+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0667a started at 16:01:28 on 13-Jul-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0667a in P2(1)2(1)2(1) CELL 0.71073 8.3288 9.0098 25.4028 90.000 90.000 90.000 ZERR 4.00 0.0002 0.0003 0.0008 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 O UNIT 64 88 44 V = 1906.25 F(000) = 824.0 Mu = 0.12 mm-1 Cell Wt = 1561.34 Rho = 1.360 MERG 4 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 5 SIZE 0.03 0.12 0.17 ACTA BOND $H WGHT 0.00740 1.39930 L.S. 10 TEMP -153.00 FVAR 0.52600 MOLE 1 C1 1 0.228364 0.617102 0.931767 11.00000 0.02306 0.02400 = 0.01741 -0.00218 0.00231 -0.00062 AFIX 13 H1 2 0.172654 0.715259 0.933763 11.00000 -1.20000 AFIX 0 C2 1 0.103172 0.495983 0.927432 11.00000 0.02175 0.02315 = 0.01715 -0.00143 0.00183 -0.00142 AFIX 13 H2 2 0.032573 0.496026 0.959273 11.00000 -1.20000 AFIX 0 C3 1 0.003386 0.522474 0.877952 11.00000 0.02228 0.02073 = 0.01817 -0.00161 0.00115 -0.00223 AFIX 13 H3 2 -0.054730 0.619114 0.881379 11.00000 -1.20000 AFIX 0 C4 1 0.111843 0.528359 0.830198 11.00000 0.02090 0.02351 = 0.01520 0.00030 -0.00107 0.00125 AFIX 13 H4 2 0.162681 0.429681 0.823348 11.00000 -1.20000 AFIX 0 C5 1 0.238640 0.647375 0.840442 11.00000 0.02604 0.02331 = 0.01858 0.00119 0.00239 -0.00133 AFIX 13 H5 2 0.187556 0.747502 0.843263 11.00000 -1.20000 AFIX 0 C6 1 0.337515 0.600949 0.979404 11.00000 0.02243 0.03309 = 0.02042 -0.00162 0.00151 -0.00187 AFIX 23 H6A 2 0.395731 0.505175 0.978608 11.00000 -1.20000 H6B 2 0.416418 0.682990 0.981098 11.00000 -1.20000 AFIX 0 C7 1 0.292392 0.624372 1.071604 11.00000 0.02869 0.01853 = 0.02069 0.00128 -0.00374 -0.00050 C8 1 0.165902 0.635791 1.112984 11.00000 0.03151 0.03547 = 0.02072 0.00057 0.00025 0.00335 AFIX 137 H8A 2 0.214706 0.622057 1.147748 11.00000 -1.50000 H8B 2 0.084553 0.558931 1.107170 11.00000 -1.50000 H8C 2 0.115351 0.733885 1.111217 11.00000 -1.50000 AFIX 0 C9 1 0.124039 0.236182 0.948476 11.00000 0.02753 0.02373 = 0.02141 0.00285 -0.00407 -0.00397 C10 1 0.231671 0.104387 0.942372 11.00000 0.02856 0.02295 = 0.02824 0.00014 -0.00319 -0.00357 AFIX 137 H10A 2 0.329261 0.119120 0.963281 11.00000 -1.50000 H10B 2 0.260543 0.092544 0.905209 11.00000 -1.50000 H10C 2 0.175722 0.015155 0.954626 11.00000 -1.50000 AFIX 0 C11 1 -0.246567 0.416045 0.901261 11.00000 0.02293 0.03603 = 0.02250 0.00235 -0.00061 -0.00264 C12 1 -0.352602 0.284094 0.895519 11.00000 0.04098 0.04912 = 0.03732 -0.00424 0.00667 -0.02107 AFIX 137 H12A 2 -0.336552 0.217312 0.925512 11.00000 -1.50000 H12B 2 -0.326119 0.231836 0.862818 11.00000 -1.50000 H12C 2 -0.464963 0.316239 0.894446 11.00000 -1.50000 AFIX 0 C13 1 0.047489 0.508852 0.738717 11.00000 0.02706 0.02392 = 0.01788 -0.00103 0.00221 -0.00488 C14 1 -0.039227 0.585171 0.695201 11.00000 0.03527 0.03516 = 0.01893 0.00197 -0.00090 0.00201 AFIX 137 H14A 2 -0.019185 0.532797 0.662034 11.00000 -1.50000 H14B 2 -0.000895 0.687679 0.692286 11.00000 -1.50000 H14C 2 -0.154684 0.585275 0.702637 11.00000 -1.50000 AFIX 0 C15 1 0.413212 0.775703 0.782434 11.00000 0.02980 0.03467 = 0.02270 0.00365 -0.00167 -0.00983 C16 