+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0769 started at 15:32:30 on 04-Jul-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0769 in P-1 CELL 0.71073 8.8971 9.5970 9.8882 64.918 81.546 68.435 ZERR 1.00 0.0004 0.0004 0.0003 0.002 0.002 0.002 LATT 1 SFAC C H N O UNIT 22 48 8 6 V = 711.13 F(000) = 284.0 Mu = 0.09 mm-1 Cell Wt = 520.68 Rho = 1.216 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 EQIV $1 -x+1, -y+3, -z+2 EQIV $2 -x+1, -y+2, -z+2 EQIV $3 -x+1, -y+3, -z+1 EQIV $4 x+1, y-1, z+1 HTAB N3 O1_$1 HTAB N3 O101_$2 HTAB N4 O1_$3 HTAB N4 N1 HTAB O101 O2_$4 FMAP 2 PLAN 5 SIZE 0.06 0.12 0.22 ACTA HTAB 2.00000 BOND $H WGHT 0.02190 0.82630 L.S. 20 TEMP -153.00 FVAR 1.07689 MOLE 1 C1 1 0.685205 1.144788 0.565253 11.00000 0.01709 0.02342 = 0.03243 -0.01586 0.00225 -0.00821 AFIX 23 H1A 2 0.778319 1.045710 0.615822 11.00000 -1.20000 H1B 2 0.706459 1.239931 0.563218 11.00000 -1.20000 AFIX 0 C2 1 0.540260 0.960058 0.717414 11.00000 0.02087 0.01856 = 0.02752 -0.00967 -0.00205 -0.00578 AFIX 23 H2A 2 0.606379 0.896630 0.810184 11.00000 -1.20000 H2B 2 0.591250 0.909577 0.645603 11.00000 -1.20000 AFIX 0 C3 1 0.370589 0.950864 0.752277 11.00000 0.02108 0.02316 = 0.02213 -0.00894 -0.00068 -0.00756 AFIX 23 H3A 2 0.377205 0.839978 0.826679 11.00000 -1.20000 H3B 2 0.306799 1.030413 0.795931 11.00000 -1.20000 AFIX 0 C4 1 0.325319 0.834870 0.594401 11.00000 0.01944 0.01897 = 0.02747 -0.00965 0.00389 -0.00832 AFIX 23 H4A 2 0.249672 0.778821 0.655813 11.00000 -1.20000 H4B 2 0.435856 0.762187 0.633068 11.00000 -1.20000 AFIX 0 C5 1 0.528413 1.184147 0.775693 11.00000 0.02300 0.02348 = 0.02149 -0.01061 -0.00240 -0.00748 AFIX 23 H5A 2 0.637007 1.140419 0.820999 11.00000 -1.20000 H5B 2 0.455996 1.138553 0.854066 11.00000 -1.20000 AFIX 0 C6 1 0.464696 1.370845 0.720468 11.00000 0.02723 0.02214 = 0.02108 -0.01026 -0.00200 -0.00703 AFIX 23 H6A 2 0.524950 1.418288 0.630649 11.00000 -1.20000 H6B 2 0.349155 1.413548 0.692278 11.00000 -1.20000 AFIX 0 C7 1 0.483519 1.421977 0.840473 11.00000 0.02538 0.01536 = 0.01922 -0.00517 -0.00193 -0.00562 C8 1 0.113818 1.065169 0.621211 11.00000 0.01864 0.02076 = 0.02819 -0.01111 0.00316 -0.00859 AFIX 23 H8A 2 0.073682 1.002876 0.718607 11.00000 -1.20000 H8B 2 0.061596 1.060925 0.541934 11.00000 -1.20000 AFIX 0 C9 1 0.065303 1.242486 0.600636 11.00000 0.02011 0.02259 = 0.02839 -0.01282 0.00203 -0.00613 AFIX 23 H9A 2 -0.051869 1.284375 0.619148 11.00000 -1.20000 H9B 2 0.124101 1.248169 0.674678 11.00000 -1.20000 AFIX 0 C10 1 0.102281 1.349182 0.445184 11.00000 0.01937 0.01768 = 0.02817 -0.01022 -0.00173 -0.00264 N1 3 0.538697 1.130410 0.653924 11.00000 0.01783 0.01952 = 0.02315 -0.01117 0.00101 -0.00638 N2 3 0.288917 0.987152 0.615800 11.00000 0.01835 0.01791 = 0.02245 -0.00888 -0.00029 -0.00594 N3 3 0.368250 1.424888 0.941121 11.00000 0.02526 0.03205 = 0.02118 -0.01381 0.00274 -0.01430 AFIX 93 H3C 2 0.375599 1.451361 1.014300 11.00000 -1.20000 H3D 2 0.284121 1.400355 0.934983 11.00000 -1.20000 AFIX 0 N4 3 0.244638 1.370759 0.427010 11.00000 0.02380 0.02573 = 0.02231 -0.00739 0.00008 -0.00882 AFIX 93 H4C 2 0.271556 1.432438 0.338730 11.00000 -1.20000 H4D 2 0.311783 1.323337 0.503280 11.00000 -1.20000 AFIX 0 O1 4 0.605066 1.455507 0.843622 11.00000 0.02767 0.03366 = 0.02530 -0.01520 0.00421 -0.01570 O2 4 0.002196 1.411862 0.343291 11.00000 0.03201 0.03590 = 0.03379 -0.00424 -0.00985 -0.01236 MOLE 2 C101 1 0.984613 0.747285 0.987697 11.00000 0.03414 0.05712 = 0.04813 -0.00175 0.00453 -0.01965 AFIX 137 H11A 2 1.079181 0.734973 1.037193 11.00000 -1.50000 H11B 2 0.926106 0.863791 0.931483 11.00000 -1.50000 H11C 2 1.019917 0.691898 0.919170 11.00000 -1.50000 AFIX 0 O101 4 0.882254 0.677281 1.095616 11.00000 0.03009 0.04235 = 0.03050 -0.00519 -0.00518 -0.01689 AFIX 147 H101 2 0.938108 0.589046 1.161368 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 2007src0769 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - N1 C4_$5 C2 - N1 C3 C3 - N2 C2 C4 - N2 C1_$5 C5 - N1 C6 C6 - C7 C5 C7 - O1 N3 C6 C8 - N2 C9 C9 - C10 C8 C10 - O2 N4 C9 N1 - C1 C2 C5 N2 - C8 C3 C4 N3 - C7 N4 - C10 O1 - C7 O2 - C10 C101 - O101 O101 - C101 Operators for generating equivalent atoms: $1 -x+1, -y+3, -z+2 $2 -x+1, -y+2, -z+2 $3 -x+1, -y+3, -z+1 $4 x+1, y-1, z+1 $5 -x+1, -y+2, -z+1 11965 Reflections read, of which 21 rejected -11 =< h =< 11, -12 =< k =< 12, -12 =< l =< 12, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -1 -7 4 0.58 0.19 4 1.03 1 Inconsistent equivalents 3234 Unique reflections, of which 0 suppressed R(int) = 0.0487 R(sigma) = 0.0498 Friedel opposites merged Maximum memory for data reduction = 2328 / 32651 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 = 2853 / 205650 wR2 = 0.1332 before cycle 1 for 3234 data and 165 / 165 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0219 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07688 0.00230 -0.002 OSF Mean shift/esd = 0.002 Maximum = 0.005 for U12 C7 Max. shift = 0.000 A for H101 Max. dU = 0.000 for C5 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2853 / 205650 wR2 = 0.1332 before cycle 2 for 3234 data and 165 / 165 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0219 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07688 0.00230 -0.001 OSF Mean shift/esd = 0.001 Maximum = -0.002 for U13 O101 Max. shift = 0.000 A for H101 Max. dU = 0.000 for C5 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2853 / 205650 wR2 = 0.1332 before cycle 3 for 3234 data and 165 / 165 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0219 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07688 0.00230 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for tors H11A Max. shift = 0.000 A for H11C Max. dU = 0.000 for C3 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2853 / 205650 wR2 = 0.1332 before cycle 4 for 3234 data and 165 / 165 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0219 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07688 0.00230 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H11B Max. dU = 0.000 for C4 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2853 / 205650 wR2 = 0.1332 before cycle 5 for 3234 data and 165 / 165 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0219 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07688 0.00230 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C5 Max. shift = 0.000 A for H11C Max. dU = 0.000 for O1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2853 / 205650 wR2 = 0.1332 before cycle 6 for 3234 data and 165 / 165 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0219 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07688 0.00230 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O101 Max. shift = 0.000 A for H11B Max. dU = 0.000 for O101 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2853 / 205650 wR2 = 0.1332 before cycle 7 for 3234 data and 165 / 165 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0219 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07688 0.00230 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C5 Max. shift = 0.000 A for H11C Max. dU = 0.000 for C101 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2853 / 205650 wR2 = 0.1332 before cycle 8 for 3234 data and 165 / 165 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0219 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07688 0.00230 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O101 Max. shift = 0.000 A for C7 Max. dU = 0.000 for N2 Least-squares cycle 9 Maximum vector length = 511 Memory required = 2853 / 205650 wR2 = 0.1332 before cycle 9 for 3234 data and 165 / 165 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0219 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07688 0.00230 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O101 Max. shift = 0.000 A for O2 Max. dU = 0.000 for C5 Least-squares cycle 10 Maximum vector length = 511 Memory required = 2853 / 205650 wR2 = 0.1332 before cycle 10 for 3234 data and 165 / 165 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0219 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07688 0.00230 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O101 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C101 Least-squares cycle 11 Maximum vector length = 511 Memory required = 2853 / 205650 wR2 = 0.1332 before cycle 11 for 3234 data and 165 / 165 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0219 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07688 0.00230 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C5 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C5 Least-squares cycle 12 Maximum vector length = 511 Memory required = 2853 / 205650 wR2 = 0.1332 before cycle 12 for 3234 data and 165 / 165 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0219 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07688 0.00230 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O101 Max. shift = 0.000 A for O2 Max. dU = 0.000 for N3 Least-squares cycle 13 Maximum vector length = 511 Memory required = 2853 / 205650 wR2 = 0.1332 before cycle 13 for 3234 data and 165 / 165 