+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0461 started at 12:46:26 on 27-Apr-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0460 in P-1 CELL 0.71073 6.1704 7.1051 10.8713 79.486 76.174 67.853 ZERR 2.00 0.0004 0.0005 0.0006 0.004 0.004 0.003 LATT 1 SFAC C H N O S UNIT 20 14 6 2 0 V = 426.39 F(000) = 192.0 Mu = 0.10 mm-1 Cell Wt = 370.37 Rho = 1.442 MERG 2 OMIT -3.00 55.00 OMIT 0 2 1 EXTI 0.06330 SHEL 7 0.77 DFIX 0.89 0.02 N12 H12a N12 H12b EQIV_$1 x+1, y, z HTAB N12 N11_$1 EQIV_$2 -x, -y+1, -z+2 HTAB N12 N14_$2 FMAP 2 PLAN 10 SIZE 0.23 0.2 0.06 ACTA BOND $H WGHT 0.06680 0.10290 L.S. 4 TEMP -153.00 FVAR 1.50249 MOLE 1 C1 1 -0.066260 0.788669 0.412539 11.00000 0.02306 0.01856 = 0.01809 -0.00104 -0.00368 -0.00790 C2 1 0.134681 0.787356 0.319309 11.00000 0.01990 0.02559 = 0.02353 -0.00072 -0.00317 -0.01008 AFIX 43 H2 2 0.283345 0.757347 0.343400 11.00000 -1.20000 AFIX 0 C3 1 0.116511 0.830018 0.191383 11.00000 0.02458 0.02946 = 0.02068 -0.00067 0.00016 -0.01342 AFIX 43 H3 2 0.252925 0.828916 0.128063 11.00000 -1.20000 AFIX 0 C4 1 -0.100193 0.874106 0.156177 11.00000 0.03016 0.02802 = 0.01932 0.00071 -0.00524 -0.01392 AFIX 43 H4 2 -0.112059 0.902755 0.068704 11.00000 -1.20000 AFIX 0 C5 1 -0.300209 0.876531 0.248472 11.00000 0.02602 0.02734 = 0.02364 0.00028 -0.00733 -0.01229 AFIX 43 H5 2 -0.448764 0.907979 0.223883 11.00000 -1.20000 AFIX 0 C6 1 -0.284200 0.833186 0.376641 11.00000 0.02166 0.02640 = 0.02150 -0.00149 -0.00153 -0.01078 AFIX 43 H6 2 -0.421065 0.833878 0.439502 11.00000 -1.20000 AFIX 0 C7 1 -0.046453 0.739461 0.546507 11.00000 0.01693 0.02035 = 0.02183 -0.00220 -0.00420 -0.00754 C9 1 0.145365 0.661303 0.704924 11.00000 0.02289 0.02144 = 0.01716 -0.00109 -0.00353 -0.00944 C10 1 -0.085617 0.668903 0.748765 11.00000 0.01953 0.02447 = 0.01780 -0.00144 -0.00293 -0.00931 C13 1 -0.200340 0.640515 0.875942 11.00000 0.01979 0.03025 = 0.02109 -0.00229 -0.00438 -0.01002 N11 3 -0.203530 0.716990 0.645361 11.00000 0.01943 0.02483 = 0.01775 -0.00126 -0.00273 -0.00917 N12 3 0.334608 0.618760 0.757348 11.00000 0.02017 0.03597 = 0.02053 0.00254 -0.00450 -0.01425 N14 3 -0.296055 0.619117 0.979855 11.00000 0.02496 0.04872 = 0.02152 -0.00219 -0.00279 -0.01637 O8 4 0.172892 0.707441 0.575916 11.00000 0.01906 0.02702 = 0.01863 0.00008 -0.00333 -0.01091 H12A 2 0.460276 0.649622 0.713132 11.00000 0.02832 H12B 2 0.325061 0.571107 0.838971 11.00000 0.04514 HKLF 4 Covalent radii and connectivity table for 2009src0461 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C1 - C6 C2 C7 C2 - C3 C1 C3 - C4 C2 C4 - C3 C5 C5 - C4 C6 C6 - C5 C1 C7 - N11 O8 C1 C9 - N12 O8 C10 C10 - C9 N11 C13 C13 - N14 C10 N11 - C7 C10 N12 - C9 N14 - C13 O8 - C9 C7 Operators for generating equivalent atoms: $1 x+1, y, z $2 -x, -y+1, -z+2 9562 Reflections read, of which 23 rejected -7 =< h =< 7, -9 =< k =< 9, -14 =< l =< 14, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 1946 Unique reflections, of which 0 suppressed R(int) = 0.0526 R(sigma) = 0.0417 Friedel opposites merged Maximum memory for data reduction = 1351 / 