 0.00074 0.00066 0.00080 0.00057 0.00059 0.00057 0.00033 H2 0.08295 0.60539 1.00458 1.00000 0.03569 0.00000 0.00000 Final Structure Factor Calculation for 2007src0348 in P2(1)/n Total number of l.s. parameters = 219 Maximum vector length = 511 Memory required = 2411 / 21973 wR2 = 0.1548 before cycle 5 for 3754 data and 0 / 219 parameters GooF = S = 1.124; Restrained GooF = 1.124 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0571 * P )^2 + 1.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0598 for 2758 Fo > 4sig(Fo) and 0.0879 for all 3754 data wR2 = 0.1548, GooF = S = 1.124, Restrained GooF = 1.124 for all data Occupancy sum of asymmetric unit = 24.00 for non-hydrogen and 18.00 for hydrogen atoms Principal mean square atomic displacements U 0.0242 0.0173 0.0147 C1 0.0235 0.0213 0.0138 C2 0.0221 0.0186 0.0150 C3 0.0255 0.0239 0.0191 C4 0.0369 0.0291 0.0202 C5 0.0414 0.0278 0.0180 C6 0.0361 0.0241 0.0174 C7 0.0249 0.0237 0.0185 C8 0.0222 0.0195 0.0153 C9 0.0285 0.0232 0.0190 C10 0.0345 0.0326 0.0187 C11 0.0359 0.0293 0.0195 C12 0.0359 0.0281 0.0198 C13 0.0296 0.0235 0.0185 C14 0.0254 0.0246 0.0194 C15 0.0260 0.0224 0.0191 C16 0.0240 0.0193 0.0163 C17 0.0299 0.0266 0.0210 C18 0.0400 0.0379 0.0195 C19 0.0498 0.0277 0.0183 C20 0.0456 0.0294 0.0234 C21 0.0304 0.0287 0.0231 C22 0.0325 0.0237 0.0146 O1 0.0331 0.0238 0.0145 O2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.019 0.028 0.038 0.049 0.063 0.082 0.108 0.157 1.000 Number in group 377. 397. 367. 367. 378. 381. 382. 356. 382. 367. GooF 1.223 1.054 1.156 1.160 1.139 1.072 1.002 1.063 0.890 1.413 K 4.361 1.708 1.000 0.991 0.996 0.975 0.994 1.010 1.018 0.987 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.14 1.32 1.66 inf Number in group 396. 358. 385. 368. 370. 374. 377. 377. 373. 376. GooF 1.000 1.057 0.953 1.031 1.093 1.158 1.269 1.285 1.067 1.267 K 0.921 1.015 0.988 1.064 1.006 1.006 1.044 1.059 1.031 0.959 R1 0.226 0.174 0.180 0.131 0.101 0.079 0.063 0.056 0.046 0.044 Recommended weighting scheme: WGHT 0.0557 1.1766 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) -10 3 3 2312.43 1255.95 6.76 0.244 1.18 -11 1 2 182.53 22.92 6.48 0.033 1.36 -12 2 1 1170.35 705.23 6.45 0.183 1.17 -12 3 2 95.15 12.99 6.30 0.025 1.06 -13 2 2 167.00 13.12 6.26 0.025 1.10 -11 4 3 158.79 60.20 5.84 0.053 0.99 12 2 1 1411.38 835.33 5.81 0.199 1.17 10 3 1 196.14 1.11 5.78 0.007 1.19 -11 2 3 989.66 532.63 5.74 0.159 1.25 -1 1 18 76.90 1.54 5.67 0.009 1.02 0 1 17 31.97 0.67 5.59 0.006 1.08 0 2 19 61.99 6.95 5.32 0.018 0.93 2 2 16 130.44 14.53 5.12 0.026 1.06 12 1 0 46.41 0.50 5.11 0.005 1.26 -12 1 3 195.70 17.57 5.06 0.029 1.25 -11 4 1 47.37 1.70 5.00 0.009 1.00 13 1 0 82.08 28.27 4.77 0.037 1.17 0 2 0 1557.16 1106.46 4.52 0.229 2.82 -14 3 3 398.94 220.55 4.47 0.102 0.95 -12 4 4 71.17 0.00 4.47 0.000 0.94 -13 4 3 81.49 21.57 4.17 0.032 0.91 12 2 16 122.64 41.23 4.00 0.044 0.81 1 3 1 742.32 536.27 3.96 0.160 1.85 16 4 4 56.44 144.06 3.89 0.083 0.78 0 4 0 420.85 285.55 3.81 0.116 1.41 -1 3 16 205.12 125.54 3.76 0.077 0.99 0 3 1 1130.57 851.68 3.74 0.201 1.87 -1 4 18 65.43 5.79 3.71 0.017 0.84 13 0 13 861.40 3.30 3.67 0.013 0.89 -1 1 15 950.47 685.18 3.43 0.180 1.22 1 4 15 126.54 59.49 