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0219 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07688 0.00230 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O101 Max. shift = 0.000 A for C7 Max. dU = 0.000 for O2 Least-squares cycle 14 Maximum vector length = 511 Memory required = 2853 / 205650 wR2 = 0.1332 before cycle 14 for 3234 data and 165 / 165 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0219 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07688 0.00230 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O101 Max. shift = 0.000 A for O2 Max. dU = 0.000 for C1 Least-squares cycle 15 Maximum vector length = 511 Memory required = 2853 / 205650 wR2 = 0.1332 before cycle 15 for 3234 data and 165 / 165 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0219 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07688 0.00230 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O101 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C2 Least-squares cycle 16 Maximum vector length = 511 Memory required = 2853 / 205650 wR2 = 0.1332 before cycle 16 for 3234 data and 165 / 165 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0219 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07688 0.00230 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O101 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C2 Least-squares cycle 17 Maximum vector length = 511 Memory required = 2853 / 205650 wR2 = 0.1332 before cycle 17 for 3234 data and 165 / 165 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0219 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07688 0.00230 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O101 Max. shift = 0.000 A for C7 Max. dU = 0.000 for N2 Least-squares cycle 18 Maximum vector length = 511 Memory required = 2853 / 205650 wR2 = 0.1332 before cycle 18 for 3234 data and 165 / 165 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0219 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07688 0.00230 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O101 Max. shift = 0.000 A for O2 Max. dU = 0.000 for N3 Least-squares cycle 19 Maximum vector length = 511 Memory required = 2853 / 205650 wR2 = 0.1332 before cycle 19 for 3234 data and 165 / 165 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0219 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07688 0.00230 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C7 Max. dU = 0.000 for C4 Least-squares cycle 20 Maximum vector length = 511 Memory required = 2853 / 205650 wR2 = 0.1332 before cycle 20 for 3234 data and 165 / 165 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0219 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07688 0.00230 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C5 Max. shift = 0.000 A for O2 Max. dU = 0.000 for N3 Largest correlation matrix elements -0.530 U23 C1 / U22 C1 -0.514 U23 C1 / U33 C1 -0.506 U23 C9 / U22 C9 -0.518 U23 O1 / U22 O1 -0.512 U23 N3 / U22 N3 -0.501 U23 N1 / U22 N1 -0.514 U23 N3 / U33 N3 -0.506 U23 O1 / U33 O1 -0.500 U23 C9 / U33 