+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2010src0796a started at 00:49:55 on 25-Aug-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2010src0796a CELL 0.71073 4.1302 12.9513 13.0829 62.708 86.495 86.546 ZERR 2.00 0.0002 0.0009 0.0009 0.003 0.004 0.004 LATT 1 SFAC C H N O UNIT 32 26 2 4 V = 620.35 F(000) = 264.0 Mu = 0.09 mm-1 Cell Wt = 502.55 Rho = 1.345 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 EQIV $1 [ -x-1, -y+1, -z+1 ] HTAB N1 O1_$1 SIZE 0.03 0.10 0.16 ACTA BOND $H WGHT 0.00000 1.12960 L.S. 20 TEMP -153.00 FVAR 1.02168 C1 1 -0.260061 0.437107 0.399816 11.00000 0.03096 0.03498 = 0.04600 -0.02442 0.00195 -0.00237 C2 1 -0.077633 0.359474 0.356662 11.00000 0.02430 0.03005 = 0.03501 -0.01802 0.00250 -0.00220 C3 1 0.074445 0.266489 0.457828 11.00000 0.02474 0.03129 = 0.03411 -0.01899 0.00403 -0.00856 C4 1 0.281158 0.171197 0.477282 11.00000 0.02937 0.03551 = 0.03756 -0.02282 0.00387 -0.00458 AFIX 43 H4 2 0.346741 0.154051 0.415675 11.00000 -1.20000 AFIX 0 C5 1 0.391566 0.101174 0.586731 11.00000 0.03161 0.03125 = 0.03932 -0.01584 -0.00318 -0.00057 AFIX 43 H5 2 0.531357 0.035623 0.599953 11.00000 -1.20000 AFIX 0 C6 1 0.300033 0.125858 0.677015 11.00000 0.03096 0.03532 = 0.03172 -0.01223 -0.00135 -0.00375 AFIX 43 H6 2 0.376170 0.076441 0.751669 11.00000 -1.20000 AFIX 0 C7 1 0.098411 0.221850 0.660109 11.00000 0.03072 0.04680 = 0.03469 -0.02469 0.00472 -0.00834 AFIX 43 H7 2 0.039477 0.239922 0.721575 11.00000 -1.20000 AFIX 0 C8 1 -0.012610 0.289628 0.551572 11.00000 0.02560 0.03396 = 0.04012 -0.02215 0.00270 -0.00583 C9 1 -0.070534 0.388103 0.244483 11.00000 0.03090 0.02981 = 0.03380 -0.01564 -0.00060 0.00128 AFIX 43 H9 2 -0.166970 0.461652 0.195477 11.00000 -1.20000 AFIX 0 C10 1 0.069232 0.319051 0.187819 11.00000 0.02807 0.03227 = 0.03411 -0.01804 -0.00320 0.00047 C11 1 0.023052 0.199593 0.234305 11.00000 0.02915 0.03609 = 0.03054 -0.01736 -0.00215 -0.00216 AFIX 43 H11 2 -0.097665 0.161140 0.304962 11.00000 -1.20000 AFIX 0 C12 1 0.150163 0.137121 0.179030 11.00000 0.03190 0.02981 = 0.03988 -0.02020 -0.00662 0.00222 AFIX 43 H12 2 0.115758 0.056156 0.211384 11.00000 -1.20000 AFIX 0 C13 1 0.327452 0.191781 0.076736 11.00000 0.02778 0.04476 = 0.03636 -0.02758 -0.00507 0.00507 C14 1 0.368601 0.309668 0.026987 11.00000 0.03126 0.03969 = 0.02551 -0.01356 0.00309 -0.00129 AFIX 43 H14 2 0.485310 0.347818 -0.044585 11.00000 -1.20000 AFIX 0 C15 1 0.236705 0.372193 0.083075 11.00000 0.03246 0.03247 = 0.03117 -0.01466 -0.00096 -0.00094 AFIX 43 H15 2 0.262568 0.453814 0.048327 11.00000 -1.20000 AFIX 0 C16 1 0.632462 0.171671 -0.075965 11.00000 0.04608 0.06717 = 0.04565 -0.03746 0.00748 -0.00163 AFIX 137 H16A 2 0.501451 0.233570 -0.134771 11.00000 -1.50000 H16B 2 0.696189 0.112359 -0.100881 11.00000 -1.50000 H16C 2 0.827286 0.204485 -0.064950 11.00000 -1.50000 AFIX 0 N1 3 -0.212286 0.389487 0.514754 11.00000 0.03549 0.03585 = 0.03368 -0.02242 0.00170 0.00008 AFIX 43 H1 2 -0.297062 0.418258 0.560069 11.00000 -1.20000 AFIX 0 O1 4 -0.428901 0.525136 0.343586 11.00000 0.04789 0.03906 = 0.04635 -0.02640 -0.00154 0.00858 O2 4 0.446503 0.120056 0.030044 11.00000 0.04602 0.05041 = 0.04403 -0.03226 0.00102 0.00093 HKLF 4 