19508 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 = 1694 / 172597 wR2 = 0.1230 before cycle 1 for 1946 data and 136 / 136 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.035; Restrained GooF = 1.034 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.50247 0.00528 -0.003 OSF 2 0.06342 0.01469 0.008 EXTI Mean shift/su = 0.018 Maximum = -0.055 for U22 C1 Max. shift = 0.000 A for H12A Max. dU = 0.000 for H12A Least-squares cycle 2 Maximum vector length = 511 Memory required = 1694 / 172597 wR2 = 0.1230 before cycle 2 for 1946 data and 136 / 136 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.035; Restrained GooF = 1.034 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.50234 0.00528 -0.025 OSF 2 0.06344 0.01470 0.001 EXTI Mean shift/su = 0.006 Maximum = -0.025 for OSF Max. shift = 0.000 A for H12B Max. dU = 0.000 for H12A Least-squares cycle 3 Maximum vector length = 511 Memory required = 1694 / 172597 wR2 = 0.1230 before cycle 3 for 1946 data and 136 / 136 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.035; Restrained GooF = 1.034 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.50233 0.00528 -0.001 OSF 2 0.06343 0.01470 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.001 for x H12A Max. shift = 0.000 A for H12A Max. dU = 0.000 for H12A Least-squares cycle 4 Maximum vector length = 511 Memory required = 1694 / 172597 wR2 = 0.1230 before cycle 4 for 1946 data and 136 / 136 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.035; Restrained GooF = 1.034 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.50233 0.00528 0.000 OSF 2 0.06342 0.01470 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for EXTI Max. shift = 0.000 A for H12A Max. dU = 0.000 for H12A No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.2833 0.7573 0.3434 43 0.950 0.000 C2 C3 C1 H3 0.2529 0.8289 0.1281 43 0.950 0.000 C3 C4 C2 H4 -0.1121 0.9027 0.0687 43 0.950 0.000 C4 C3 C5 H5 -0.4488 0.9080 0.2239 43 0.950 0.000 C5 C4 C6 H6 -0.4211 0.8339 0.4395 43 0.950 0.000 C6 C5 C1 2009src0461 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.06625 0.78867 0.41254 1.00000 0.02301 0.01851 0.01807 -0.00104 -0.00367 -0.00787 0.01982 0.00190 0.00025 0.00020 0.00013 0.00000 0.00075 0.00068 0.00069 0.00052 0.00054 0.00057 0.00033 C2 0.13468 0.78736 0.31931 1.00000 0.01988 0.02556 0.02349 -0.00072 -0.00316 -0.01007 0.02274 0.00207 0.00026 0.00022 0.00014 0.00000 0.00073 0.00074 0.00073 0.00056 0.00056 0.00059 0.00033 H2 0.28335 0.75735 0.34340 1.00000 0.02729 0.00000 0.00000 C3 0.11651 0.83002 0.19138 1.00000 0.02456 0.02942 0.02065 -0.00066 0.00017 -0.01341 0.02474 0.00210 0.00027 0.00023 0.00014 0.00000 0.00078 0.00079 0.00072 0.00059 0.00057 0.00063 0.00035 H3 0.25292 0.82892 0.12806 1.00000 0.02969 0.00000 0.00000 C4 -0.10019 0.87410 0.15618 1.00000 0.03015 0.02798 0.01928 0.00071 -0.00525 -0.01391 0.02499 0.00208 0.00028 0.00023 0.00014 0.00000 0.00083 0.00077 0.00069 0.00057 0.00059 0.00065 0.00035 H4 -0.11206 0.90275 0.06871 1.00000 0.02999 0.00000 0.00000 C5 -0.30019 0.87653 