3.41 0.053 0.93 1 2 16 1085.27 837.39 3.35 0.199 1.07 -1 5 2 2270.57 1761.14 3.34 0.289 1.12 0 5 16 38.35 1.19 3.26 0.008 0.81 -13 3 1 105.33 52.55 3.25 0.050 1.01 0 1 19 52.04 25.13 3.21 0.035 0.97 18 0 0 8.96 46.38 3.18 0.047 0.86 11 1 13 362.79 218.75 3.15 0.102 0.97 10 1 15 217.90 140.55 3.14 0.082 0.93 -1 1 16 67.37 34.13 3.12 0.040 1.15 0 3 16 77.96 39.47 3.12 0.043 0.99 -12 3 1 360.33 264.53 3.11 0.112 1.06 -10 3 4 95.11 1.80 3.10 0.009 1.17 -9 6 8 -0.86 30.45 3.09 0.038 0.78 1 1 16 25.84 4.19 3.09 0.014 1.14 1 4 2 527.31 401.78 3.09 0.138 1.39 11 1 0 113.02 69.56 3.06 0.057 1.37 12 3 0 536.99 406.21 3.00 0.139 1.06 2 2 15 92.76 46.40 2.96 0.047 1.12 -13 2 1 814.65 642.03 2.94 0.175 1.10 Bond lengths and angles C1 - Distance Angles O1 1.4419 (0.0022) C3 1.5113 (0.0026) 110.86 (0.15) C2 1.5586 (0.0027) 106.79 (0.15) 113.22 (0.15) C1 - O1 C3 C2 - Distance Angles O2 1.4254 (0.0022) C15 1.4806 (0.0027) 109.82 (0.15) C9 1.5278 (0.0026) 107.61 (0.15) 109.97 (0.16) C1 1.5586 (0.0027) 110.50 (0.15) 110.17 (0.16) 108.74 (0.15) C2 - O2 C15 C9 C3 - Distance Angles C4 1.3907 (0.0027) C8 1.3961 (0.0027) 118.98 (0.18) C1 1.5113 (0.0026) 119.39 (0.17) 121.63 (0.17) C3 - C4 C8 C4 - Distance Angles C3 1.3907 (0.0027) C5 1.3907 (0.0028) 120.59 (0.19) C4 - C3 C5 - Distance Angles C6 1.3807 (0.0032) C4 1.3907 (0.0028) 120.04 (0.19) C5 - C6 C6 - Distance Angles C5 1.3807 (0.0031) C7 1.3900 (0.0031) 119.98 (0.19) C6 - C5 C7 - Distance Angles C8 1.3882 (0.0028) C6 1.3900 (0.0031) 120.05 (0.19) C7 - C8 C8 - Distance Angles C7 1.3882 (0.0028) C3 1.3961 (0.0027) 120.36 (0.18) C8 - C7 C9 - Distance Angles C14 1.3903 (0.0027) C10 1.3918 (0.0027) 118.93 (0.18) C2 1.5278 (0.0026) 121.25 (0.17) 119.79 (0.17) C9 - C14 C10 C10 - Distance Angles C11 1.3899 (0.0029) C9 1.3918 (0.0027) 120.22 (0.19) C10 - C11 C11 - Distance Angles C12 1.3826 (0.0031) C10 1.3899 (0.0029) 120.48 (0.19) C11 - C12 C12 - Distance Angles C13 1.3818 (0.0031) C11 1.3826 (0.0031) 119.65 (0.19) C12 - C13 C13 - Distance Angles C12 1.3818 (0.0031) C14 1.3910 (0.0029) 120.13 (0.20) C13 - C12 C14 - Distance Angles C9 1.3903 (0.0027) C13 1.3910 (0.0029) 120.57 (0.19) C14 - C9 C15 - Distance Angles C16 1.2016 (0.0028) C2 1.4806 (0.0027) 174.79 (0.21) C15 - C16 C16 - Distance Angles C15 1.2016 (0.0028) C17 1.4399 (0.0027) 174.77 (0.22) C16 - C15 C17 - Distance Angles C22 1.3954 (0.0029) C18 1.3976 (0.0028) 119.09 (0.18) C16 1.4399 (0.0027) 122.18 (0.18) 118.73 (0.18) C17 - C22 C18 C18 - Distance Angles C19 1.3838 (0.0029) C17 1.3976 (0.0028) 120.13 (0.20) C18 - C19 C19 - Distance Angles C20 1.3831 (0.0034) C18 1.3838 (0.0029) 120.59 (0.20) C19 - C20 C20 - Distance Angles C19 1.3831 (0.0034) C21 1.3885 (0.0034) 119.61 (0.20) C20 - C19 C21 - Distance Angles C22 1.3853 (0.0030) C20 1.3885 (0.0034) 120.30 (0.21) C21 - C22 C22 - Distance Angles C21 1.3853 (0.0030) C17 1.3954 (0.0029) 120.28 (0.20) C22 - C21 O1 - Distance Angles C1 1.4419 (0.0022) O1 - O2 - Distance Angles C2 1.4254 (0.0022) O2 - FMAP and GRID set by program FMAP 2 2 10 GRID -3.571 -2 -2 3.571 2 2 R1 = 0.0879 for 3754 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.24 at 0.6099 0.2563 0.3986 [ 0.72 A from C3 ] Deepest hole -0.34 at 0.9871 