1 0.533240 0.751532 0.739726 11.00000 0.04705 0.05874 = 0.03164 -0.00279 0.01514 -0.02213 AFIX 137 H16A 2 0.540089 0.840740 0.717768 11.00000 -1.50000 H16B 2 0.499983 0.667032 0.718019 11.00000 -1.50000 H16C 2 0.638526 0.730938 0.755324 11.00000 -1.50000 AFIX 0 O1 3 0.329648 0.615684 0.886085 11.00000 0.02176 0.03161 = 0.01889 0.00065 0.00107 -0.00215 O2 3 0.226874 0.607048 1.023427 11.00000 0.02316 0.03828 = 0.01694 -0.00180 0.00080 -0.00295 O3 3 0.435314 0.630576 1.078679 11.00000 0.02502 0.03398 = 0.02302 -0.00269 -0.00377 0.00122 O4 3 0.186856 0.355062 0.922935 11.00000 0.02355 0.02095 = 0.02162 0.00154 0.00045 0.00050 O5 3 0.000856 0.240410 0.973102 11.00000 0.03444 0.03184 = 0.03943 0.00762 0.01545 -0.00177 O6 3 -0.112524 0.404403 0.870447 11.00000 0.02253 0.02506 = 0.02076 -0.00251 0.00172 -0.00521 O7 3 -0.270305 0.520167 0.929874 11.00000 0.02611 0.03542 = 0.03172 -0.00130 0.00714 0.00114 O8 3 0.018854 0.576798 0.785699 11.00000 0.02874 0.02665 = 0.01694 0.00167 -0.00044 0.00209 O9 3 0.131228 0.402041 0.734111 11.00000 0.05833 0.03676 = 0.02183 -0.00311 0.00024 0.01540 O10 3 0.347782 0.643321 0.797740 11.00000 0.03106 0.02825 = 0.02327 -0.00048 0.00911 -0.00682 O11 3 0.378261 0.891175 0.802641 11.00000 0.04286 0.03114 = 0.05120 0.00586 0.00686 -0.00675 HKLF 4 Covalent radii and connectivity table for 2009src0667a in P2(1)2(1)2(1) C 0.770 H 0.320 O 0.660 C1 - O1 C2 C6 C2 - O4 C1 C3 C3 - O6 C4 C2 C4 - O8 C3 C5 C5 - O1 O10 C4 C6 - O2 C1 C7 - O3 O2 C8 C8 - C7 C9 - O5 O4 C10 C10 - C9 C11 - O7 O6 C12 C12 - C11 C13 - O9 O8 C14 C14 - C13 C15 - O11 O10 C16 C16 - C15 O1 - C5 C1 O2 - C7 C6 O3 - C7 O4 - C9 C2 O5 - C9 O6 - C11 C3 O7 - C11 O8 - C13 C4 O9 - C13 O10 - C15 C5 O11 - C15 17319 Reflections read, of which 64 rejected -10 =< h =< 10, -11 =< k =< 11, -32 =< l =< 31, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 2507 Unique reflections, of which 0 suppressed R(int) = 0.0519 R(sigma) = 0.0345 Friedel opposites merged Maximum memory for data reduction = 2450 / 24304 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 = 3155 / 308074 wR2 = 0.0903 before cycle 1 for 2507 data and 249 / 249 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0074 * P )^2 + 1.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52597 0.00085 -0.040 OSF Mean shift/su = 0.025 Maximum = 0.114 for x O1 Max. shift = 0.002 A for H12B Max. dU = 0.000 for C16 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3155 / 308074 wR2 = 0.0903 before cycle 2 for 2507 data and 249 / 249 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0074 * P )^2 + 1.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52594 0.00085 -0.026 OSF Mean shift/su = 0.010 Maximum = 0.046 for tors H14A Max. shift = 0.001 A for H14B Max. dU = 0.000 for C16 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3155 / 308074 wR2 = 0.0903 before cycle 3 for 2507 data and 249 / 249 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0074 * P )^2 + 1.