+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0683a started at 23:42:06 on 02-Aug-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0683a in P2(1)2(1)2(1) CELL 0.71073 4.7550 12.4624 24.7840 90.000 90.000 90.000 ZERR 4.00 0.0001 0.0003 0.0007 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 N O UNIT 56 68 4 32 V = 1468.67 F(000) = 688.0 Mu = 0.12 mm-1 Cell Wt = 1309.14 Rho = 1.480 MERG 4 OMIT -3.00 55.00 SHEL 7 0.77 DFIX 1.01 0.02 N1 H1N FMAP 2 PLAN 20 SIZE 0.01 0.07 0.20 ACTA HTAB O2 O6_$1 HTAB O3 O6_$2 HTAB O4 O5_$3 HTAB O5 O4_$4 HTAB O8 O3_$1 HTAB N1 O7_$2] EQIV $1 -x+1, y+1/2, -z+3/2 EQIV $2 x-1, y, z EQIV $3 x-1/2, -y+3/2, -z+2 EQIV $4 x+1, y, z BOND $H WGHT 0.00530 1.78750 L.S. 10 TEMP -153.00 FVAR 0.80985 MOLE 1 C1 1 0.403330 0.938056 0.824168 11.00000 0.01820 0.01678 = 0.01386 0.00134 0.00237 0.00139 AFIX 13 H1 2 0.579643 0.959461 0.804988 11.00000 -1.20000 AFIX 0 C2 1 0.329309 0.821989 0.809544 11.00000 0.01708 0.01467 = 0.01003 -0.00009 0.00014 0.00118 AFIX 13 H2 2 0.489268 0.774673 0.820503 11.00000 -1.20000 AFIX 0 C3 1 0.067210 0.786717 0.840017 11.00000 0.01385 0.01144 = 0.01525 -0.00077 -0.00093 0.00012 AFIX 13 H3 2 -0.093213 0.834696 0.830085 11.00000 -1.20000 AFIX 0 C4 1 0.126064 0.797255 0.900093 11.00000 0.01438 0.01685 = 0.01490 0.00057 0.00171 0.00025 AFIX 13 H4 2 0.285042 0.748961 0.910483 11.00000 -1.20000 AFIX 0 C5 1 0.204253 0.914440 0.912116 11.00000 0.02044 0.01411 = 0.01588 0.00138 0.00136 0.00159 AFIX 13 H5 2 0.042062 0.961222 0.901803 11.00000 -1.20000 AFIX 0 C6 1 0.278506 0.936509 0.970595 11.00000 0.02408 0.01950 = 0.01596 -0.00332 -0.00228 0.00121 AFIX 23 H6A 2 0.337070 1.012423 0.974096 11.00000 -1.20000 H6B 2 0.108260 0.926294 0.993008 11.00000 -1.20000 AFIX 0 C7 1 0.461456 0.754632 0.719960 11.00000 0.01781 0.01243 = 0.01451 0.00022 0.00008 -0.00455 C8 1 0.405446 0.766851 0.660275 11.00000 0.01648 0.01477 = 0.01403 -0.00007 -0.00013 0.00230 C9 1 0.235444 0.690186 0.635615 11.00000 0.02048 0.01581 = 0.02204 0.00119 -0.00197 -0.00427 AFIX 43 H9 2 0.167121 0.630795 0.655754 11.00000 -1.20000 AFIX 0 C10 1 0.166267 0.700981 0.581429 11.00000 0.02909 0.02235 = 0.02201 -0.00346 -0.00489 -0.00872 AFIX 43 H10 2 0.050143 0.648802 0.564561 11.00000 -1.20000 AFIX 0 C11 1 0.265260 0.787119 0.551904 11.00000 0.03244 0.02313 = 0.01600 0.00176 -0.00328 -0.00361 AFIX 43 H11 2 0.215499 0.794363 0.514960 11.00000 -1.20000 AFIX 0 C12 1 0.436982 0.862929 0.576111 11.00000 0.02753 0.02131 = 0.02068 0.00503 -0.00395 -0.00508 AFIX 43 H12 2 0.506962 0.921578 0.555634 11.00000 -1.20000 AFIX 0 C13 1 0.507254 0.853170 0.630598 11.00000 0.01782 0.01168 = 0.01991 0.00078 -0.00047 0.00213 C14 1 0.697747 0.934231 0.656139 11.00000 0.02278 0.01474 = 0.02196 0.00155 -0.00367 0.00132 N1 3 0.293647 0.814085 0.751194 11.00000 0.01648 0.01716 = 0.01223 -0.00024 -0.00099 0.00205 O1 4 0.445727 0.946064 0.880882 11.00000 0.01860 0.01574 = 0.01486 0.00072 -0.00032 -0.00158 O2 4 0.180386 1.003104 0.806633 11.00000 0.01800 0.01176 = 0.02254 0.00325 -0.00061 0.00271 AFIX 147 H2A 2 0.242057 1.064214 0.798605 11.00000 -1.50000 AFIX 0 O3 4 -0.004924 0.678226 0.827599 11.00000 0.02297 0.01315 = 0.02043 0.00099 -0.00762 -0.00153 AFIX 147 H3A 2 -0.103752 0.676768 