0.0588 0.9478 [ 0.13 A from H1A ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 3054 / 23873 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1099 0.2437 0.8986 1.00000 0.05 0.24 0.72 C3 0.80 C1 1.46 H1 1.84 C4 Q2 1 0.0489 0.1658 1.1382 1.00000 0.05 0.24 1.38 C16 1.73 C17 1.94 H8 2.08 C15 Q3 1 0.3797 0.1136 0.9223 1.00000 0.05 0.23 1.11 C11 1.21 C12 1.69 H11 1.80 H12 Q4 1 0.1636 0.3050 1.1024 1.00000 0.05 0.22 0.80 C15 0.92 C16 2.04 C2 2.18 C17 Q5 1 -0.0430 -0.1786 0.9230 1.00000 0.05 0.21 1.59 H1A 1.61 C15 1.68 C16 2.14 H8 Q6 1 0.1341 0.5567 1.0660 1.00000 0.05 0.21 1.39 H2 1.44 O2 1.73 C15 1.86 C2 Q7 1 0.0102 0.1596 1.0055 1.00000 0.05 0.20 0.96 O1 1.23 H1A 1.63 H1A 1.96 C1 Q8 1 0.1201 -0.0062 0.9622 1.00000 0.05 0.20 0.44 H1 1.26 C1 2.07 O1 2.11 C2 Q9 1 0.1639 0.6205 0.6946 1.00000 0.05 0.20 0.96 H6 1.31 C6 1.97 C7 2.13 H7 Q10 1 0.1794 0.7570 1.0216 1.00000 0.05 0.19 1.33 O2 1.74 H2 1.90 H10 2.30 H1 Q11 1 0.3859 0.4917 0.9937 1.00000 0.05 0.19 1.26 C13 1.64 C12 1.71 C14 1.86 H13 Q12 1 0.1618 0.3135 1.4363 1.00000 0.05 0.19 1.60 H19 1.66 H10 1.88 H20 1.95 H11 Q13 1 0.1646 0.7225 0.9554 1.00000 0.05 0.18 1.13 O2 1.68 H14 1.74 H2 1.86 H1 Q14 1 0.1578 0.5078 0.8421 1.00000 0.05 0.18 1.39 C8 1.54 C3 1.86 C7 2.03 H8 Q15 1 0.0816 0.7826 0.9461 1.00000 0.05 0.18 1.48 H2 1.49 H1 1.56 O2 2.01 H8 Q16 1 0.5000 0.5000 1.0000 0.50000 0.05 0.18 1.82 H12 1.97 C12 2.28 C13 2.35 H13 Q17 1 0.1191 0.2278 0.9825 1.00000 0.05 0.18 0.87 C2 0.90 C1 1.39 H1 1.60 C15 Q18 1 0.5196 0.2093 0.9611 1.00000 0.05 0.18 0.77 H12 1.54 C12 1.58 H11 2.27 C11 Q19 1 0.1028 0.1890 1.0036 1.00000 0.05 0.17 1.20 C2 1.24 C1 1.34 C15 1.53 H1 Q20 1 0.1027 0.7115 0.8643 1.00000 0.05 0.17 1.32 H8 1.46 C8 2.04 C7 2.24 H4 Shortest distances between peaks (including symmetry equivalents) 17 19 0.53 2 5 1.15 10 13 1.27 13 15 1.33 8 15 1.36 8 17 1.37 8 19 1.38 5 7 1.41 7 19 1.45 14 20 1.50 1 17 1.57 6 10 1.59 4 6 1.63 15 20 1.63 8 13 1.68 5 19 1.70 7 15 1.76 11 16 1.77 7 17 1.81 16 18 1.82 7 7 1.83 1 8 1.84 13 20 1.91 8 10 1.94 5 15 1.97 1 14 1.99 1 19 2.00 10 15 2.02 4 5 2.04 2 4 2.09 4 19 2.14 7 8 2.14 5 17 2.20 3 9 2.26 12 18 2.28 7 8 2.31 3 18 2.32 6 13 2.34 4 17 2.36 11 18 2.36 11 12 2.38 6 19 2.41 6 17 2.43 8 20 2.43 13 14 2.44 2 20 2.45 3 11 2.51 2 15 2.52 2 7 2.53 15 19 2.54 5 7 2.56 10 12 2.57 5 6 2.57 7 19 2.63 1 7 2.64 5 20 2.64 15 17 2.65 7 15 2.67 6 15 2.67 2 19 2.70 11 18 2.71 1 20 2.71 10 19 2.72 5 8 2.72 5 8 2.77 1 15 2.79 14 15 2.80 9 14 2.84 18 18 2.85 10 17 2.89 7 13 2.92 13 17 2.93 2 6 2.94 13 19 2.95 4 10 2.98 7 17 2.98 7 10 2.99 Time profile in seconds ----------------------- 0.10: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.02: 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. 2.69: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.03: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.30: Structure factors and derivatives 1.91: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.33: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.01: Merge reflections for Fourier and .fcf 0.11: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0348 finished at 17:17:10 Total CPU time: 6.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++