Covalent radii and connectivity table for 2010src0796a C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1 N1 C2 C2 - C9 C3 C1 C3 - C4 C8 C2 C4 - C5 C3 C5 - C6 C4 C6 - C5 C7 C7 - C8 C6 C8 - C7 N1 C3 C9 - C2 C10 C10 - C15 C11 C9 C11 - C12 C10 C12 - C11 C13 C13 - C14 C12 O2 C14 - C13 C15 C15 - C10 C14 C16 - O2 N1 - C1 C8 O1 - C1 O2 - C13 C16 Operators for generating equivalent atoms: $1 -x-1, -y+1, -z+1 10310 Reflections read, of which 38 rejected -5 =< h =< 5, -16 =< k =< 16, -16 =< l =< 16, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 2830 Unique reflections, of which 0 suppressed R(int) = 0.0592 R(sigma) = 0.0706 Friedel opposites merged Maximum memory for data reduction = 1763 / 28388 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 = 2242 / 215198 wR2 = 0.1633 before cycle 1 for 2830 data and 173 / 173 parameters GooF = S = 1.116; Restrained GooF = 1.116 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.02170 0.00265 0.007 OSF Mean shift/su = 0.005 Maximum = -0.014 for U13 C13 Max. shift = 0.000 A for H16C Max. dU = 0.000 for C16 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2242 / 215198 wR2 = 0.1633 before cycle 2 for 2830 data and 173 / 173 parameters GooF = S = 1.116; Restrained GooF = 1.116 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.02172 0.00265 0.008 OSF Mean shift/su = 0.002 Maximum = 0.008 for OSF Max. shift = 0.000 A for H16C Max. dU = 0.000 for C16 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2242 / 215198 wR2 = 0.1633 before cycle 3 for 2830 data and 173 / 173 parameters GooF = S = 1.116; Restrained GooF = 1.116 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.02172 0.00265 0.001 OSF Mean shift/su = 0.000 Maximum = 0.001 for U22 C16 Max. shift = 0.000 A for H16C Max. dU = 0.000 for C16 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2242 / 215198 wR2 = 0.1633 before cycle 4 for 2830 data and 173 / 173 parameters GooF = S = 1.116; Restrained GooF = 1.116 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.02172 0.00265 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z C13 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C16 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2242 / 215198 wR2 = 0.1633 before cycle 5 for 2830 data and 173 / 173 parameters GooF = S = 1.116; Restrained GooF = 1.116 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.02172 0.00265 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C16 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2242 / 215198 wR2 = 0.1633 before cycle 6 for 2830 data and 173 / 173 parameters GooF = S = 1.116; Restrained GooF = 1.116 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.02172 0.00265 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C11 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2242 / 215198 wR2 = 0.1633 before cycle 7 for 2830 data and 173 / 173 parameters GooF = S = 1.116; Restrained GooF = 1.116 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.02172 0.00265 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z C7 Max. shift = 0.000 A for C7 Max. dU = 0.000 for O2 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2242 / 215198 wR2 = 0.1633 before cycle 