0.799516 11.00000 -1.50000 AFIX 0 O4 4 -0.119698 0.769494 0.930032 11.00000 0.01818 0.02280 = 0.01986 0.00573 0.00257 0.00043 AFIX 147 H4A 2 -0.077719 0.724270 0.953838 11.00000 -1.50000 AFIX 0 O5 4 0.496917 0.869725 0.990959 11.00000 0.02421 0.02857 = 0.01579 0.00205 -0.00057 0.00558 AFIX 147 H5A 2 0.605348 0.852413 0.965658 11.00000 -1.50000 AFIX 0 O6 4 0.641096 0.690789 0.737191 11.00000 0.02240 0.01542 = 0.01700 -0.00065 -0.00409 0.00651 O7 4 0.810479 0.921387 0.699378 11.00000 0.02376 0.01966 = 0.02424 0.00195 -0.00701 -0.00140 O8 4 0.729687 1.021345 0.626424 11.00000 0.07012 0.02395 = 0.03661 0.01385 -0.02876 -0.02558 AFIX 147 H8 2 0.826826 1.066395 0.643401 11.00000 -1.50000 AFIX 0 H1N 2 0.147095 0.860548 0.735662 11.00000 -1.20000 HKLF 4 Covalent radii and connectivity table for 2009src0683a in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - O2 O1 C2 C2 - N1 C3 C1 C3 - O3 C4 C2 C4 - O4 C3 C5 C5 - O1 C6 C4 C6 - O5 C5 C7 - O6 N1 C8 C8 - C13 C9 C7 C9 - C10 C8 C10 - C11 C9 C11 - C10 C12 C12 - C11 C13 C13 - C8 C12 C14 C14 - O7 O8 C13 N1 - C7 C2 O1 - C1 C5 O2 - C1 O3 - C3 O4 - C4 O5 - C6 O6 - C7 O7 - C14 O8 - C14 Operators for generating equivalent atoms: $1 -x+1, y+1/2, -z+3/2 $2 x-1, y, z $3 x-1/2, -y+3/2, -z+2 $4 x+1, y, z 17754 Reflections read, of which 111 rejected -6 =< h =< 5, -16 =< k =< 16, -32 =< l =< 32, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 1992 Unique reflections, of which 0 suppressed R(int) = 0.0617 R(sigma) = 0.0397 Friedel opposites merged Maximum memory for data reduction = 2361 / 19752 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 = 2955 / 267615 wR2 = 0.0923 before cycle 1 for 1992 data and 216 / 216 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.026 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.099; Restrained GooF = 1.099 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0053 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.80985 0.00149 0.000 OSF Mean shift/su = 0.025 Maximum = -0.097 for z N1 Max. shift = 0.002 A for H1N Max. dU = 0.000 for O3 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2955 / 267615 wR2 = 0.0923 before cycle 2 for 1992 data and 216 / 216 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.025 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.099; Restrained GooF = 1.099 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0053 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.80979 0.00149 -0.041 OSF Mean shift/su = 0.009 Maximum = -0.041 for OSF Max. shift = 0.001 A for H8 Max. dU = 0.000 for O3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2955 / 267615 wR2 = 0.0923 before cycle 3 for 1992 data and 216 / 216 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.025 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.099; Restrained GooF = 1.099 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0053 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.80979 0.00149 -0.003 OSF Mean shift/su = 0.001 Maximum = -0.003 for tors H3A Max. shift = 0.000 A for H3A Max. dU = 0.000 for C10 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2955 / 267615 wR2 = 0.0923 before cycle 4 for 1992 data and 216 / 216 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.025 