+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0459 started at 12:03:06 on 27-Apr-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0459 in P-1 CELL 0.71073 5.4433 6.1440 15.5205 87.696 84.420 70.454 ZERR 2.00 0.0002 0.0003 0.0007 0.003 0.003 0.002 LATT 1 SFAC C H N O UNIT 20 26 6 2 V = 486.82 F(000) = 204.0 Mu = 0.09 mm-1 Cell Wt = 382.47 Rho = 1.305 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 DFIX 0.89 0.02 N12 H12a N12 H12b FMAP 2 PLAN 10 SIZE 0.04 0.06 0.09 ACTA EQIV_$1 x, y-1, z HTAB N12 N11_$1 EQIV_$2 -x+3, -y, -z HTAB N12 N14_$2 BOND $H WGHT 0.02570 0.49100 L.S. 4 TEMP -153.00 FVAR 1.23680 MOLE 1 C1 1 0.482462 0.489846 0.263401 11.00000 0.01771 0.02350 = 0.02367 -0.00321 0.00167 -0.00738 AFIX 13 H1 2 0.323991 0.479823 0.238469 11.00000 -1.20000 AFIX 0 C2 1 0.496631 0.371740 0.352830 11.00000 0.02392 0.02853 = 0.02741 -0.00157 0.00382 -0.00685 AFIX 23 H2A 2 0.514749 0.207304 0.346351 11.00000 -1.20000 H2B 2 0.652185 0.378343 0.379349 11.00000 -1.20000 AFIX 0 C3 1 0.249197 0.491759 0.411754 11.00000 0.02799 0.03887 = 0.02854 -0.00280 0.00889 -0.00727 AFIX 23 H3A 2 0.096636 0.469002 0.388455 11.00000 -1.20000 H3B 2 0.266413 0.420338 0.470161 11.00000 -1.20000 AFIX 0 C4 1 0.201747 0.749536 0.418831 11.00000 0.03037 0.03805 = 0.03566 -0.01385 0.00608 -0.00473 AFIX 23 H4A 2 0.032399 0.823385 0.452918 11.00000 -1.20000 H4B 2 0.341512 0.772675 0.449862 11.00000 -1.20000 AFIX 0 C5 1 0.197937 0.864124 0.329947 11.00000 0.02503 0.02579 = 0.04458 -0.00786 0.00275 -0.00476 AFIX 23 H5A 2 0.180077 1.028405 0.336707 11.00000 -1.20000 H5B 2 0.044238 0.858597 0.301995 11.00000 -1.20000 AFIX 0 C6 1 0.447062 0.745117 0.271942 11.00000 0.02282 0.02162 = 0.03465 -0.00161 0.00083 -0.00689 AFIX 23 H6A 2 0.600138 0.761451 0.297161 11.00000 -1.20000 H6B 2 0.435408 0.819425 0.213992 11.00000 -1.20000 AFIX 0 C7 1 0.713884 0.370136 0.203048 11.00000 0.02099 0.01983 = 0.02300 -0.00209 -0.00098 -0.00711 C9 1 0.966882 0.070440 0.128384 11.00000 0.01990 0.02211 = 0.01958 -0.00033 0.00185 -0.00765 C10 1 1.055187 0.254612 0.113896 11.00000 0.02179 0.02104 = 0.02049 -0.00069 0.00204 -0.00818 C13 1 1.273429 0.265231 0.058675 11.00000 0.02376 0.01947 = 0.02548 -0.00076 0.00068 -0.00892 N11 3 0.887925 0.444502 0.162805 11.00000 0.01997 0.02237 = 0.02383 -0.00258 0.00267 -0.00744 N12 3 1.045234 -0.145492 0.100498 11.00000 0.02773 0.02032 = 0.03183 -0.00525 0.01004 -0.01202 N14 3 1.452589 0.269498 0.013748 11.00000 0.02871 0.02475 = 0.03799 -0.00328 0.00843 -0.01248 O8 4 0.749836 0.141043 0.185747 11.00000 0.02172 0.02073 = 0.02547 -0.00325 0.00558 -0.00975 H12B 2 0.967849 -0.241942 0.121603 11.00000 0.02484 H12A 2 1.188283 -0.196285 0.064198 11.00000 0.03692 HKLF 4 Covalent radii and connectivity table for 2009src0459 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - C7 C6 C2 C2 - C3 C1 C3 - C4 C2 C4 - C5 C3 C5 - C4 C6 C6 - C1 C5 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, y-1, z $2 -x+3, -y, -z 8875 Reflections read, of which 16 rejected -7 =< h =< 7, -7 =< k =< 7, -20 =< l =< 20, Max. 2-theta = 54.94 0 Systematic absence violations 0 Inconsistent equivalents 2205 Unique reflections, of which 0 suppressed R(int) = 0.0580 R(sigma) = 0.0485 Friedel opposites merged Maximum memory for data reduction = 1584 / 21960 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 = 1965 / 170415 wR2 = 0.1310 before cycle 1 for 2205 data and 135 / 135 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.083; Restrained GooF = 1.083 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 0.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.23708 0.00334 0.084 OSF Mean shift/su = 0.024 Maximum = 0.099 for U13 N12 Max. shift = 0.001 A for H12A Max. dU = 0.000 for H12B Least-squares cycle 2 Maximum vector length = 511 Memory required = 1965 / 170415 wR2 = 0.1310 before cycle 2 for 2205 data and 135 / 135 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.083; Restrained GooF = 1.083 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 0.