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52594 0.00085 0.000 OSF Mean shift/su = 0.001 Maximum = 0.028 for tors H14A Max. shift = 0.001 A for H14B Max. dU = 0.000 for C16 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3155 / 308074 wR2 = 0.0903 before cycle 4 for 2507 data and 249 / 249 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0074 * P )^2 + 1.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52595 0.00085 0.001 OSF Mean shift/su = 0.001 Maximum = 0.016 for tors H14A Max. shift = 0.000 A for H14B Max. dU = 0.000 for C16 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3155 / 308074 wR2 = 0.0903 before cycle 5 for 2507 data and 249 / 249 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0074 * P )^2 + 1.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52595 0.00085 0.000 OSF Mean shift/su = 0.000 Maximum = 0.009 for tors H14A Max. shift = 0.000 A for H14B Max. dU = 0.000 for C14 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3155 / 308074 wR2 = 0.0903 before cycle 6 for 2507 data and 249 / 249 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0074 * P )^2 + 1.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52595 0.00085 0.000 OSF Mean shift/su = 0.000 Maximum = 0.005 for tors H14A Max. shift = 0.000 A for H14A Max. dU = 0.000 for C16 Least-squares cycle 7 Maximum vector length = 511 Memory required = 3155 / 308074 wR2 = 0.0903 before cycle 7 for 2507 data and 249 / 249 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0074 * P )^2 + 1.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52595 0.00085 0.000 OSF Mean shift/su = 0.000 Maximum = 0.003 for tors H14A Max. shift = 0.000 A for H14B Max. dU = 0.000 for C14 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3155 / 308074 wR2 = 0.0903 before cycle 8 for 2507 data and 249 / 249 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0074 * P )^2 + 1.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52595 0.00085 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for tors H14A Max. shift = 0.000 A for H14B Max. dU = 0.000 for C14 Least-squares cycle 9 Maximum vector length = 511 Memory required = 3155 / 308074 wR2 = 0.0903 before cycle 9 for 2507 data and 249 / 249 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0074 * P )^2 + 1.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52595 0.00085 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for z O3 Max. shift = 0.000 A for H14A Max. dU = 0.000 for C16 Least-squares cycle 10 Maximum vector length = 511 Memory required = 3155 / 308074 wR2 = 0.0903 before cycle 10 for 2507 data and 249 / 249 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0074 * P )^2 + 1.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52595 0.00085 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for z O2 Max. shift = 0.000 A for H14B Max. dU = 0.000 for C5 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.1726 0.7153 0.9338 13 1.000 0.000 C1 O1 C2 C6 H2 0.0326 0.4960 0.9593 13 1.000 0.000 C2 O4 C1 C3 H3 -0.0547 0.6191 0.8814 13 1.000 0.000 C3 O6 C4 C2 H4 0.1627 0.4297 0.8234 13 1.000 0.000 C4 O8 C3 C5 H5 0.1875 0.7475 0.8433 13 1.000 0.000 C5 O1 O10 C4 H6A 0.3957 0.5052 0.9786 23 0.990 0.000 C6 O2 C1 H6B 