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.099; Restrained GooF = 1.099 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0053 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.80978 0.00149 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for U23 O2 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C10 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2955 / 267615 wR2 = 0.0923 before cycle 5 for 1992 data and 216 / 216 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.025 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.099; Restrained GooF = 1.099 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0053 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.80978 0.00149 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H8 Max. dU = 0.000 for O8 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2955 / 267615 wR2 = 0.0923 before cycle 6 for 1992 data and 216 / 216 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.025 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.099; Restrained GooF = 1.099 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0053 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.80978 0.00149 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z O2 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C4 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2955 / 267615 wR2 = 0.0923 before cycle 7 for 1992 data and 216 / 216 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.025 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.099; Restrained GooF = 1.099 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0053 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.80978 0.00149 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z O4 Max. shift = 0.000 A for H2A Max. dU = 0.000 for C6 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2955 / 267615 wR2 = 0.0923 before cycle 8 for 1992 data and 216 / 216 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.025 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.099; Restrained GooF = 1.099 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0053 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.80978 0.00149 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z O2 Max. shift = 0.000 A for H3A Max. dU = 0.000 for N1 Least-squares cycle 9 Maximum vector length = 511 Memory required = 2955 / 267615 wR2 = 0.0923 before cycle 9 for 1992 data and 216 / 216 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.025 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.099; Restrained GooF = 1.099 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0053 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.80978 0.00149 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z O2 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C12 Least-squares cycle 10 Maximum vector length = 511 Memory required = 2955 / 267615 wR2 = 0.0923 before cycle 10 for 1992 data and 216 / 216 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.025 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.099; Restrained GooF = 1.099 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0053 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.80978 