8 for 2830 data and 173 / 173 parameters GooF = S = 1.116; Restrained GooF = 1.116 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.02172 0.00265 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C8 Least-squares cycle 9 Maximum vector length = 511 Memory required = 2242 / 215198 wR2 = 0.1633 before cycle 9 for 2830 data and 173 / 173 parameters GooF = S = 1.116; Restrained GooF = 1.116 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.02172 0.00265 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for H16B Max. dU = 0.000 for O2 Least-squares cycle 10 Maximum vector length = 511 Memory required = 2242 / 215198 wR2 = 0.1633 before cycle 10 for 2830 data and 173 / 173 parameters GooF = S = 1.116; Restrained GooF = 1.116 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.02172 0.00265 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C6 Least-squares cycle 11 Maximum vector length = 511 Memory required = 2242 / 215198 wR2 = 0.1633 before cycle 11 for 2830 data and 173 / 173 parameters GooF = S = 1.116; Restrained GooF = 1.116 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.02172 0.00265 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for O2 Max. dU = 0.000 for C3 Least-squares cycle 12 Maximum vector length = 511 Memory required = 2242 / 215198 wR2 = 0.1633 before cycle 12 for 2830 data and 173 / 173 parameters GooF = S = 1.116; Restrained GooF = 1.116 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.02172 0.00265 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C16 Least-squares cycle 13 Maximum vector length = 511 Memory required = 2242 / 215198 wR2 = 0.1633 before cycle 13 for 2830 data and 173 / 173 parameters GooF = S = 1.116; Restrained GooF = 1.116 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.02172 0.00265 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for H16C Max. dU = 0.000 for C7 Least-squares cycle 14 Maximum vector length = 511 Memory required = 2242 / 215198 wR2 = 0.1633 before cycle 14 for 2830 data and 173 / 173 parameters GooF = S = 1.116; Restrained GooF = 1.116 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.02172 0.00265 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C6 Least-squares cycle 15 Maximum vector length = 511 Memory required = 2242 / 215198 wR2 = 0.1633 before cycle 15 for 2830 data and 173 / 173 parameters GooF = S = 1.116; Restrained GooF = 1.116 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.02172 0.00265 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for C10 Max. dU = 0.000 for C2 Least-squares cycle 16 Maximum vector length = 511 Memory required = 2242 / 215198 wR2 = 0.1633 before cycle 16 for 2830 data and 173 / 173 parameters GooF = S = 1.116; Restrained GooF = 1.116 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.02172 0.00265 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C13 Least-squares cycle 17 Maximum vector length = 511 Memory required = 2242 / 215198 wR2 = 0.1633 before cycle 17 for 2830 data and 173 / 173 parameters GooF = S = 1.116; Restrained GooF = 1.116 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.02172 0.00265 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for C10 Max. dU = 0.000 for O1 Least-squares cycle 18 Maximum vector length = 511 Memory required = 2242 / 215198 wR2 = 0.1633 before cycle 18 for 2830 data and 173 / 173 parameters GooF = S = 1.116; Restrained GooF = 1.116 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.02172 0.00265 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for H16C Max. dU = 0.000 for C10 Least-squares cycle 19 Maximum vector length = 511 Memory required = 2242 / 215198 wR2 = 0.1633 before cycle 19 for 2830 data and 173 / 173 parameters GooF = S = 1.116; Restrained GooF = 1.116 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.02172 0.00265 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C11 Least-squares cycle 20 Maximum vector length = 511 Memory required = 2242 / 215198 wR2 = 0.1633 before cycle 20 for 2830 data and 173 / 173 parameters GooF = S = 1.116; Restrained GooF = 1.116 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.02172 0.00265 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for C10 Max. dU = 0.000 for C3 Largest correlation matrix elements -0.653 U23 C16 / U22 C16 -0.618 U23 C1 / U22 C1 -0.607 U23 C8 / U33 C8 -0.653 U23 C16 / U33 C16 -0.618 U23 C7 / U33 C7 -0.605 U23 C7 / U22 C7 -0.652 U23 O2 / U22 O2 -0.616 U23 C4 / U33 C4 -0.601 U23 C12 / U33 C12 -0.652 U23 O2 / U33 O2 -0.615 U23 C4 / U22 C4 -0.592 U23 C3 / U33 C3 -0.641 U23 C13 / U22 C13 -0.612 U23 O1 / U33 O1 -0.591 U23 C12 / U22 C12 -0.635 U23 C13 / U33 C13 -0.611 U23 N1 / U22 N1 -0.587 U23 C3 / U22 C3 -0.622 U23 O1 / U22 O1 -0.608 U23 C8 / U22 C8 -0.586 U23 C2 / U33 C2 -0.618 U23 N1 / U33 N1 -0.608 U23 C1 / U33 C1 -0.584 U23 C11 / U22 C11 Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H4 0.3467 0.1541 0.4157 43 0.950 0.000 C4 C5 C3 H5 0.5314 0.0356 0.6000 43 0.950 0.000 C5 C6 C4 H6 0.3761 0.0764 0.7517 43 0.950 0.000 C6 C5 C7 H7 0.0395 0.2399 0.7216 43 0.950 0.000 C7 C8 C6 H9 -0.1669 0.4617 0.1955 43 0.950 0.000 C9 C2 C10 H11 -0.0976 0.1611 0.3050 43 0.950 0.000 C11 C12 C10 H12 0.1158 0.0562 0.2114 43 0.950 0.000 C12 C11 C13 H14 0.4853 0.3478 -0.0446 43 0.950 0.000 C14 C13 C15 H15 0.2626 0.4538 0.0483 43 0.950 0.000 C15 C10 C14 H16A 0.5014 0.2336 -0.1348 137 0.980 0.000 C16 O2 H16A H16B 0.6962 0.1124 -0.1009 137 0.980 0.000 C16 O2 H16A H16C 0.8273 0.2045 -0.0650 137 0.980 0.000 C16 O2 H16A H1 -0.2971 0.4183 0.5601 43 0.880 0.000 N1 C1 C8 2010src0796a ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.26006 0.43710 0.39982 1.00000 0.03096 0.03499 0.04598 -0.02441 0.00194 -0.00238 0.03512 0.00497 0.00079 0.00030 0.00031 0.00000 0.00179 0.00191 0.00217 0.00173 0.00155 0.00152 0.00080 C2 -0.07763 0.35947 0.35666 1.00000 0.02430 0.03007 0.03502 -0.01803 0.00249 -0.00221 0.02868 0.00469 0.00073 0.00027 0.00028 0.00000 0.00155 0.00169 0.00183 0.00147 0.00132 0.00130 0.00070 C3 0.07444 0.26649 0.45783 1.00000 0.02472 0.03128 0.03411 -0.01898 0.00404 -0.00856 0.02836 0.00451 0.00072 0.00027 0.00027 0.00000 0.00157 0.00171 0.00178 0.00147 0.00133 0.00133 0.00070 C4 0.28116 0.17120 0.47728 1.00000 0.02938 0.03552 0.03759 -0.02283 0.00389 -0.00461 0.03186 0.00476 0.00075 0.00028 0.00029 0.00000 0.00169 0.00184 0.00191 0.00159 0.00142 0.00143 0.00075 H4 0.34674 0.15405 