0.4164 0.6830 0.9811 23 0.990 0.000 C6 O2 C1 H8A 0.2147 0.6223 1.1478 137 0.980 0.000 C8 C7 H8A H8B 0.0846 0.5588 1.1072 137 0.980 0.000 C8 C7 H8A H8C 0.1152 0.7338 1.1112 137 0.980 0.000 C8 C7 H8A H10A 0.3293 0.1192 0.9632 137 0.980 0.000 C10 C9 H10A H10B 0.2604 0.0925 0.9052 137 0.980 0.000 C10 C9 H10A H10C 0.1758 0.0152 0.9547 137 0.980 0.000 C10 C9 H10A H12A -0.3368 0.2175 0.9256 137 0.980 0.000 C12 C11 H12A H12B -0.3259 0.2316 0.8629 137 0.980 0.000 C12 C11 H12A H12C -0.4650 0.3162 0.8943 137 0.980 0.000 C12 C11 H12A H14A -0.0195 0.5326 0.6620 137 0.980 0.000 C14 C13 H14A H14B -0.0006 0.6876 0.6922 137 0.980 0.000 C14 C13 H14A H14C -0.1546 0.5856 0.7027 137 0.980 0.000 C14 C13 H14A H16A 0.5401 0.8407 0.7178 137 0.980 0.000 C16 C15 H16A H16B 0.5000 0.6671 0.7180 137 0.980 0.000 C16 C15 H16A H16C 0.6385 0.7309 0.7553 137 0.980 0.000 C16 C15 H16A 2009src0667a in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.22835 0.61711 0.93177 1.00000 0.02304 0.02406 0.01733 -0.00215 0.00222 -0.00055 0.02148 0.00469 0.00034 0.00031 0.00010 0.00000 0.00133 0.00142 0.00120 0.00109 0.00108 0.00120 0.00056 H1 0.17264 0.71527 0.93376 1.00000 0.02577 0.00000 0.00000 C2 0.10318 0.49601 0.92744 1.00000 0.02175 0.02306 0.01712 -0.00140 0.00185 -0.00143 0.02064 0.00466 0.00033 0.00030 0.00010 0.00000 0.00131 0.00135 0.00121 0.00108 0.00110 0.00117 0.00055 H2 0.03259 0.49604 0.95928 1.00000 0.02477 0.00000 0.00000 C3 0.00337 0.52249 0.87796 1.00000 0.02225 0.02068 0.01812 -0.00162 0.00117 -0.00225 0.02035 0.00450 0.00032 0.00031 0.00010 0.00000 0.00134 0.00126 0.00122 0.00107 0.00108 0.00118 0.00055 H3 -0.05475 0.61913 0.88138 1.00000 0.02442 0.00000 0.00000 C4 0.11184 0.52836 0.83021 1.00000 0.02086 0.02349 0.01517 0.00032 -0.00099 0.00123 0.01984 0.00458 0.00032 0.00031 0.00010 0.00000 0.00128 0.00135 0.00117 0.00102 0.00108 0.00119 0.00055 H4 0.16269 0.42969 0.82336 1.00000 0.02381 0.00000 0.00000 C5 0.23862 0.64739 0.84044 1.00000 0.02603 0.02329 0.01855 0.00116 0.00233 -0.00132 0.02262 0.00475 0.00033 0.00033 0.00010 0.00000 0.00137 0.00138 0.00126 0.00109 0.00114 0.00123 0.00057 H5 0.18754 0.74752 0.84325 1.00000 0.02715 0.00000 0.00000 C6 0.33752 0.60096 0.97941 1.00000 0.02250 0.03309 0.02033 -0.00161 0.00149 -0.00189 0.02531 0.00494 0.00034 0.00036 0.00010 0.00000 0.00133 0.00158 0.00128 0.00126 0.00112 0.00133 0.00060 H6A 0.39574 0.50519 0.97862 1.00000 0.03037 0.00000 0.00000 H6B 0.41641 0.68301 0.98111 1.00000 0.03037 0.00000 0.00000 C7 0.29241 0.62436 1.07160 1.00000 0.02869 0.01853 0.02073 0.00127 -0.00369 -0.00051 0.02265 0.00471 0.00034 0.00030 0.00011 0.00000 0.00149 0.00137 0.00130 0.00111 0.00116 0.00120 0.00058 C8 0.16589 0.63581 1.11299 1.00000 0.03152 0.03550 0.02066 0.00061 0.00030 0.00332 0.02923 0.00538 0.00036 0.00036 0.00011 0.00000 0.00154 0.00166 0.00133 0.00128 0.00126 0.00144 0.00066 H8A 0.21472 0.62227 1.14776 1.00000 0.04384 0.00000 0.00000 H8B 0.08463 0.55884 1.10722 1.00000 0.04384 0.00000 0.00000 H8C 0.11521 0.73384 1.11118 1.00000 0.04384 0.00000 0.00000 C9 0.12403 0.23618 0.94848 1.00000 0.02758 0.02368 0.02148 