0.00149 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z O2 Max. shift = 0.000 A for H1N Max. dU = 0.000 for O6 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 0.5797 0.9595 0.8050 13 1.000 0.000 C1 O2 O1 C2 H2 0.4893 0.7747 0.8205 13 1.000 0.000 C2 N1 C3 C1 H3 -0.0932 0.8347 0.8301 13 1.000 0.000 C3 O3 C4 C2 H4 0.2851 0.7489 0.9105 13 1.000 0.000 C4 O4 C3 C5 H5 0.0421 0.9612 0.9018 13 1.000 0.000 C5 O1 C6 C4 H6A 0.3371 1.0124 0.9741 23 0.990 0.000 C6 O5 C5 H6B 0.1083 0.9263 0.9930 23 0.990 0.000 C6 O5 C5 H9 0.1671 0.6308 0.6558 43 0.950 0.000 C9 C10 C8 H10 0.0501 0.6488 0.5645 43 0.950 0.000 C10 C11 C9 H11 0.2155 0.7944 0.5150 43 0.950 0.000 C11 C10 C12 H12 0.5070 0.9216 0.5556 43 0.950 0.000 C12 C11 C13 H2A 0.2421 1.0642 0.7986 147 0.840 0.000 O2 C1 H2A H3A -0.1041 0.6768 0.7996 147 0.840 0.000 O3 C3 H3A H4A -0.0778 0.7242 0.9538 147 0.840 0.000 O4 C4 H4A H5A 0.6054 0.8525 0.9657 147 0.840 0.000 O5 C6 H5A H8 0.8272 1.0663 0.6434 147 0.840 0.000 O8 C14 H8 2009src0683a in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.40335 0.93807 0.82416 1.00000 0.01813 0.01673 0.01385 0.00132 0.00239 0.00135 0.01624 0.00542 0.00074 0.00023 0.00011 0.00000 0.00168 0.00144 0.00135 0.00116 0.00134 0.00136 0.00066 H1 0.57966 0.95948 0.80498 1.00000 0.01948 0.00000 0.00000 C2 0.32935 0.82198 0.80955 1.00000 0.01710 0.01467 0.00990 -0.00009 0.00019 0.00117 0.01389 0.00505 0.00070 0.00022 0.00011 0.00000 0.00167 0.00136 0.00123 0.00106 0.00132 0.00132 0.00062 H2 0.48929 0.77466 0.82051 1.00000 0.01666 0.00000 0.00000 C3 0.06717 0.78673 0.84001 1.00000 0.01384 0.01153 0.01510 -0.00078 -0.00097 0.00009 0.01349 0.00496 0.00067 0.00023 0.00011 0.00000 0.00157 0.00131 0.00132 0.00105 0.00127 0.00124 0.00062 H3 -0.09323 0.83472 0.83008 1.00000 0.01619 0.00000 0.00000 C4 0.12611 0.79724 0.90010 1.00000 0.01443 0.01678 0.01481 0.00051 0.00166 0.00023 0.01534 0.00526 0.00070 0.00023 0.00011 0.00000 0.00162 0.00145 0.00133 0.00116 0.00130 0.00137 0.00064 H4 0.28509 0.74895 0.91049 1.00000 0.01841 0.00000 0.00000 C5 0.20426 0.91445 0.91212 1.00000 0.02046 0.01405 0.01577 0.00133 0.00145 0.00161 0.01676 0.00539 0.00074 0.00023 0.00011 0.00000 0.00173 0.00138 0.00139 0.00110 0.00146 0.00136 0.00066 H5 0.04205 0.96123 0.90181 1.00000 0.02011 0.00000 0.00000 C6 0.27854 0.93650 0.97060 1.00000 0.02406 0.01951 0.01586 -0.00337 -0.00235 0.00120 0.01981 0.00550 0.00079 0.00024 0.00011 0.00000 0.00186 0.00150 0.00138 0.00120 0.00147 0.00147 0.00070 H6A 0.33711 1.01241 0.97411 1.00000 0.02377 0.00000 0.00000 H6B 0.10830 0.92628 0.99302 1.00000 0.02377 0.00000 0.00000 C7 0.46147 0.75463 0.71997 1.00000 0.01780 0.01246 0.01440 0.00023 0.00009 -0.00454 0.01489 0.00505 0.00071 0.00023 0.00011 0.00000 0.00167 0.00134 0.00132 0.00111 0.00139 0.00127 0.00064 C8 0.40545 0.76684 0.66027 1.00000 0.01649 0.01485 0.01400 -0.00003 -0.00023 0.00229 0.01511 0.00519 0.00070 0.00023 0.00011 0.00000 0.00164 0.00141 0.00132 0.00109 0.00134 0.00129 0.00065 C9 0.23543 0.69017 0.63562 1.00000 0.02040 0.01578 0.02200 0.00116 -0.00205 -0.00432 0.01939 0.00531 0.00072 0.00024 0.00012 0.00000 0.00174 0.00140 0.00149 0.00123 0.00145 0.00137 0.00068 H9 0.16711 0.63078 0.65576 1.00000 0.02327 0.00000 