0.24847 1.00000 0.02599 0.02731 0.02361 0.00028 -0.00731 -0.01228 0.02465 0.00205 0.00027 0.00022 0.00014 0.00000 0.00078 0.00077 0.00074 0.00059 0.00060 0.00063 0.00035 H5 -0.44875 0.90798 0.22388 1.00000 0.02959 0.00000 0.00000 C6 -0.28419 0.83319 0.37664 1.00000 0.02162 0.02636 0.02148 -0.00148 -0.00153 -0.01076 0.02303 0.00204 0.00026 0.00022 0.00014 0.00000 0.00074 0.00074 0.00072 0.00057 0.00055 0.00060 0.00034 H6 -0.42106 0.83389 0.43950 1.00000 0.02763 0.00000 0.00000 C7 -0.04646 0.73946 0.54650 1.00000 0.01689 0.02032 0.02182 -0.00221 -0.00418 -0.00752 0.01926 0.00190 0.00024 0.00020 0.00013 0.00000 0.00069 0.00069 0.00072 0.00054 0.00052 0.00055 0.00032 C9 0.14537 0.66130 0.70493 1.00000 0.02289 0.02141 0.01713 -0.00108 -0.00353 -0.00945 0.02013 0.00194 0.00026 0.00021 0.00013 0.00000 0.00073 0.00070 0.00066 0.00052 0.00053 0.00057 0.00033 C10 -0.08562 0.66891 0.74876 1.00000 0.01952 0.02444 0.01778 -0.00144 -0.00290 -0.00930 0.02030 0.00195 0.00025 0.00022 0.00013 0.00000 0.00070 0.00071 0.00067 0.00053 0.00052 0.00056 0.00033 C13 -0.20034 0.64050 0.87595 1.00000 0.01977 0.03023 0.02106 -0.00230 -0.00436 -0.01002 0.02325 0.00196 0.00025 0.00022 0.00013 0.00000 0.00074 0.00080 0.00075 0.00058 0.00057 0.00062 0.00035 N11 -0.20353 0.71699 0.64536 1.00000 0.01942 0.02480 0.01774 -0.00126 -0.00270 -0.00917 0.02048 0.00162 0.00021 0.00018 0.00011 0.00000 0.00062 0.00063 0.00060 0.00047 0.00047 0.00050 0.00031 N12 0.33461 0.61876 0.75735 1.00000 0.02015 0.03594 0.02050 0.00254 -0.00450 -0.01423 0.02482 0.00177 0.00022 0.00020 0.00012 0.00000 0.00066 0.00074 0.00064 0.00054 0.00051 0.00057 0.00032 N14 -0.29605 0.61912 0.97986 1.00000 0.02494 0.04867 0.02151 -0.00220 -0.00279 -0.01635 0.03113 0.00186 0.00023 0.00022 0.00012 0.00000 0.00070 0.00087 0.00067 0.00059 0.00052 0.00063 0.00035 O8 0.17289 0.70744 0.57591 1.00000 0.01904 0.02700 0.01860 0.00008 -0.00331 -0.01090 0.02106 0.00133 0.00017 0.00015 0.00009 0.00000 0.00053 0.00055 0.00051 0.00039 0.00038 0.00043 0.00027 H12A 0.46027 0.64964 0.71309 1.00000 0.02848 0.02364 0.00272 0.00260 0.00155 0.00000 0.00445 H12B 0.32503 0.57113 0.83901 1.00000 0.04503 0.02762 0.00366 0.00305 0.00149 0.00000 0.00544 Final Structure Factor Calculation for 2009src0461 in P-1 Total number of l.s. parameters = 136 Maximum vector length = 511 Memory required = 1558 / 24017 wR2 = 0.1230 before cycle 5 for 1946 data and 0 / 136 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.035; Restrained GooF = 1.034 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0463 for 1565 Fo > 4sig(Fo) and 0.0619 for all 1946 data wR2 = 0.1230, GooF = S = 1.035, Restrained GooF = 1.034 for all data Occupancy sum of asymmetric unit = 14.00 for non-hydrogen and 7.00 for hydrogen atoms Principal mean square atomic displacements U 0.0231 0.0190 0.0174 C1 0.0268 0.0235 0.0179 C2 0.0306 0.0271 0.0164 C3 0.0322 0.0242 0.0185 C4 0.0305 0.0227 0.0208 C5 0.0268 0.0243 0.0180 C6 0.0218 0.0204 0.0156 C7 0.0236 0.0198 0.0170 C9 0.0246 0.0189 0.0174 C10 0.0304 0.0211 0.0182 C13 0.0250 0.0192 0.0172 N11 0.0383 0.0198 0.0164 N12 0.0491 0.0237 0.0207 N14 0.0280 0.0189 0.0163 O8 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.021 0.032 0.042 0.055 0.070 0.088 0.118 0.172 1.000 Number in group 215. 