0.00284 -0.00420 -0.00404 0.02424 0.00478 0.00036 0.00032 0.00010 0.00000 0.00147 0.00142 0.00133 0.00114 0.00119 0.00132 0.00060 C10 0.23168 0.10438 0.94237 1.00000 0.02855 0.02290 0.02823 0.00012 -0.00325 -0.00354 0.02656 0.00496 0.00036 0.00032 0.00011 0.00000 0.00149 0.00143 0.00147 0.00119 0.00124 0.00131 0.00063 H10A 0.32934 0.11918 0.96323 1.00000 0.03984 0.00000 0.00000 H10B 0.26042 0.09248 0.90520 1.00000 0.03984 0.00000 0.00000 H10C 0.17580 0.01516 0.95466 1.00000 0.03984 0.00000 0.00000 C11 -0.24658 0.41610 0.90126 1.00000 0.02289 0.03602 0.02252 0.00236 -0.00067 -0.00267 0.02714 0.00523 0.00035 0.00037 0.00011 0.00000 0.00141 0.00165 0.00137 0.00128 0.00117 0.00136 0.00063 C12 -0.35260 0.28407 0.89553 1.00000 0.04096 0.04909 0.03730 -0.00417 0.00654 -0.02110 0.04245 0.00576 0.00043 0.00041 0.00014 0.00000 0.00194 0.00211 0.00182 0.00161 0.00163 0.00182 0.00087 H12A -0.33677 0.21745 0.92558 1.00000 0.06367 0.00000 0.00000 H12B -0.32588 0.23163 0.86288 1.00000 0.06367 0.00000 0.00000 H12C -0.46496 0.31620 0.89434 1.00000 0.06367 0.00000 0.00000 C13 0.04752 0.50884 0.73872 1.00000 0.02708 0.02391 0.01786 -0.00098 0.00226 -0.00499 0.02295 0.00480 0.00034 0.00032 0.00010 0.00000 0.00144 0.00144 0.00125 0.00113 0.00110 0.00128 0.00059 C14 -0.03923 0.58517 0.69519 1.00000 0.03525 0.03518 0.01890 0.00197 -0.00089 0.00205 0.02978 0.00541 0.00038 0.00037 0.00011 0.00000 0.00162 0.00164 0.00130 0.00127 0.00126 0.00148 0.00066 H14A -0.01951 0.53258 0.66205 1.00000 0.04467 0.00000 0.00000 H14B -0.00062 0.68757 0.69219 1.00000 0.04467 0.00000 0.00000 H14C -0.15464 0.58559 0.70270 1.00000 0.04467 0.00000 0.00000 C15 0.41316 0.77575 0.78243 1.00000 0.02982 0.03471 0.02274 0.00368 -0.00168 -0.00987 0.02909 0.00518 0.00037 0.00036 0.00011 0.00000 0.00162 0.00175 0.00141 0.00129 0.00125 0.00143 0.00068 C16 0.53323 0.75154 0.73972 1.00000 0.04721 0.05894 0.03148 -0.00281 0.01511 -0.02228 0.04588 0.00627 0.00044 0.00044 0.00013 0.00000 0.00212 0.00238 0.00175 0.00174 0.00158 0.00203 0.00094 H16A 0.54012 0.84075 0.71777 1.00000 0.06882 0.00000 0.00000 H16B 0.49996 0.66705 0.71801 1.00000 0.06882 0.00000 0.00000 H16C 0.63850 0.73091 0.75533 1.00000 0.06882 0.00000 0.00000 O1 0.32968 0.61570 0.88609 1.00000 0.02179 0.03158 0.01886 0.00067 0.00104 -0.00216 0.02408 0.00323 0.00022 0.00023 0.00007 0.00000 0.00093 0.00112 0.00090 0.00086 0.00078 0.00090 0.00044 O2 0.22686 0.60706 1.02342 1.00000 0.02315 0.03828 0.01689 -0.00179 0.00079 -0.00293 0.02611 0.00338 0.00023 0.00024 0.00007 0.00000 0.00095 0.00121 0.00087 0.00089 0.00079 0.00096 0.00045 O3 0.43533 0.63059 1.07868 1.00000 0.02498 0.03395 0.02298 -0.00267 -0.00379 0.00123 0.02730 0.00336 0.00023 0.00024 0.00008 0.00000 0.00103 0.00119 0.00098 0.00091 0.00081 0.00093 0.00047 O4 0.18688 0.35507 0.92293 1.00000 0.02354 0.02096 0.02163 0.00155 0.00046 0.00049 0.02205 0.00327 0.00022 0.00021 0.00007 0.00000 0.00096 0.00096 0.00093 0.00082 0.00080 0.00082 0.00042 O5 0.00087 0.24041 0.97311 1.00000 0.03434 0.03186 0.03937 0.00763 0.01549 -0.00174 0.03519 0.00400 0.00026 0.00025 0.00008 0.00000 0.00121 