0.00000 C10 0.16622 0.70097 0.58142 1.00000 0.02897 0.02228 0.02205 -0.00343 -0.00487 -0.00874 0.02443 0.00558 0.00079 0.00026 0.00012 0.00000 0.00196 0.00161 0.00151 0.00131 0.00162 0.00162 0.00076 H10 0.05009 0.64880 0.56454 1.00000 0.02932 0.00000 0.00000 C11 0.26525 0.78713 0.55190 1.00000 0.03240 0.02309 0.01603 0.00177 -0.00323 -0.00361 0.02384 0.00581 0.00082 0.00025 0.00012 0.00000 0.00209 0.00157 0.00140 0.00125 0.00152 0.00163 0.00077 H11 0.21547 0.79439 0.51496 1.00000 0.02861 0.00000 0.00000 C12 0.43698 0.86294 0.57610 1.00000 0.02757 0.02129 0.02070 0.00501 -0.00406 -0.00507 0.02319 0.00573 0.00077 0.00026 0.00012 0.00000 0.00206 0.00160 0.00155 0.00131 0.00160 0.00154 0.00077 H12 0.50697 0.92158 0.55562 1.00000 0.02782 0.00000 0.00000 C13 0.50726 0.85317 0.63059 1.00000 0.01785 0.01170 0.01990 0.00081 -0.00047 0.00205 0.01648 0.00551 0.00074 0.00023 0.00012 0.00000 0.00169 0.00133 0.00144 0.00114 0.00146 0.00134 0.00066 C14 0.69778 0.93422 0.65614 1.00000 0.02269 0.01468 0.02196 0.00158 -0.00365 0.00122 0.01978 0.00562 0.00078 0.00024 0.00012 0.00000 0.00185 0.00139 0.00154 0.00118 0.00154 0.00144 0.00070 N1 0.29362 0.81409 0.75118 1.00000 0.01648 0.01718 0.01220 -0.00023 -0.00094 0.00203 0.01529 0.00443 0.00059 0.00019 0.00009 0.00000 0.00140 0.00119 0.00112 0.00094 0.00112 0.00116 0.00054 O1 0.44572 0.94607 0.88088 1.00000 0.01867 0.01567 0.01487 0.00071 -0.00033 -0.00157 0.01640 0.00358 0.00049 0.00016 0.00008 0.00000 0.00131 0.00103 0.00098 0.00080 0.00097 0.00098 0.00050 O2 0.18039 1.00312 0.80663 1.00000 0.01798 0.01171 0.02247 0.00324 -0.00061 0.00274 0.01739 0.00379 0.00048 0.00016 0.00009 0.00000 0.00123 0.00097 0.00108 0.00084 0.00110 0.00099 0.00048 H2A 0.24206 1.06422 0.79859 1.00000 0.02608 0.00000 0.00000 O3 -0.00495 0.67822 0.82760 1.00000 0.02291 0.01305 0.02039 0.00103 -0.00763 -0.00156 0.01878 0.00371 0.00053 0.00016 0.00008 0.00000 0.00128 0.00098 0.00104 0.00083 0.00105 0.00099 0.00049 H3A -0.10411 0.67676 0.79956 1.00000 0.02817 0.00000 0.00000 O4 -0.11974 0.76948 0.93003 1.00000 0.01813 0.02274 0.01986 0.00570 0.00250 0.00040 0.02024 0.00390 0.00049 0.00017 0.00008 0.00000 0.00121 0.00114 0.00109 0.00087 0.00103 0.00102 0.00051 H4A -0.07780 0.72425 0.95384 1.00000 0.03036 0.00000 0.00000 O5 0.49690 0.86972 0.99096 1.00000 0.02418 0.02863 0.01575 0.00203 -0.00054 0.00551 0.02285 0.00415 0.00057 0.00018 0.00008 0.00000 0.00137 0.00122 0.00102 0.00094 0.00109 0.00118 0.00054 H5A 0.60539 0.85245 0.96566 1.00000 0.03428 0.00000 0.00000 O6 0.64110 0.69080 0.73719 1.00000 0.02230 0.01537 0.01700 -0.00064 -0.00403 0.00649 0.01822 0.00365 0.00050 0.00016 0.00008 0.00000 0.00126 0.00099 0.00097 0.00084 0.00098 0.00097 0.00048 O7 0.81048 0.92139 0.69938 1.00000 0.02369 0.01959 0.02434 0.00195 -0.00697 -0.00140 0.02254 0.00389 0.00054 0.00017 0.00009 0.00000 0.00135 0.00112 0.00115 0.00090 0.00114 0.00109 0.00054 O8 0.72970 1.02134 0.62642 1.00000 0.07013 0.02392 0.03663 0.01381 -0.02890 -0.02560 0.04356 0.00447 0.00076 0.00019 0.00010 0.00000 0.00227 0.00129 0.00143 0.00106 0.00166 0.00150 0.00084 H8 0.82720 1.06633 0.64336 1.00000 0.06534 0.00000 0.00000 H1N 0.14688 0.86066 0.73569 1.00000 0.05227 0.06767 0.00685 0.00277 0.00147 0.00000 0.00000 Final Structure Factor Calculation for 2009src0683a in P2(1)2(1)2(1) Total number of l.s. parameters = 216 Maximum vector length = 511 Memory required = 2741 / 25046 wR2 = 0.0923 before cycle 11 for 1992 data and 2 / 216 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.025 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.099; Restrained GooF = 1.099 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0053 * P )^2 + 1.