0.41567 1.00000 0.03824 0.00000 0.00000 C5 0.39156 0.10118 0.58673 1.00000 0.03161 0.03127 0.03932 -0.01585 -0.00317 -0.00057 0.03411 0.00490 0.00079 0.00029 0.00029 0.00000 0.00175 0.00179 0.00200 0.00159 0.00148 0.00144 0.00077 H5 0.53136 0.03563 0.59995 1.00000 0.04094 0.00000 0.00000 C6 0.30002 0.12586 0.67701 1.00000 0.03093 0.03533 0.03174 -0.01223 -0.00135 -0.00374 0.03374 0.00497 0.00078 0.00029 0.00029 0.00000 0.00174 0.00185 0.00182 0.00152 0.00141 0.00145 0.00076 H6 0.37615 0.07644 0.75167 1.00000 0.04049 0.00000 0.00000 C7 0.09841 0.22185 0.66011 1.00000 0.03072 0.04682 0.03471 -0.02471 0.00472 -0.00834 0.03501 0.00486 0.00077 0.00030 0.00029 0.00000 0.00174 0.00213 0.00193 0.00172 0.00147 0.00156 0.00080 H7 0.03948 0.23992 0.72157 1.00000 0.04201 0.00000 0.00000 C8 -0.01261 0.28963 0.55157 1.00000 0.02561 0.03396 0.04009 -0.02213 0.00270 -0.00583 0.03116 0.00465 0.00074 0.00028 0.00029 0.00000 0.00163 0.00182 0.00196 0.00161 0.00141 0.00139 0.00074 C9 -0.07052 0.38810 0.24449 1.00000 0.03089 0.02983 0.03383 -0.01564 -0.00062 0.00129 0.03122 0.00479 0.00076 0.00028 0.00028 0.00000 0.00171 0.00176 0.00187 0.00151 0.00141 0.00139 0.00074 H9 -0.16695 0.46165 0.19548 1.00000 0.03746 0.00000 0.00000 C10 0.06923 0.31905 0.18782 1.00000 0.02806 0.03230 0.03411 -0.01805 -0.00320 0.00047 0.03035 0.00466 0.00075 0.00028 0.00028 0.00000 0.00166 0.00177 0.00182 0.00151 0.00139 0.00138 0.00073 C11 0.02306 0.19959 0.23430 1.00000 0.02915 0.03611 0.03052 -0.01735 -0.00216 -0.00215 0.03101 0.00466 0.00076 0.00029 0.00028 0.00000 0.00168 0.00185 0.00179 0.00153 0.00137 0.00141 0.00073 H11 -0.09765 0.16114 0.30496 1.00000 0.03721 0.00000 0.00000 C12 0.15016 0.13713 0.17903 1.00000 0.03191 0.02980 0.03988 -0.02020 -0.00660 0.00223 0.03211 0.00471 0.00076 0.00029 0.00029 0.00000 0.00175 0.00173 0.00196 0.00156 0.00146 0.00141 0.00075 H12 0.11576 0.05616 0.21138 1.00000 0.03853 0.00000 0.00000 C13 0.32745 0.19178 0.07673 1.00000 0.02778 0.04472 0.03637 -0.02756 -0.00510 0.00509 0.03290 0.00479 0.00077 0.00031 0.00029 0.00000 0.00165 0.00204 0.00191 0.00169 0.00143 0.00148 0.00077 C14 0.36860 0.30966 0.02699 1.00000 0.03127 0.03972 0.02552 -0.01358 0.00309 -0.00128 0.03287 0.00494 0.00077 0.00029 0.00028 0.00000 0.00176 0.00198 0.00169 0.00153 0.00136 0.00149 0.00077 H14 0.48531 0.34781 -0.04458 1.00000 0.03944 0.00000 0.00000 C15 0.23670 0.37219 0.08308 1.00000 0.03247 0.03246 0.03118 -0.01464 -0.00095 -0.00096 0.03201 0.00482 0.00076 0.00029 0.00027 0.00000 0.00176 0.00179 0.00181 0.00151 0.00142 0.00143 0.00075 H15 0.26257 0.45381 0.04833 1.00000 0.03841 0.00000 0.00000 C16 0.63246 0.17167 -0.07596 1.00000 0.04612 0.06723 0.04564 -0.03749 0.00749 -0.00164 0.04889 0.00596 0.00093 0.00037 0.00032 0.00000 0.00222 0.00273 0.00230 0.00216 0.00181 0.00198 0.00101 H16A 0.50143 0.23356 -0.13477 1.00000 0.07334 0.00000 0.00000 H16B 0.69624 0.11236 -0.10087 1.00000 0.07334 0.00000 0.00000 H16C 0.82725 0.20450 -0.06495 1.00000 0.07334 0.00000 0.00000 N1 -0.21229 0.38949 0.51475 1.00000 0.03549 0.03585 0.03371 -0.02244 0.00170 0.00008 0.03267 0.00400 0.00064 0.00023 0.00023 0.00000 0.00152 0.00156 0.00158 0.00132 0.00122 0.00124 0.00065 H1 -0.29707 