0.00119 0.00119 0.00103 0.00103 0.00108 0.00053 O6 -0.11253 0.40441 0.87045 1.00000 0.02252 0.02503 0.02077 -0.00247 0.00177 -0.00522 0.02277 0.00319 0.00023 0.00022 0.00007 0.00000 0.00094 0.00096 0.00089 0.00081 0.00078 0.00089 0.00041 O7 -0.27031 0.52017 0.92988 1.00000 0.02604 0.03540 0.03174 -0.00128 0.00716 0.00114 0.03106 0.00384 0.00024 0.00025 0.00008 0.00000 0.00106 0.00120 0.00111 0.00100 0.00095 0.00100 0.00049 O8 0.01884 0.57681 0.78570 1.00000 0.02871 0.02659 0.01690 0.00164 -0.00045 0.00212 0.02407 0.00335 0.00024 0.00022 0.00007 0.00000 0.00105 0.00103 0.00088 0.00081 0.00082 0.00093 0.00044 O9 0.13125 0.40204 0.73411 1.00000 0.05830 0.03673 0.02176 -0.00310 0.00027 0.01548 0.03893 0.00411 0.00031 0.00026 0.00008 0.00000 0.00149 0.00123 0.00099 0.00096 0.00108 0.00135 0.00056 O10 0.34776 0.64331 0.79774 1.00000 0.03105 0.02825 0.02327 -0.00052 0.00911 -0.00687 0.02752 0.00348 0.00025 0.00023 0.00007 0.00000 0.00109 0.00108 0.00097 0.00085 0.00089 0.00097 0.00047 O11 0.37822 0.89119 0.80264 1.00000 0.04283 0.03112 0.05128 0.00585 0.00694 -0.00669 0.04174 0.00424 0.00030 0.00026 0.00009 0.00000 0.00135 0.00126 0.00139 0.00115 0.00120 0.00121 0.00058 Final Structure Factor Calculation for 2009src0667a in P2(1)2(1)2(1) Total number of l.s. parameters = 249 Maximum vector length = 511 Memory required = 2908 / 24024 wR2 = 0.0903 before cycle 11 for 2507 data and 2 / 249 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0074 * P )^2 + 1.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0445 for 2245 Fo > 4sig(Fo) and 0.0532 for all 2507 data wR2 = 0.0903, GooF = S = 1.121, Restrained GooF = 1.121 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 27.00 for non-hydrogen and 22.00 for hydrogen atoms Principal mean square atomic displacements U 0.0254 0.0229 0.0161 C1 0.0246 0.0210 0.0164 C2 0.0244 0.0193 0.0173 C3 0.0240 0.0206 0.0150 C4 0.0270 0.0234 0.0175 C5 0.0337 0.0227 0.0195 C6 0.0302 0.0199 0.0178 C7 0.0374 0.0296 0.0206 C8 0.0325 0.0212 0.0191 C9 0.0324 0.0263 0.0209 C10 0.0370 0.0225 0.0220 C11 0.0683 0.0360 0.0231 C12 0.0312 0.0204 0.0173 C13 0.0373 0.0335 0.0186 C14 0.0432 0.0230 0.0211 C15 0.0790 0.0393 0.0193 C16 0.0320 0.0218 0.0184 O1 0.0390 0.0226 0.0167 O2 0.0350 0.0270 0.0199 O3 0.0240 0.0225 0.0197 O4 0.0536 0.0338 0.0182 O5 0.0301 0.0198 0.0184 O6 0.0367 0.0354 0.0210 O7 0.0300 0.0256 0.0166 O8 0.0664 0.0297 0.0207 O9 0.0402 0.0262 0.0162 O10 0.0553 0.0445 0.0254 O11 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.024 0.032 0.041 0.050 0.060 0.075 0.099 0.135 1.000 Number in group 263. 246. 260. 256. 239. 243. 252. 247. 249. 252. GooF 1.283 1.288 1.233 1.146 1.127 1.004 0.992 0.972 0.945 1.138 K 1.948 1.127 1.106 1.053 1.017 0.999 1.001 0.998 0.994 1.002 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.06 1.17 1.35 1.73 inf Number in group 254. 247. 254. 255. 244. 251. 254. 245. 251. 