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0492 for 1738 Fo > 4sig(Fo) and 0.0618 for all 1992 data wR2 = 0.0923, GooF = S = 1.099, Restrained GooF = 1.099 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 23.00 for non-hydrogen and 17.00 for hydrogen atoms Principal mean square atomic displacements U 0.0201 0.0159 0.0127 C1 0.0176 0.0142 0.0099 C2 0.0157 0.0134 0.0114 C3 0.0171 0.0160 0.0129 C4 0.0214 0.0157 0.0132 C5 0.0255 0.0203 0.0137 C6 0.0204 0.0144 0.0099 C7 0.0181 0.0140 0.0132 C8 0.0249 0.0201 0.0132 C9 0.0354 0.0251 0.0128 C10 0.0344 0.0219 0.0153 C11 0.0333 0.0203 0.0159 C12 0.0200 0.0184 0.0110 C13 0.0260 0.0195 0.0139 C14 0.0190 0.0149 0.0120 N1 0.0194 0.0154 0.0144 O1 0.0234 0.0189 0.0098 O2 0.0296 0.0140 0.0128 O3 0.0276 0.0186 0.0145 O4 0.0325 0.0209 0.0152 O5 0.0276 0.0161 0.0110 O6 0.0315 0.0192 0.0170 O7 0.0982 0.0201 0.0125 O8 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.027 0.043 0.057 0.070 0.085 0.102 0.125 0.158 0.225 1.000 Number in group 204. 198. 208. 196. 197. 193. 205. 199. 192. 200. GooF 1.285 1.240 1.155 1.203 1.000 0.999 1.011 0.932 1.042 1.058 K 2.220 1.137 1.059 1.047 1.009 1.001 1.012 0.999 0.993 1.005 Resolution(A) 0.77 0.80 0.83 0.88 0.92 0.98 1.07 1.17 1.37 1.73 inf Number in group 204. 198. 203. 198. 195. 197. 200. 200. 198. 199. GooF 1.281 1.388 1.029 1.118 1.115 1.074 0.868 0.878 0.939 1.185 K 1.140 1.069 1.036 1.027 1.008 0.970 0.990 0.989 1.013 1.005 R1 0.177 0.144 0.111 0.101 0.083 0.058 0.036 0.033 0.031 0.022 Recommended weighting scheme: WGHT 0.0047 1.7930 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) 1 15 1 111.63 44.41 3.93 0.056 0.82 2 14 8 518.17 378.09 3.85 0.163 0.81 0 15 6 52.40 0.99 3.85 0.008 0.81 3 8 21 112.67 55.98 3.58 0.063 0.81 5 7 5 -6.40 19.72 3.52 0.037 0.83 1 0 24 352.81 473.08 3.42 0.182 1.01 4 0 5 43.53 1.87 3.41 0.011 1.16 0 2 30 42.70 7.67 3.27 0.023 0.82 1 0 30 367.43 263.57 3.25 0.136 0.81 4 2 23 52.17 13.00 3.16 0.030 0.79 5 1 15 48.30 9.15 3.10 0.025 0.82 4 2 12 32.32 87.04 3.08 0.078 1.02 0 13 3 -4.55 25.42 3.01 0.042 0.95 2 12 7 92.73 45.21 3.01 0.056 0.92 1 14 14 84.85 38.48 2.99 0.052 0.78 5 8 1 57.47 3.42 2.96 0.015 0.81 1 0 23 37.81 2.11 2.95 0.012 1.05 2 5 27 90.32 22.96 2.95 0.040 0.81 2 3 29 69.85 24.24 2.89 0.041 0.79 6 0 6 88.11 1.50 2.86 0.010 0.78 0 6 7 786.72 672.88 2.85 0.217 1.79 5 1 12 39.53 4.62 2.78 0.018 0.86 5 9 3 136.27 61.09 2.77 0.065 0.78 4 0 11 237.39 155.75 2.74 0.104 1.05 5 1 13 125.67 68.89 2.68 0.069 0.85 1 0 5 43.91 75.76 2.67 0.073 3.43 0 0 6 592.85 712.56 2.66 0.223 4.13 4 6 10 62.40 106.33 2.66 0.086 0.95 4 2 16 17.49 48.65 2.65 0.058 0.93 1 0 6 223.70 169.91 2.64 0.109 3.12 5 7 11 -0.07 26.42 2.63 0.043 0.79 3 11 8 16.13 42.65 2.63 0.055 0.88 0 0 24 381.60 479.73 2.62 0.183 1.03 5 8 3 61.20 16.56 2.58 