0.41826 0.56007 1.00000 0.03921 0.00000 0.00000 O1 -0.42890 0.52514 0.34359 1.00000 0.04791 0.03906 0.04636 -0.02639 -0.00154 0.00858 0.04224 0.00372 0.00060 0.00021 0.00021 0.00000 0.00149 0.00143 0.00151 0.00124 0.00120 0.00120 0.00063 O2 0.44650 0.12006 0.03004 1.00000 0.04604 0.05043 0.04405 -0.03229 0.00103 0.00093 0.04293 0.00362 0.00059 0.00022 0.00021 0.00000 0.00146 0.00156 0.00150 0.00131 0.00119 0.00121 0.00064 Final Structure Factor Calculation for 2010src0796a Total number of l.s. parameters = 173 Maximum vector length = 511 Memory required = 2069 / 22995 wR2 = 0.1633 before cycle 21 for 2830 data and 0 / 173 parameters GooF = S = 1.116; Restrained GooF = 1.116 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 1.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0877 for 1847 Fo > 4sig(Fo) and 0.1415 for all 2830 data wR2 = 0.1633, GooF = S = 1.116, Restrained GooF = 1.116 for all data Occupancy sum of asymmetric unit = 19.00 for non-hydrogen and 13.00 for hydrogen atoms Principal mean square atomic displacements U 0.0475 0.0306 0.0273 C1 0.0366 0.0263 0.0231 C2 0.0393 0.0267 0.0191 C3 0.0429 0.0277 0.0250 C4 0.0403 0.0312 0.0308 C5 0.0403 0.0313 0.0296 C6 0.0502 0.0287 0.0261 C7 0.0429 0.0278 0.0228 C8 0.0341 0.0329 0.0267 C9 0.0359 0.0280 0.0272 C10 0.0363 0.0304 0.0264 C11 0.0427 0.0291 0.0245 C12 0.0496 0.0261 0.0229 C13 0.0420 0.0335 0.0231 C14 0.0328 0.0323 0.0310 C15 0.0689 0.0512 0.0265 C16 0.0395 0.0367 0.0218 N1 0.0550 0.0468 0.0250 O1 0.0551 0.0473 0.0263 O2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.013 0.020 0.028 0.036 0.048 0.062 0.085 0.128 1.000 Number in group 312. 269. 295. 272. 268. 298. 271. 283. 279. 283. GooF 1.260 1.147 1.106 1.179 1.184 1.149 1.084 0.983 0.947 1.073 K 18.285 2.487 1.533 1.256 1.128 1.046 1.018 0.997 0.997 1.008 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.04 1.15 1.31 1.66 inf Number in group 289. 278. 291. 284. 273. 286. 280. 281. 285. 283. GooF 1.241 1.257 1.234 1.191 1.123 1.074 0.955 0.925 0.876 1.197 K 1.289 1.181 1.193 1.093 1.064 1.001 0.994 0.983 1.010 1.007 R1 0.355 0.337 0.287 0.262 0.180 0.145 0.081 0.074 0.059 0.039 Recommended weighting scheme: WGHT 0.0000 1.1281 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) 2 14 6 30.43 0.42 3.87 0.007 0.86 -1 1 0 323.47 247.03 3.67 0.162 3.83 1 1 12 28.11 0.62 3.49 0.008 0.98 4 11 5 18.14 0.23 3.44 0.005 0.80 1 -4 9 44.52 18.43 3.13 0.044 0.99 -4 0 9 28.56 4.58 3.11 0.022 0.79 1 0 0 203.61 153.96 3.11 0.128 4.12 -1 6 4 312.48 249.23 3.08 0.163 1.82 -1 4 4 438.17 362.15 3.04 0.197 2.23 4 -7 3 37.65 8.01 2.99 0.029 0.80 2 3 11 23.88 0.46 2.97 0.007 1.04 -4 4 4 9.19 0.05 2.97 0.002 0.94 4 -4 6 21.21 1.42 2.95 0.012 0.82 -5 3 4 31.16 0.22 2.93 0.005 0.78 -2 7 2 -1.72 11.06 2.92 0.034 1.33 2 14 8 23.75 0.07 2.89 0.003 0.86 -2 -7 7 18.19 0.12 2.89 0.004 0.88 2 3 14 18.71 2.74 2.84 0.017 0.84 0 3 0 831.76 947.09 2.84 0.318 3.83 -4 -5 6 34.54 9.49 2.82 0.032 0.79 0 -2 1 1296.49 1440.72 2.79 0.392 4.41 -2 -2 11 59.50 30.24 2.78 0.057 0.86 0 -1 1 2318.70 2558.29 2.77 0.523 6.77 -1 12 3 27.37 48.18 2.77 0.072 1.00 0 3 1 110.39 148.65 2.76 0.126 4.27 2 -3 12 22.42 0.09 2.75 0.003 0.79 1 3 13 41.77 19.50 