C9 Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.7783 1.0457 0.6158 23 0.990 0.000 C1 N1 C4_$5 H1B 0.7065 1.2399 0.5632 23 0.990 0.000 C1 N1 C4_$5 H2A 0.6064 0.8966 0.8102 23 0.990 0.000 C2 N1 C3 H2B 0.5912 0.9096 0.6456 23 0.990 0.000 C2 N1 C3 H3A 0.3772 0.8400 0.8267 23 0.990 0.000 C3 N2 C2 H3B 0.3068 1.0304 0.7959 23 0.990 0.000 C3 N2 C2 H4A 0.2497 0.7788 0.6558 23 0.990 0.000 C4 N2 C1_$5 H4B 0.4359 0.7622 0.6331 23 0.990 0.000 C4 N2 C1_$5 H5A 0.6370 1.1404 0.8210 23 0.990 0.000 C5 N1 C6 H5B 0.4560 1.1386 0.8541 23 0.990 0.000 C5 N1 C6 H6A 0.5249 1.4183 0.6306 23 0.990 0.000 C6 C7 C5 H6B 0.3492 1.4135 0.6923 23 0.990 0.000 C6 C7 C5 H8A 0.0737 1.0029 0.7186 23 0.990 0.000 C8 N2 C9 H8B 0.0616 1.0609 0.5419 23 0.990 0.000 C8 N2 C9 H9A -0.0519 1.2844 0.6191 23 0.990 0.000 C9 C10 C8 H9B 0.1241 1.2482 0.6747 23 0.990 0.000 C9 C10 C8 H3C 0.3756 1.4514 1.0143 93 0.880 0.000 N3 C7 O1 H3D 0.2841 1.4004 0.9350 93 0.880 0.000 N3 C7 O1 H4C 0.2716 1.4324 0.3387 93 0.880 0.000 N4 C10 O2 H4D 0.3118 1.3233 0.5033 93 0.880 0.000 N4 C10 O2 H11A 1.0792 0.7350 1.0372 137 0.980 0.000 C101 O101 H11A H11B 0.9261 0.8638 0.9315 137 0.980 0.000 C101 O101 H11A H11C 1.0199 0.6919 0.9192 137 0.980 0.000 C101 O101 H11A H101 0.9381 0.5890 1.1614 147 0.840 0.000 O101 C101 H101 2007src0769 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.68521 1.14479 0.56525 1.00000 0.01709 0.02342 0.03243 -0.01586 0.00225 -0.00821 0.02244 0.00276 0.00024 0.00026 0.00024 0.00000 0.00098 0.00103 0.00115 0.00091 0.00082 0.00082 0.00044 H1A 0.77832 1.04571 0.61582 1.00000 0.02693 0.00000 0.00000 H1B 0.70646 1.23993 0.56322 1.00000 0.02693 0.00000 0.00000 C2 0.54026 0.96006 0.71741 1.00000 0.02087 0.01856 0.02751 -0.00967 -0.00205 -0.00578 0.02219 0.00285 0.00025 0.00024 0.00024 0.00000 0.00101 0.00099 0.00107 0.00085 0.00081 0.00081 0.00043 H2A 0.60638 0.89663 0.81018 1.00000 0.02662 0.00000 0.00000 H2B 0.59125 0.90958 0.64560 1.00000 0.02662 0.00000 0.00000 C3 0.37059 0.95086 0.75228 1.00000 0.02108 0.02316 0.02213 -0.00894 -0.00068 -0.00756 0.02208 0.00282 0.00025 0.00026 0.00023 0.00000 0.00102 0.00102 0.00101 0.00084 0.00079 0.00083 0.00043 H3A 0.37721 0.83998 0.82668 1.00000 0.02649 0.00000 0.00000 H3B 0.30680 1.03041 0.79593 1.00000 0.02649 0.00000 0.00000 C4 0.32532 0.83487 0.59440 1.00000 0.01944 0.01897 0.02747 -0.00965 0.00389 -0.00832 0.02172 0.00285 0.00025 0.00025 0.00023 0.00000 0.00099 0.00098 0.00107 0.00084 0.00080 0.00080 0.00043 H4A 0.24967 0.77882 0.65581 1.00000 0.02606 0.00000 0.00000 H4B 0.43586 0.76219 0.63307 1.00000 0.02606 0.00000 0.00000 C5 0.52841 1.18415 0.77569 1.00000 0.02300 0.02348 0.02149 -0.01061 -0.00240 -0.00748 0.02190 0.00275 0.00025 0.00025 0.00023 0.00000 0.00104 0.00104 0.00101 0.00085 0.00079 0.00084 0.00043 H5A 0.63701 1.14042 0.82100 1.00000 0.02629 0.00000 0.00000 H5B 0.45600 1.13855 0.85407 1.00000 0.02629 0.00000 0.00000 C6 0.46470 1.37084 0.72047 1.00000 0.02723 0.02214 0.02108 -0.01026 -0.00200 -0.00702 0.02307 0.00283 0.00026 0.00025 0.00023 0.00000 0.00110 0.00103 0.00101 