180. 201. 196. 190. 195. 188. 192. 193. 196. GooF 0.938 0.963 1.107 1.019 1.140 1.068 1.125 1.002 0.981 0.992 K 1.670 1.133 0.931 0.971 0.948 0.970 0.989 1.017 1.034 1.024 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.66 inf Number in group 199. 200. 185. 195. 200. 190. 194. 193. 195. 195. GooF 1.014 1.082 1.076 1.147 1.046 1.025 0.886 0.936 0.999 1.111 K 1.019 1.070 1.054 1.001 1.026 1.030 1.033 1.035 1.044 0.997 R1 0.164 0.130 0.107 0.089 0.071 0.055 0.037 0.037 0.037 0.035 Recommended weighting scheme: WGHT 0.0662 0.1039 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 1 11 6.46 11.90 3.92 0.049 0.98 6 2 6 22.59 34.14 3.67 0.083 0.97 -2 -5 8 1.16 5.00 3.63 0.032 0.87 6 8 4 58.73 40.65 3.19 0.090 0.79 3 2 4 1.60 0.23 3.12 0.007 1.80 0 0 9 16.39 25.12 2.95 0.071 1.17 0 -3 10 1.89 4.18 2.94 0.029 0.91 3 0 1 19.87 26.90 2.92 0.073 1.90 -3 -8 1 19.50 28.16 2.90 0.075 0.85 -5 -1 6 8.09 12.62 2.83 0.050 0.89 -4 3 7 14.46 22.12 2.83 0.067 0.82 2 1 4 7.73 4.94 2.82 0.031 2.27 1 -5 9 9.81 17.92 2.81 0.060 0.81 6 0 8 -0.16 4.47 2.81 0.030 0.84 -2 3 3 10.05 14.35 2.75 0.054 1.36 2 -1 5 15.12 10.92 2.68 0.047 1.65 4 6 0 1.82 0.13 2.67 0.005 1.06 -2 -1 6 43.13 55.68 2.67 0.106 1.37 -2 3 11 5.23 10.23 2.67 0.045 0.79 7 4 6 13.68 8.04 2.67 0.040 0.85 -3 0 10 87.16 65.59 2.66 0.115 0.85 2 1 12 4.02 7.12 2.66 0.038 0.90 -2 6 0 0.87 3.84 2.65 0.028 0.91 5 8 0 6.17 0.39 2.63 0.009 0.81 -1 1 11 6.06 11.11 2.63 0.047 0.91 3 1 6 4.83 2.66 2.62 0.023 1.50 0 1 0 89.77 115.85 2.62 0.152 6.55 5 -3 3 8.70 15.75 2.57 0.056 0.88 7 6 6 10.34 16.43 2.57 0.057 0.80 6 6 7 25.79 36.00 2.56 0.085 0.86 -2 0 5 8.10 11.38 2.55 0.048 1.55 -1 1 3 79.15 97.16 2.54 0.139 2.46 0 -1 13 9.82 4.19 2.52 0.029 0.79 7 1 6 15.21 22.66 2.51 0.067 0.82 -6 -4 5 6.38 12.50 2.50 0.050 0.81 -6 1 5 0.58 3.51 2.48 0.026 0.77 0 -7 2 5.33 9.21 2.47 0.043 0.90 7 2 3 4.68 2.15 2.47 0.021 0.87 6 -2 4 11.65 6.22 2.45 0.035 0.82 2 3 6 38.57 31.01 2.45 0.079 1.54 7 3 5 19.31 26.31 2.44 0.073 0.87 0 6 5 0.14 2.51 2.44 0.022 1.01 3 0 9 -0.44 0.82 2.42 0.013 1.09 -1 6 4 9.83 15.22 2.39 0.055 0.96 5 7 9 137.25 111.92 2.39 0.150 0.81 -1 0 2 160.65 192.46 2.38 0.196 3.52 6 5 8 2.97 6.34 2.37 0.036 0.87 1 -1 10 54.72 67.57 2.37 0.116 1.03 -6 -6 4 14.05 22.55 2.36 0.067 0.77 6 -2 2 -0.60 3.41 2.35 0.026 0.83 Bond lengths and angles C1 - Distance Angles C6 1.3949 (0.0020) C2 1.3995 (0.0019) 119.79 (0.13) C7 1.4578 (0.0019) 120.17 (0.13) 120.03 (0.13) C1 - C6 C2 C2 - Distance Angles C3 1.3905 (0.0020) C1 1.3995 (0.0019) 119.94 (0.14) H2 0.9500 120.03 120.03 C2 - C3 C1 C3 - Distance Angles C4 1.3848 (0.0021) C2 1.3905 (0.0020) 120.08 (0.13) H3 0.9500 119.96 119.96 C3 - C4 C2 C4 - Distance Angles C3 1.3848 (0.0021) C5 1.3887 (0.0021) 120.14 (0.13) H4 0.9500 119.93 119.93 C4 - C3 C5 C5 - Distance Angles C4 1.3887 (0.0021) C6 1.3900 (0.0020) 