0.034 0.81 2 9 13 102.36 145.98 2.54 0.101 1.01 5 2 10 589.67 473.71 2.53 0.182 0.88 1 13 8 1.96 24.57 2.53 0.041 0.90 4 9 14 94.33 54.95 2.53 0.062 0.80 4 11 4 139.59 197.72 2.48 0.118 0.81 0 2 25 39.66 11.66 2.44 0.029 0.98 1 4 29 -9.70 11.57 2.41 0.028 0.81 1 0 21 24.22 47.97 2.41 0.058 1.15 2 0 22 55.22 1.46 2.40 0.010 1.02 1 1 4 2969.93 3178.32 2.40 0.471 3.61 0 11 14 19.02 0.06 2.39 0.002 0.95 1 12 9 78.91 45.76 2.39 0.057 0.95 0 6 0 121.40 85.07 2.37 0.077 2.08 4 11 10 105.18 48.02 2.36 0.058 0.78 5 3 15 9.80 39.08 2.36 0.052 0.81 0 5 5 10704.58 10159.43 2.35 0.843 2.23 Bond lengths and angles C1 - Distance Angles O2 1.4035 (0.0037) O1 1.4236 (0.0034) 111.85 (0.25) C2 1.5324 (0.0040) 107.38 (0.26) 109.39 (0.23) H1 1.0000 109.39 109.39 109.39 C1 - O2 O1 C2 C2 - Distance Angles N1 1.4598 (0.0034) C3 1.5221 (0.0042) 112.13 (0.26) C1 1.5324 (0.0040) 108.94 (0.23) 110.08 (0.24) H2 1.0000 108.54 108.54 108.54 C2 - N1 C3 C1 C3 - Distance Angles O3 1.4286 (0.0034) C4 1.5211 (0.0037) 109.66 (0.23) C2 1.5221 (0.0043) 111.28 (0.24) 108.05 (0.25) H3 1.0000 109.27 109.27 109.27 C3 - O3 C4 C2 C4 - Distance Angles O4 1.4271 (0.0038) C3 1.5211 (0.0037) 109.70 (0.26) C5 1.5364 (0.0040) 109.14 (0.24) 108.44 (0.23) H4 1.0000 109.85 109.85 109.85 C4 - O4 C3 C5 C5 - Distance Angles O1 1.4398 (0.0039) C6 1.5170 (0.0039) 106.17 (0.27) C4 1.5364 (0.0040) 110.42 (0.24) 114.44 (0.24) H5 1.0000 108.55 108.55 108.55 C5 - O1 C6 C4 C6 - Distance Angles O5 1.4231 (0.0039) C5 1.5170 (0.0039) 113.75 (0.26) H6A 0.9900 108.81 108.81 H6B 0.9900 108.81 108.81 107.68 C6 - O5 C5 H6A C7 - Distance Angles O6 1.2428 (0.0037) N1 1.3359 (0.0039) 124.53 (0.26) C8 1.5111 (0.0038) 121.46 (0.27) 113.94 (0.27) C7 - O6 N1 C8 - Distance Angles C13 1.3903 (0.0041) C9 1.3928 (0.0042) 120.05 (0.27) C7 1.5111 (0.0038) 122.32 (0.27) 117.57 (0.27) C8 - C13 C9 C9 - Distance Angles C10 1.3895 (0.0041) C8 1.3928 (0.0042) 119.68 (0.29) H9 0.9500 120.16 120.16 C9 - C10 C8 C10 - Distance Angles C11 1.3819 (0.0044) C9 1.3895 (0.0041) 120.41 (0.31) H10 0.9500 119.79 119.79 C10 - C11 C9 C11 - Distance Angles C10 1.3819 (0.0044) C12 1.3852 (0.0045) 120.11 (0.29) H11 0.9500 119.94 119.94 C11 - C10 C12 C12 - Distance Angles C11 1.3852 (0.0045) C13 1.3965 (0.0041) 120.01 (0.30) H12 0.9500 119.99 119.99 C12 - C11 C13 C13 - Distance Angles C8 1.3903 (0.0041) C12 1.3965 (0.0041) 119.73 (0.30) C14 1.4974 (0.0045) 120.59 (0.27) 119.66 (0.28) C13 - C8 C12 C14 - Distance Angles O7 1.2089 (0.0036) O8 1.3207 (0.0036) 123.52 (0.32) C13 1.4974 (0.0045) 123.63 (0.28) 112.85 (0.27) C14 - O7 O8 N1 - Distance Angles C7 1.3359 (0.0039) C2 1.4598 (0.0034) 122.79 (0.27) H1N 0.9855 (0.0192) 121.61 (2.31) 115.40 (2.32) N1 - C7 C2 O1 - Distance Angles C1 1.4236 (0.0034) C5 1.4398 (0.0039) 113.51 (0.24) O1 - C1 O2 - Distance Angles C1 1.4035 (0.0038) H2A 0.8400 109.47 O2 - C1 O3 - Distance Angles C3 1.4286 (0.0035) H3A 0.8400 109.47 O3 - C3 O4 - Distance Angles C4 1.4271 (0.0039) H4A 0.8400 109.47 O4 - C4 O5 - Distance Angles C6 1.4231 (0.0039) H5A 0.8400 109.47 O5 - C6 O6 - Distance Angles C7 1.2428 (0.0037) O6 - O7 - Distance Angles C14 1.2089 (0.0036) O7 - O8 - Distance Angles C14 1.3207 (0.0036) H8 0.8400 109.47 O8 - C14 Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.89 2.715(3) 165.7 O2-H2A...O6_$1 0.84 1.97 2.807(3) 172.6 O3-H3A...O6_$2 0.84 1.84 2.674(3) 176.0 O4-H4A...O5_$3 0.84 1.89 2.677(3) 156.3 O5-H5A...O4_$4 0.84 1.78 2.614(3) 170.3 O8-H8...O3_$1 0.985(19) 1.99(2) 2.952(3) 166(4) N1-H1N...O7_$2] FMAP and GRID set by program FMAP 2 3 29 GRID -0.962 -2 -2 0.962 2 2 R1 = 0.0618 for 1992 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.27 at 0.1097 0.2378 0.1888 [ 0.71 A from C8 ] Deepest hole -0.27 at 0.2626 -0.0013 0.0208 [ 1.22 A from H6A ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2610 / 17769 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3903 0.7622 0.6888 1.00000 0.05 0.27 0.71 C8 0.85 C7 1.74 N1 1.76 C9 Q2 1 0.6108 0.8792 0.6429 1.00000 0.05 0.25 0.66 C13 0.87 C14 1.76 C8 1.77 O7 Q3 1 0.4077 0.9355 0.8527 1.00000 0.05 0.24 0.71 C1 0.73 O1 1.47 H1 1.78 C5 Q4 1 0.2620 0.8076 0.7797 1.00000 0.05 0.24 0.73 N1 0.83 C2 1.39 H1N 1.54 H2 Q5 1 0.3828 0.8764 0.8156 1.00000 0.05 0.22 0.74 C2 0.80 C1 1.37 H2 1.42 H1 Q6 1 -0.0140 0.8004 0.9128 1.00000 0.05 0.22 0.74 C4 0.76 O4 1.42 H4A 1.56 H4 Q7 1 0.5030 0.8572 0.6061 1.00000 0.05 0.22 0.61 C13 0.81 C12 1.49 H12 1.81 C8 Q8 1 0.3337 0.5782 0.5787 1.00000 0.05 0.22 1.65 H10 1.73 C10 2.04 C9 2.17 H9 Q9 1 0.7219 1.0601 0.7137 1.00000 0.05 0.22 1.81 O7 1.82 H8 2.12 C14 2.22 O8 Q10 1 -0.0262 0.6820 0.5754 1.00000 0.05 0.21 0.61 H10 0.96 C10 1.95 C9 1.99 C11 Q11 1 0.4182 0.8226 0.6484 1.00000 0.05 0.21 0.72 C13 0.76 C8 1.86 C12 1.89 C9 Q12 1 1.2278 0.9951 0.6370 1.00000 0.05 0.21 2.11 H8 2.22 C13 2.41 O8 2.41 C14 Q13 1 0.4686 0.8562 1.0256 1.00000 0.05 0.21 0.89 O5 1.15 H4A 1.62 H5A 1.92 C6 Q14 1 0.1751 0.6190 0.7315 1.00000 0.05 0.20 1.88 H9 2.19 C7 2.23 H2A 2.26 H3A Q15 1 0.8242 0.8398 0.7226 1.00000 0.05 0.20 1.17 O7 1.59 H1N 2.03 C7 2.08 O6 Q16 1 0.5461 0.8967 0.6456 1.00000 0.05 0.20 0.68 C13 0.90 C14 1.79 C8 1.84 O8 Q17 1 0.2157 0.7403 0.7387 1.00000 0.05 0.20 1.04 N1 1.27 C7 1.54 H1N 2.10 C2 Q18 1 0.3691 0.8122 0.9530 1.00000 0.05 0.20 1.27 H5A 1.33 O5 1.38 H4 1.67 C6 Q19 1 0.1059 0.7190 0.6059 1.00000 0.05 0.20 0.71 C10 1.02 C9 1.37 H10 1.68 H9 Q20 1 0.3963 0.6949 0.8684 1.00000 0.05 0.19 1.35 H4 1.61 H2 1.94 H8 1.97 C4 Shortest distances between peaks (including symmetry equivalents) 2 16 0.38 2 7 1.08 10 19 1.09 11 16 1.11 7 16 1.11 2 11 1.16 3 5 1.18 7 11 1.20 1 11 1.26 4 17 1.34 4 5 1.36 1 17 1.51 14 17 1.53 9 14 1.62 13 18 1.94 12 16 1.96 6 18 2.08 1 16 2.12 1 2 2.13 8 10 2.15 8 19 2.17 11 19 2.23 15 17 2.27 2 15 2.27 7 12 2.29 1 14 2.31 2 12 2.33 11 12 2.35 1 4 2.40 1 7 2.43 1 15 2.43 15 16 2.43 6 13 2.48 3 4 2.51 1 19 2.52 4 15 2.55 9 17 2.55 7 19 2.56 18 20 2.56 6 20 2.60 5 20 2.61 11 17 2.64 4 14 2.67 5 17 2.67 11 15 2.67 4 20 2.69 9 20 2.70 3 8 2.75 9 16 2.77 9 15 2.80 13 18 2.88 2 9 2.91 3 18 2.93 Time profile in seconds ----------------------- 0.05: 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. 0.72: 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 1.05: Structure factors and derivatives 1.09: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.28: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0683a finished at 23:42:10 Total CPU time: 3.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++