2.73 0.046 0.96 5 3 6 51.29 18.45 2.68 0.044 0.79 5 4 0 16.76 0.11 2.66 0.003 0.80 3 6 10 -4.74 6.13 2.63 0.026 0.97 4 3 8 236.93 181.81 2.63 0.139 0.89 2 -11 2 11.87 0.00 2.59 0.001 0.86 3 7 0 -2.60 5.70 2.59 0.025 1.07 2 4 13 28.64 8.11 2.57 0.029 0.91 0 2 14 25.39 3.26 2.57 0.019 0.88 -1 0 13 34.70 17.14 2.56 0.043 0.87 -2 -7 9 25.94 5.58 2.55 0.024 0.78 -3 5 12 29.26 5.19 2.55 0.024 0.83 -2 10 13 65.81 36.23 2.54 0.062 0.84 -1 15 11 51.31 23.05 2.53 0.050 0.80 1 10 3 32.29 56.74 2.52 0.078 1.23 3 -7 5 16.14 3.30 2.51 0.019 0.87 5 4 5 16.15 1.64 2.50 0.013 0.80 -1 12 15 31.78 13.09 2.50 0.037 0.78 5 6 3 33.04 15.26 2.48 0.040 0.79 5 3 0 2.71 16.68 2.46 0.042 0.81 -4 4 10 26.61 1.41 2.45 0.012 0.79 -4 2 10 16.88 1.77 2.44 0.014 0.78 0 -3 9 8.92 0.00 2.43 0.000 1.08 -1 -10 3 44.26 24.39 2.43 0.051 0.96 Bond lengths and angles C1 - Distance Angles O1 1.2350 (0.0040) N1 1.3607 (0.0042) 125.94 (0.30) C2 1.5082 (0.0042) 127.28 (0.32) 106.75 (0.28) C1 - O1 N1 C2 - Distance Angles C9 1.3376 (0.0044) C3 1.4647 (0.0045) 134.66 (0.29) C1 1.5082 (0.0042) 119.88 (0.30) 105.36 (0.27) C2 - C9 C3 C3 - Distance Angles C4 1.3887 (0.0044) C8 1.4119 (0.0043) 118.09 (0.30) C2 1.4647 (0.0045) 135.07 (0.29) 106.77 (0.27) C3 - C4 C8 C4 - Distance Angles C5 1.3856 (0.0046) C3 1.3887 (0.0044) 119.86 (0.30) H4 0.9500 120.07 120.07 C4 - C5 C3 C5 - Distance Angles C6 1.3847 (0.0045) C4 1.3856 (0.0046) 120.61 (0.31) H5 0.9500 119.69 119.69 C5 - C6 C4 C6 - Distance Angles C5 1.3847 (0.0045) C7 1.3905 (0.0046) 121.03 (0.32) H6 0.9500 119.48 119.48 C6 - C5 C7 C7 - Distance Angles C8 1.3730 (0.0046) C6 1.3905 (0.0046) 117.75 (0.30) H7 0.9500 121.13 121.13 C7 - C8 C6 C8 - Distance Angles C7 1.3730 (0.0046) N1 1.3905 (0.0040) 127.69 (0.29) C3 1.4119 (0.0043) 122.64 (0.30) 109.65 (0.29) C8 - C7 N1 C9 - Distance Angles C2 1.3376 (0.0044) C10 1.4751 (0.0042) 127.73 (0.30) H9 0.9500 116.14 116.14 C9 - C2 C10 C10 - Distance Angles C15 1.3808 (0.0044) C11 1.3994 (0.0045) 117.65 (0.29) C9 1.4751 (0.0042) 120.53 (0.29) 121.73 (0.29) C10 - C15 C11 C11 - Distance Angles C12 1.3755 (0.0043) C10 1.3994 (0.0045) 120.86 (0.31) H11 0.9500 119.57 119.57 C11 - C12 C10 C12 - Distance Angles C11 1.3755 (0.0043) C13 1.3792 (0.0046) 120.14 (0.31) H12 0.9500 119.93 119.93 C12 - C11 C13 C13 - Distance Angles C14 1.3747 (0.0046) C12 1.3792 (0.0046) 120.41 (0.29) O2 1.3808 (0.0037) 124.60 (0.30) 114.98 (0.30) C13 - C14 C12 C14 - Distance Angles C13 1.3747 (0.0046) C15 1.3906 (0.0044) 118.96 (0.30) H14 0.9500 120.52 120.52 C14 - C13 C15 C15 - Distance Angles C10 1.3808 (0.0044) C14 1.3906 (0.0044) 121.89 (0.31) H15 0.9500 119.06 119.06 C15 - C10 C14 C16 - Distance Angles O2 1.4288 (0.0042) H16A 0.9800 109.47 H16B 0.9800 109.47 109.47 H16C 0.9800 109.47 109.47 109.47 C16 - O2 H16A H16B N1 - Distance Angles C1 1.3607 (0.0042) C8 1.3905 (0.0040) 111.46 (0.26) H1 0.8800 124.27 124.27 N1 - C1 C8 O1 - Distance Angles C1 1.2350 (0.0040) O1 - O2 - Distance Angles C13 1.3808 (0.0037) C16 1.4288 (0.0042) 117.59 (0.28) O2 - C13 Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.00 2.864(3) 168.9 N1-H1...O1_$1 FMAP and GRID set by program FMAP 2 1 25 GRID -4.545 -2 -1 4.545 2 1 R1 = 0.1415 for 