120.35 (0.14) H5 0.9500 119.82 119.82 C5 - C4 C6 C6 - Distance Angles C5 1.3900 (0.0020) C1 1.3949 (0.0020) 119.70 (0.13) H6 0.9500 120.15 120.15 C6 - C5 C1 C7 - Distance Angles N11 1.2946 (0.0018) O8 1.3907 (0.0017) 113.24 (0.12) C1 1.4578 (0.0019) 129.72 (0.13) 117.03 (0.12) C7 - N11 O8 C9 - Distance Angles N12 1.3300 (0.0019) O8 1.3652 (0.0016) 117.27 (0.12) C10 1.3741 (0.0020) 135.56 (0.14) 107.17 (0.12) C9 - N12 O8 C10 - Distance Angles C9 1.3741 (0.0020) N11 1.4046 (0.0018) 109.37 (0.12) C13 1.4112 (0.0019) 128.06 (0.13) 122.55 (0.13) C10 - C9 N11 C13 - Distance Angles N14 1.1551 (0.0019) C10 1.4112 (0.0019) 179.31 (0.17) C13 - N14 N11 - Distance Angles C7 1.2946 (0.0018) C10 1.4046 (0.0018) 104.82 (0.12) N11 - C7 N12 - Distance Angles C9 1.3300 (0.0019) H12A 0.8901 (0.0139) 120.11 (1.14) H12B 0.8868 (0.0151) 117.93 (1.36) 121.68 (1.76) N12 - C9 H12A N14 - Distance Angles C13 1.1551 (0.0019) N14 - O8 - Distance Angles C9 1.3652 (0.0016) C7 1.3907 (0.0017) 105.39 (0.11) O8 - C9 Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.890(14) 2.228(14) 3.1020(17) 167.0(16) N12-H12A...N11_$1 0.887(15) 2.186(16) 3.0482(19) 163.9(18) N12-H12B...N14_$2 FMAP and GRID set by program FMAP 2 1 19 GRID -3.125 -2 -2 3.125 2 2 R1 = 0.0619 for 1946 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.32 at 0.0523 0.2150 0.5742 [ 0.18 A from C1 ] Deepest hole -0.23 at 0.4018 0.1517 0.7172 [ 0.73 A from C5 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 1658 / 16204 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.4308 0.8201 0.4969 1.00000 0.05 0.22 0.61 H6 1.41 C6 2.16 C1 2.23 N11 Q2 1 0.3438 0.7042 0.4778 1.00000 0.05 0.22 1.31 O8 1.54 H2 1.93 H6 2.26 C2 Q3 1 -0.3740 0.7615 0.5953 1.00000 0.05 0.20 1.21 N11 1.71 H12A 1.74 H6 1.92 C7 Q4 1 0.3342 0.7397 0.3520 1.00000 0.05 0.20 0.32 H2 1.27 C2 2.21 H5 2.31 H6 Q5 1 -0.2794 0.8201 0.3139 1.00000 0.05 0.20 0.70 C6 0.76 C5 1.43 H6 1.49 H5 Q6 1 -0.1629 0.7117 0.6963 1.00000 0.05 0.19 0.65 N11 0.78 C10 1.62 C7 1.82 C9 Q7 1 0.1079 0.8498 0.2593 1.00000 0.05 0.19 0.74 C2 0.76 C3 1.47 H2 1.49 H3 Q8 1 0.0141 0.6389 0.8247 1.00000 0.05 0.19 1.09 C10 1.30 C13 1.38 C9 1.83 H12B Q9 1 0.1591 0.7375 0.4473 1.00000 0.05 0.19 1.22 H2 1.39 O8 1.40 C2 1.42 C1 Q10 1 -0.2499 0.7899 0.5000 1.00000 0.05 0.17 1.29 H6 1.29 C1 1.36 C7 1.37 C6 Shortest distances between peaks (including symmetry equivalents) 1 10 1.06 1 3 1.16 3 10 1.17 2 9 1.19 4 9 1.31 2 4 1.36 4 7 1.77 3 6 1.79 6 8 1.86 1 2 1.93 1 5 1.98 5 10 2.04 7 9 2.11 6 10 2.25 9 10 2.35 1 1 2.38 5 7 2.40 2 3 2.57 4 5 2.58 1 4 2.64 1 10 2.73 1 3 2.84 2 2 2.84 1 6 2.86 2 5 2.86 2 10 2.86 2 7 2.91 3 5 2.95 6 9 2.97 1 9 2.99 Time profile in seconds ----------------------- 0.03: 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 0.00: Analyse other restraints etc. 0.45: 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 0.17: Structure factors and derivatives 0.28: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0461 finished at 12:46:27 Total CPU time: 1.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++