0.00085 0.00082 0.00086 0.00044 H6A 0.52495 1.41829 0.63065 1.00000 0.02769 0.00000 0.00000 H6B 0.34916 1.41355 0.69228 1.00000 0.02769 0.00000 0.00000 C7 0.48352 1.42198 0.84047 1.00000 0.02538 0.01536 0.01922 -0.00517 -0.00193 -0.00561 0.02080 0.00281 0.00025 0.00024 0.00022 0.00000 0.00107 0.00092 0.00098 0.00078 0.00079 0.00082 0.00043 C8 0.11382 1.06517 0.62121 1.00000 0.01864 0.02076 0.02819 -0.01111 0.00316 -0.00859 0.02182 0.00286 0.00024 0.00024 0.00024 0.00000 0.00099 0.00100 0.00109 0.00087 0.00081 0.00082 0.00043 H8A 0.07368 1.00288 0.71861 1.00000 0.02618 0.00000 0.00000 H8B 0.06160 1.06093 0.54193 1.00000 0.02618 0.00000 0.00000 C9 0.06530 1.24249 0.60064 1.00000 0.02011 0.02259 0.02839 -0.01282 0.00203 -0.00613 0.02331 0.00295 0.00025 0.00025 0.00024 0.00000 0.00102 0.00104 0.00111 0.00089 0.00083 0.00084 0.00044 H9A -0.05187 1.28437 0.61915 1.00000 0.02798 0.00000 0.00000 H9B 0.12410 1.24817 0.67468 1.00000 0.02798 0.00000 0.00000 C10 0.10228 1.34918 0.44518 1.00000 0.01937 0.01768 0.02817 -0.01022 -0.00173 -0.00264 0.02228 0.00287 0.00025 0.00024 0.00024 0.00000 0.00101 0.00098 0.00110 0.00085 0.00082 0.00080 0.00044 N1 0.53870 1.13041 0.65392 1.00000 0.01783 0.01952 0.02315 -0.01117 0.00101 -0.00638 0.01930 0.00226 0.00020 0.00020 0.00019 0.00000 0.00083 0.00084 0.00087 0.00071 0.00065 0.00068 0.00036 N2 0.28892 0.98715 0.61580 1.00000 0.01835 0.01791 0.02245 -0.00888 -0.00029 -0.00594 0.01930 0.00227 0.00020 0.00020 0.00019 0.00000 0.00083 0.00083 0.00087 0.00070 0.00066 0.00067 0.00036 N3 0.36825 1.42489 0.94112 1.00000 0.02526 0.03205 0.02118 -0.01381 0.00274 -0.01430 0.02391 0.00244 0.00021 0.00022 0.00019 0.00000 0.00094 0.00099 0.00089 0.00078 0.00070 0.00079 0.00039 H3C 0.37560 1.45136 1.01430 1.00000 0.02869 0.00000 0.00000 H3D 0.28412 1.40036 0.93498 1.00000 0.02869 0.00000 0.00000 N4 0.24464 1.37076 0.42701 1.00000 0.02380 0.02573 0.02231 -0.00739 0.00008 -0.00882 0.02464 0.00248 0.00021 0.00022 0.00020 0.00000 0.00092 0.00094 0.00090 0.00075 0.00071 0.00076 0.00040 H4C 0.27156 1.43244 0.33873 1.00000 0.02957 0.00000 0.00000 H4D 0.31178 1.32334 0.50328 1.00000 0.02957 0.00000 0.00000 O1 0.60507 1.45551 0.84362 1.00000 0.02767 0.03366 0.02530 -0.01520 0.00421 -0.01570 0.02648 0.00200 0.00018 0.00019 0.00016 0.00000 0.00082 0.00086 0.00079 0.00068 0.00062 0.00069 0.00035 O2 0.00220 1.41186 0.34329 1.00000 0.03201 0.03590 0.03379 -0.00424 -0.00985 -0.01236 0.03605 0.00230 0.00020 0.00021 0.00019 0.00000 0.00092 0.00093 0.00092 0.00075 0.00072 0.00076 0.00042 C101 0.98461 0.74728 0.98770 1.00000 0.03414 0.05712 0.04813 -0.00175 0.00453 -0.01964 0.05278 0.00470 0.00034 0.00039 0.00034 0.00000 0.00148 0.00185 0.00169 0.00142 0.00122 0.00136 0.00080 H11A 1.07919 0.73496 1.03719 1.00000 0.07918 0.00000 0.00000 H11B 0.92611 0.86379 0.93149 1.00000 0.07918 0.00000 0.00000 H11C 1.01991 0.69190 0.91916 1.00000 0.07918 0.00000 0.00000 O101 0.88225 0.67728 1.09562 1.00000 0.03009 0.04234 0.03050 -0.00519 -0.00518 -0.01689 0.03573 0.00233 0.00020 0.00022 0.00018 0.00000 0.00089 