2830 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.31 at 0.1467 0.2458 0.2520 [ 0.92 A from C11 ] Deepest hole -0.26 at 0.3265 0.8768 0.0148 [ 0.78 A from C16 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2342 / 28273 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1467 0.2458 0.2520 1.00000 0.05 0.31 0.92 C11 0.99 C10 1.43 H11 1.96 C9 Q2 1 0.2724 0.3751 0.1620 1.00000 0.05 0.25 1.07 C15 1.08 C10 1.37 H15 1.77 C9 Q3 1 0.2564 0.1066 0.6337 1.00000 0.05 0.24 0.75 C6 0.83 C5 1.52 H6 1.59 H5 Q4 1 -0.6501 0.5992 0.2485 1.00000 0.05 0.24 1.50 O1 2.09 H16A 2.41 H1 2.49 H14 Q5 1 0.1064 0.3544 0.2171 1.00000 0.05 0.24 0.75 C10 0.96 C9 1.67 H9 1.72 C15 Q6 1 0.1916 0.1552 0.2299 1.00000 0.05 0.23 0.83 C12 0.89 C11 1.47 H12 1.52 H11 Q7 1 0.3263 0.5208 0.0512 1.00000 0.05 0.23 0.94 H15 1.83 C15 1.88 H14 2.02 H15 Q8 1 0.1318 0.3031 0.4938 1.00000 0.05 0.22 0.86 C3 0.89 C8 1.84 N1 1.85 C2 Q9 1 0.1871 0.0381 0.0641 1.00000 0.05 0.22 1.46 O2 1.82 H16B 2.05 H12 2.19 C13 Q10 1 0.2568 0.2582 0.4416 1.00000 0.05 0.22 0.78 C3 1.00 C4 1.55 H4 1.87 C2 Q11 1 0.0025 0.2766 0.7320 1.00000 0.05 0.21 0.56 H7 1.44 C7 2.29 C8 2.45 H16C Q12 1 0.3718 0.3797 -0.0916 1.00000 0.05 0.21 0.74 H14 1.39 C14 2.04 H9 2.24 H16A Q13 1 -0.5438 0.3726 0.2279 1.00000 0.05 0.21 1.90 H9 1.97 C10 2.01 C9 2.15 C15 Q14 1 -0.1012 0.4393 0.3459 1.00000 0.05 0.21 0.93 C1 0.98 C2 1.69 O1 1.73 C9 Q15 1 0.3136 0.0552 0.0184 1.00000 0.05 0.21 1.10 O2 1.93 H16B 1.97 C16 2.06 H16B Q16 1 -0.0966 0.2196 0.7596 1.00000 0.05 0.21 0.70 H7 1.48 C7 1.90 H16B 2.15 H16A Q17 1 1.0119 0.1217 -0.1665 1.00000 0.05 0.20 1.50 H16B 1.56 H7 2.01 H6 2.05 C7 Q18 1 0.1643 0.2544 0.3089 1.00000 0.05 0.20 1.48 C10 1.60 C11 1.60 H4 1.69 H11 Q19 1 0.6765 0.0413 -0.0390 1.00000 0.05 0.20 0.91 H16B 1.53 C16 1.84 O2 2.11 H16C Q20 1 0.3586 0.1850 -0.0252 1.00000 0.05 0.20 0.89 O2 1.32 C16 1.37 C13 1.38 H16A Shortest distances between peaks (including symmetry equivalents) 9 15 0.73 11 16 0.79 1 18 0.81 2 5 0.92 15 19 1.15 8 10 1.16 2 13 1.17 16 17 1.27 1 5 1.27 9 19 1.30 5 18 1.32 1 6 1.33 5 13 1.50 15 20 1.53 1 2 1.64 15 19 1.67 2 7 1.79 19 19 1.82 10 18 1.82 11 17 1.83 13 18 1.87 9 20 1.87 2 18 1.89 6 18 1.98 17 19 2.02 1 13 2.04 9 17 2.07 7 12 2.10 7 7 2.12 8 14 2.16 4 11 2.19 4 12 2.20 15 15 2.22 12 20 2.26 19 20 2.28 7 13 2.30 9 19 2.35 3 10 2.38 3 8 2.40 5 7 2.43 4 16 2.47 5 14 2.49 5 6 2.51 10 14 2.52 15 17 2.54 10 13 2.60 2 6 2.60 15 17 2.61 1 10 2.63 19 20 2.66 4 14 2.67 5 10 2.71 9 15 2.74 16 19 2.74 8 18 2.76 14 18 2.80 9 17 2.82 17 20 2.83 3 17 2.83 9 9 2.86 17 19 2.87 13 14 2.87 2 7 2.93 3 16 2.94 12 13 2.98 8 11 2.99 Time profile in seconds ----------------------- 0.00: Read and process instructions 0.00: Fit rigid groups 0.00: 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 0.02: Analyse other restraints etc. 0.39: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.95: Structure factors and derivatives 1.97: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.30: Solve l.s. equations 0.00: Generate HTAB table 0.09: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010src0796a finished at 00:50:00 Total CPU time: 3.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++