252. GooF 1.104 1.274 1.204 1.199 1.125 0.944 0.924 0.960 1.016 1.369 K 1.058 1.050 1.048 1.033 1.001 0.995 0.990 0.995 1.009 1.002 R1 0.127 0.138 0.120 0.090 0.068 0.050 0.033 0.033 0.030 0.022 Recommended weighting scheme: WGHT 0.0059 1.4135 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) 3 0 9 59.49 24.73 4.34 0.026 1.98 6 9 4 35.54 4.78 4.08 0.012 0.81 6 0 21 18.83 64.29 3.45 0.042 0.91 10 0 8 74.43 7.28 3.35 0.014 0.81 5 10 1 -4.24 15.15 3.33 0.021 0.79 3 0 8 13.10 1.32 3.28 0.006 2.09 2 2 12 3333.67 3030.92 3.18 0.291 1.74 2 9 10 66.99 27.99 3.17 0.028 0.91 9 1 17 34.42 4.87 3.14 0.012 0.78 1 10 0 -1.90 29.66 3.09 0.029 0.90 6 7 3 67.09 36.49 3.06 0.032 0.94 3 0 11 19529.83 17989.83 3.05 0.708 1.78 9 0 11 27.98 82.65 3.04 0.048 0.86 7 5 14 28.97 5.74 3.00 0.013 0.87 1 1 30 209.79 147.49 2.97 0.064 0.84 7 6 13 241.75 176.12 2.92 0.070 0.84 4 0 25 59.47 28.69 2.84 0.028 0.91 3 0 27 -6.33 9.18 2.84 0.016 0.89 3 2 10 2481.54 2265.57 2.83 0.251 1.73 6 3 21 79.28 45.66 2.81 0.036 0.87 3 0 3 68.60 42.30 2.79 0.034 2.64 3 5 3 51.15 28.55 2.76 0.028 1.49 2 4 2 2098.37 1909.75 2.76 0.231 1.96 5 1 22 41.75 18.45 2.75 0.023 0.94 3 0 17 30.62 5.94 2.73 0.013 1.32 2 4 6 60.37 36.44 2.70 0.032 1.79 7 8 1 53.79 90.47 2.68 0.050 0.82 1 2 3 3058.19 3295.54 2.68 0.303 3.59 5 4 20 49.01 26.22 2.66 0.027 0.92 0 2 1 51.93 30.84 2.66 0.029 4.44 9 1 5 90.56 58.11 2.66 0.040 0.91 2 0 2 15912.00 16859.19 2.61 0.685 3.96 5 9 5 50.12 23.24 2.60 0.025 0.85 4 10 2 71.93 41.63 2.60 0.034 0.83 0 8 16 347.67 268.39 2.58 0.086 0.92 2 4 1 4897.63 4570.03 2.58 0.357 1.98 3 0 10 8.19 0.60 2.56 0.004 1.87 2 11 6 16.19 43.21 2.55 0.035 0.79 3 8 2 18.16 38.56 2.54 0.033 1.04 4 8 4 18.05 39.23 2.53 0.033 0.98 7 3 20 109.55 74.14 2.53 0.045 0.83 4 3 27 21.84 46.72 2.51 0.036 0.82 1 1 12 3132.44 2907.20 2.50 0.285 2.00 0 9 19 83.81 48.56 2.49 0.037 0.80 3 5 1 128.93 94.82 2.48 0.051 1.51 3 9 7 25.75 8.54 2.43 0.015 0.91 5 4 19 175.65 225.89 2.42 0.079 0.95 4 3 22 17.04 2.60 2.42 0.009 0.96 1 7 19 29.04 9.88 2.42 0.017 0.92 1 0 10 2550.16 2349.45 2.41 0.256 2.43 Bond lengths and angles C1 - Distance Angles O1 1.4349 (0.0030) C2 1.5131 (0.0038) 109.88 (0.21) C6 1.5207 (0.0037) 106.92 (0.21) 113.63 (0.23) H1 1.0000 108.77 108.77 108.77 C1 - O1 C2 C6 C2 - Distance Angles O4 1.4532 (0.0032) C1 1.5131 (0.0038) 107.78 (0.21) C3 1.5257 (0.0037) 109.46 (0.21) 108.82 (0.22) H2 1.0000 110.24 110.24 110.24 C2 - O4 C1 C3 C3 - Distance Angles O6 1.4491 (0.0032) C4 1.5134 (0.0034) 108.53 (0.20) C2 1.5257 (0.0037) 110.89 (0.21) 109.91 (0.22) H3 1.0000 109.16 109.16 109.16 C3 - O6 C4 C2 C4 - Distance Angles O8 1.4383 (0.0030) C3 1.5134 (0.0034) 108.61 (0.21) C5 1.5273 (0.0038) 107.04 (0.22) 107.51 (0.21) H4 1.0000 111.17 111.17 111.17 C4 - O8 C3 C5 C5 - Distance Angles O1 1.4148 (0.0031) O10 1.4156 (0.0031) 106.17 (0.21) C4 1.5273 (0.0038) 111.61 (0.22) 107.18 (0.21) H5 1.0000 110.58 110.58 110.58 C5 - O1 O10 C4 C6 - Distance Angles O2 1.4500 (0.0031) C1 1.5207 (0.0037) 103.30 (0.20) H6A 0.9900 111.10 111.10 H6B 0.9900 111.10 111.10 109.06 C6 - O2 C1 H6A C7 - Distance Angles O3 1.2051 (0.0033) O2 1.3491 (0.0032) 122.71 (0.27) C8 1.4922 (0.0039) 126.11 (0.26) 111.18 (0.24) C7 - O3 O2 C8 - Distance Angles C7 1.4922 (0.0039) 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 O5 