0.00102 0.00090 0.00075 0.00069 0.00078 0.00042 H101 0.93811 0.58904 1.16136 1.00000 0.05359 0.00000 0.00000 Final Structure Factor Calculation for 2007src0769 in P-1 Total number of l.s. parameters = 165 Maximum vector length = 511 Memory required = 2688 / 22995 wR2 = 0.1332 before cycle 21 for 3234 data and 0 / 165 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0219 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0618 for 2474 Fo > 4sig(Fo) and 0.0870 for all 3234 data wR2 = 0.1332, GooF = S = 1.076, Restrained GooF = 1.076 for all data Occupancy sum of asymmetric unit = 18.00 for non-hydrogen and 24.00 for hydrogen atoms Principal mean square atomic displacements U 0.0332 0.0186 0.0156 C1 0.0283 0.0204 0.0179 C2 0.0233 0.0227 0.0202 C3 0.0295 0.0191 0.0165 C4 0.0257 0.0231 0.0170 C5 0.0288 0.0224 0.0180 C6 0.0265 0.0208 0.0152 C7 0.0291 0.0198 0.0166 C8 0.0288 0.0226 0.0185 C9 0.0286 0.0229 0.0153 C10 0.0238 0.0178 0.0164 N1 0.0225 0.0183 0.0171 N2 0.0333 0.0210 0.0174 N3 0.0285 0.0236 0.0218 N4 0.0358 0.0224 0.0213 O1 0.0523 0.0331 0.0228 O2 0.0889 0.0420 0.0274 C101 0.0542 0.0290 0.0239 O101 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.018 0.027 0.037 0.048 0.061 0.080 0.105 0.153 1.000 Number in group 340. 337. 311. 331. 320. 303. 327. 318. 322. 325. GooF 1.199 1.096 1.090 1.148 1.131 0.996 0.985 0.999 0.964 1.112 K 4.765 1.459 1.058 1.082 1.015 1.014 0.995 1.005 1.008 0.999 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.65 inf Number in group 332. 317. 325. 322. 321. 325. 320. 323. 323. 326. GooF 1.137 1.135 1.015 1.166 1.022 1.015 1.013 0.883 0.996 1.314 K 1.080 1.059 1.061 1.035 1.024 0.994 0.990 0.986 1.011 1.000 R1 0.185 0.199 0.169 0.146 0.111 0.080 0.066 0.048 0.046 0.037 Recommended weighting scheme: WGHT 0.0219 0.8258 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) 8 0 5 10.84 0.31 3.63 0.006 0.89 0 3 4 118.98 82.16 3.61 0.096 2.22 4 4 12 17.68 42.60 3.38 0.069 0.79 -1 1 0 26.12 11.29 3.38 0.036 5.02 5 6 12 33.07 9.85 3.35 0.033 0.78 5 8 11 186.67 126.28 3.34 0.119 0.82 -4 7 9 29.22 9.77 3.28 0.033 0.80 11 5 2 12.31 0.01 3.15 0.001 0.81 -1 5 9 0.03 8.73 3.11 0.031 1.02 0 11 4 19.88 4.27 3.06 0.022 0.81 0 9 7 11.10 0.02 3.05 0.002 0.94 -2 -3 2 130.56 97.78 3.02 0.105 2.01 -9 -3 4 17.32 2.88 3.00 0.018 0.86 -7 -8 1 14.22 0.29 2.97 0.006 0.91 -3 0 11 31.40 12.23 2.92 0.037 0.78 -1 2 4 21.80 10.32 2.92 0.034 2.21 0 -3 3 8.21 1.88 2.88 0.014 1.70 -2 10 4 16.22 1.23 2.87 0.012 0.81 -6 -6 6 -5.51 13.72 2.84 0.039 0.81 -3 7 9 34.66 13.74 2.83 0.039 0.85 11 4 5 4.81 17.00 2.80 0.044 0.77 -1 0 1 608.33 701.34 2.77 0.280 6.11 8 -2 1 9.51 25.77 2.74 0.054 0.92 0 2 12 36.66 17.76 2.74 0.045 0.79 9 6 2 19.94 36.71 2.73 0.064 0.95 -2 3 9 36.79 57.27 2.72 0.080 1.02 3 -1 3 377.79 320.49 2.71 0.189 1.76 -3 -3 5 24.07 12.97 2.70 0.038 1.24 -3 1 0 235.14 193.79 2.70 0.147 2.38 -3 -2 2 342.61 290.67 2.69 0.180 2.12 -2 -6 6 -3.93 4.72 2.68 0.023 0.87 4 11 5 7.19 0.18 2.68 0.004 0.87 -9 0 5 36.50 20.50 2.68 0.048 0.82 -6 0 2 -0.97 5.63 2.68 0.025 1.32 0 3 3 478.18 402.98 2.66 0.212 2.60 -3 2 1 4.79 0.16 2.65 0.004 2.03 1 7 3 148.99 117.14 2.65 0.114 1.34 6 7 5 5.31 15.50 2.64 0.042 1.14 -4 3 7 16.34 6.75 2.62 0.027 1.08 8 7 4 10.28 2.84 2.62 0.018 1.00 0 -1 2 1318.49 1454.99 2.59 0.403 3.39 4 0 2 490.68 425.67 2.58 0.218 1.87 -2 3 4 283.22 335.34 2.57 0.194 1.77 -6 4 1 4.60 15.30 2.54 0.041 1.01 1 9 5 5.88 0.04 2.54 0.002 1.02 2 7 10 10.57 21.50 2.53 0.049 0.94 -6 1 6 5.55 0.12 2.50 0.004 1.01 -3 -5 2 6.19 0.02 2.50 0.001 1.40 -3 7 1 23.80 11.48 2.47 0.036 0.99 9 8 4 7.28 0.09 2.46 0.003 0.89 Bond lengths and angles C1 - Distance Angles N1 1.4767 (0.0025) C4_$5 1.5192 (0.0029) 114.28 (0.16) H1A 0.9900 108.69 108.69 H1B 0.9900 108.69 108.69 107.61 C1 - N1 C4_$5 H1A C2 - Distance Angles N1 1.4774 (0.0026) C3 1.5247 (0.0028) 112.04 (0.16) H2A 0.9900 109.20 109.20 H2B 0.9900 109.20 109.20 107.90 C2 - N1 C3 H2A C3 - Distance Angles N2 1.4746 (0.0026) C2 1.5247 (0.0028) 110.72 (0.17) H3A 0.9900 109.50 109.50 H3B 0.9900 109.50 109.50 108.07 C3 - N2 C2 H3A C4 - Distance Angles N2 1.4764 (0.0026) C1_$5 1.5192 (0.0029) 115.92 (0.17) H4A 0.9900 108.30 108.30 H4B 0.9900 108.30 108.30 107.41 C4 - N2 C1_$5 H4A C5 - Distance Angles N1 1.4777 (0.0025) C6 1.5312 (0.0028) 112.14 (0.16) H5A 0.9900 109.18 109.18 H5B 0.9900 109.18 109.18 107.89 C5 - N1 C6 H5A C6 - Distance Angles C7 1.5131 (0.0028) C5 1.5312 (0.0028) 110.72 (0.17) H6A 0.9900 109.50 109.50 H6B 0.9900 109.50 109.50 108.07 C6 - C7 C5 H6A C7 - Distance Angles O1 1.2443 (0.0025) N3 1.3212 (0.0026) 122.76 (0.19) C6 1.5131 (0.0028) 120.26 (0.18) 116.96 (0.18) C7 - O1 N3 C8 - Distance Angles N2 1.4637 (0.0025) C9 1.5218 (0.0028) 112.70 (0.16) H8A 0.9900 109.05 109.05 H8B 0.9900 109.05 109.05 107.81 C8 - N2 C9 H8A C9 - Distance Angles C10 1.5113 (0.0029) C8 1.5218 (0.0028) 111.61 (0.17) H9A 0.9900 109.30 109.30 H9B 0.9900 109.30 109.30 107.96 C9 - C10 C8 H9A C10 - Distance Angles O2 1.2354 (0.0026) N4 1.3318 (0.0027) 123.51 (0.20) C9 1.5113 (0.0029) 119.97 (0.19) 116.52 (0.18) C10 - O2 N4 N1 - Distance Angles C1 1.4767 (0.0025) C2 1.4774 (0.0026) 110.88 (0.16) C5 1.4777 (0.0025) 109.83 (0.15) 109.65 (0.16) N1 - C1 C2 N2 - Distance Angles C8 1.4637 (0.0025) C3 1.4746 (0.0026) 111.87 (0.16) C4 1.4764 (0.0026) 109.84 (0.15) 109.77 (0.16) N2 - C8 C3 N3 - Distance Angles C7 1.3212 (0.0026) H3C 0.8800 120.00 H3D 0.8800 120.00 120.00 N3 - C7 H3C N4 - Distance Angles C10 1.3318 (0.0027) H4C 0.8800 120.00 H4D 0.8800 120.00 120.00 N4 - C10 H4C O1 - Distance Angles C7 1.2443 (0.0025) O1 - O2 - Distance Angles C10 1.2354 (0.0026) O2 - C101 - Distance Angles O101 1.4056 (0.0030) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C101 - O101 H11A H11B O101 - Distance Angles C101 1.4056 (0.0030) H101 0.8400 109.47 O101 - C101 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.01 2.885(2) 171.1 N3-H3C...O1_$1 0.88 1.99 2.865(2) 170.7 N3-H3D...O101_$2 0.88 2.06 2.921(2) 164.9 N4-H4C...O1_$3 0.88 2.35 3.178(2) 157.0 N4-H4D...N1 0.84 1.86 2.666(2) 161.2 O101-H101...O2_$4 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)