1.2021 (0.0035) O4 1.3575 (0.0033) 123.56 (0.28) C10 1.4960 (0.0041) 126.20 (0.27) 110.21 (0.24) C9 - O5 O4 C10 - Distance Angles C9 1.4960 (0.0041) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - C9 H10A H10B C11 - Distance Angles O7 1.2027 (0.0037) O6 1.3677 (0.0034) 122.69 (0.28) C12 1.4887 (0.0044) 125.78 (0.28) 111.51 (0.27) C11 - O7 O6 C12 - Distance Angles C11 1.4887 (0.0044) 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 C13 - Distance Angles O9 1.1941 (0.0035) O8 1.3625 (0.0031) 123.39 (0.26) C14 1.4890 (0.0039) 125.65 (0.26) 110.96 (0.24) C13 - O9 O8 C14 - Distance Angles C13 1.4890 (0.0039) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - C13 H14A H14B C15 - Distance Angles O11 1.1959 (0.0038) O10 1.3681 (0.0035) 122.66 (0.27) C16 1.4915 (0.0043) 127.06 (0.30) 110.25 (0.28) C15 - O11 O10 C16 - Distance Angles C15 1.4915 (0.0043) H16A 0.9800 109.47 H16B 0.9800 109.47 109.47 H16C 0.9800 109.47 109.47 109.47 C16 - C15 H16A H16B O1 - Distance Angles C5 1.4148 (0.0031) C1 1.4349 (0.0030) 110.23 (0.19) O1 - C5 O2 - Distance Angles C7 1.3491 (0.0032) C6 1.4500 (0.0031) 116.53 (0.21) O2 - C7 O3 - Distance Angles C7 1.2051 (0.0033) O3 - O4 - Distance Angles C9 1.3575 (0.0033) C2 1.4532 (0.0032) 117.83 (0.21) O4 - C9 O5 - Distance Angles C9 1.2021 (0.0035) O5 - O6 - Distance Angles C11 1.3677 (0.0034) C3 1.4491 (0.0032) 114.32 (0.21) O6 - C11 O7 - Distance Angles C11 1.2027 (0.0037) O7 - O8 - Distance Angles C13 1.3625 (0.0031) C4 1.4383 (0.0030) 117.24 (0.21) O8 - C13 O9 - Distance Angles C13 1.1941 (0.0035) O9 - O10 - Distance Angles C15 1.3681 (0.0035) C5 1.4156 (0.0031) 116.80 (0.23) O10 - C15 O11 - Distance Angles C15 1.1959 (0.0038) O11 - FMAP and GRID set by program FMAP 2 3 30 GRID -0.926 -2 -2 0.926 2 2 R1 = 0.0532 for 2507 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.24 at 0.8698 0.1939 0.2384 [ 0.80 A from H16C ] Deepest hole -0.21 at 0.8808 0.8785 0.0550 [ 0.96 A from C6 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2726 / 20334 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6302 0.8061 0.7384 1.00000 0.05 0.24 0.80 H16C 0.95 C16 0.97 H16A 1.74 H16B Q2 1 0.1784 0.5780 0.8404 1.00000 0.05 0.20 0.76 C4 0.80 C5 1.41 H4 1.53 H5 Q3 1 0.3809 0.9289 0.7674 1.00000 0.05 0.19 0.96 O11 1.46 C15 2.00 H16A 2.16 C16 Q4 1 0.3796 0.5216 0.8842 1.00000 0.05 0.19 0.95 O1 1.95 C1 1.97 C5 2.27 H12C Q5 1 0.1806 0.5468 0.9277 1.00000 0.05 0.19 0.75 C1 0.79 C2 1.53 H1 1.54 H2 Shortest distances between peaks (including symmetry equivalents) 4 5 2.00 2 4 2.07 2 5 2.24 1 3 2.46 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.02: Interpret restraints etc. 0.00: 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. 0.70: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.58: Structure factors and derivatives 1.73: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.06: Apply other restraints 0.31: Solve l.s. equations 0.00: Generate HTAB table 0.11: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0667a finished at 16:01:33 Total CPU time: 4.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++