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.23715 0.00334 0.020 OSF Mean shift/su = 0.009 Maximum = 0.038 for U13 N12 Max. shift = 0.000 A for H12A Max. dU = 0.000 for H12B Least-squares cycle 3 Maximum vector length = 511 Memory required = 1965 / 170415 wR2 = 0.1309 before cycle 3 for 2205 data and 135 / 135 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.083; Restrained GooF = 1.082 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 0.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.23716 0.00334 0.003 OSF Mean shift/su = 0.001 Maximum = 0.003 for OSF Max. shift = 0.000 A for H12B Max. dU = 0.000 for H12A Least-squares cycle 4 Maximum vector length = 511 Memory required = 1965 / 170415 wR2 = 0.1309 before cycle 4 for 2205 data and 135 / 135 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.083; Restrained GooF = 1.082 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 0.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.23716 0.00334 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for y H12B Max. shift = 0.000 A for H12B Max. dU = 0.000 for H12A Largest correlation matrix elements -0.553 y H12B / x H12B Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.3240 0.4798 0.2385 13 1.000 0.000 C1 C7 C6 C2 H2A 0.5147 0.2073 0.3463 23 0.990 0.000 C2 C3 C1 H2B 0.6522 0.3783 0.3793 23 0.990 0.000 C2 C3 C1 H3A 0.0966 0.4691 0.3884 23 0.990 0.000 C3 C4 C2 H3B 0.2664 0.4203 0.4701 23 0.990 0.000 C3 C4 C2 H4A 0.0324 0.8234 0.4529 23 0.990 0.000 C4 C5 C3 H4B 0.3416 0.7726 0.4499 23 0.990 0.000 C4 C5 C3 H5A 0.1800 1.0284 0.3367 23 0.990 0.000 C5 C4 C6 H5B 0.0442 0.8586 0.3020 23 0.990 0.000 C5 C4 C6 H6A 0.4354 0.8194 0.2140 23 0.990 0.000 C6 C1 C5 H6B 0.6001 0.7614 0.2972 23 0.990 0.000 C6 C1 C5 2009src0459 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.48247 0.48986 0.26341 1.00000 0.01766 0.02353 0.02370 -0.00322 0.00168 -0.00738 0.02165 0.00294 0.00036 0.00033 0.00012 0.00000 0.00089 0.00100 0.00100 0.00077 0.00074 0.00076 0.00042 H1 0.32399 0.47984 0.23848 1.00000 0.02598 0.00000 0.00000 C2 0.49663 0.37175 0.35281 1.00000 0.02393 0.02854 0.02747 -0.00160 0.00382 -0.00686 0.02750 0.00334 0.00040 0.00037 0.00013 0.00000 0.00101 0.00110 0.00110 0.00085 0.00082 0.00085 0.00046 H2A 0.51474 0.20732 0.34633 1.00000 0.03300 0.00000 0.00000 H2B 0.65218 0.37834 0.37934 1.00000 0.03300 0.00000 0.00000 C3 0.24917 0.49178 0.41174 1.00000 0.02803 0.03885 0.02856 -0.00281 0.00890 -0.00727 0.03351 0.00369 0.00043 0.00040 0.00015 0.00000 0.00111 0.00128 0.00115 0.00094 0.00089 0.00096 0.00052 H3A 0.09660 0.46906 0.38843 1.00000 0.04021 0.00000 0.00000 H3B 0.26636 0.42034 0.47014 1.00000 0.04021 0.00000 0.00000 C4 0.20176 0.74953 0.41884 1.00000 0.03034 0.03810 0.03574 -0.01390 0.00614 -0.00473 0.03664 0.00367 0.00046 0.00041 0.00015 0.00000 0.00116 0.00130 0.00128 0.00102 0.00095 0.00099 0.00056 H4A 0.03244 0.82338 0.45294 1.00000 0.04397 0.00000 0.00000 H4B 0.34157 0.77263 0.44985 1.00000 0.04397 0.00000 0.00000 C5 0.19790 0.86412 0.32996 1.00000 0.02504 0.02581 0.04461 -0.00789 0.00277 -0.00476 0.03294 0.00356 0.00042 0.00038 0.00015 0.00000 0.00108 0.00112 0.00134 0.00096 0.00094 0.00088 0.00052 H5A 0.18004 1.02840 0.33672 1.00000 0.03953 0.00000 0.00000 H5B 0.04420 0.85859 0.30201 1.00000 0.03953 0.00000 0.00000 C6 0.44706 0.74509 0.27194 1.00000 0.02283 0.02163 0.03471 -0.00162 0.00083 -0.00691 0.02671 0.00325 0.00039 0.00034 0.00014 0.00000 0.00100 0.00103 0.00117 0.00085 0.00085 0.00082 0.00046 H6A 0.43540 0.81939 0.21399 1.00000 0.03205 0.00000 0.00000 H6B 0.60014 0.76143 0.29716 1.00000 0.03205 0.00000 0.00000 C7 0.71387 0.37015 0.20305 1.00000 0.02102 0.01979 0.02301 -0.00211 -0.00097 -0.00713 0.02120 0.00288 0.00037 0.00033 0.00012 0.00000 0.00094 0.00095 0.00098 0.00075 0.00076 0.00076 0.00041 C9 0.96690 0.07044 0.12838 1.00000 0.01988 0.02216 0.01959 -0.00037 0.00186 -0.00763 0.02063 0.00291 0.00036 0.00034 0.00012 0.00000 0.00091 0.00095 0.00094 0.00073 0.00072 0.00075 0.00040 C10 1.05518 0.25462 0.11390 1.00000 0.02182 0.02108 0.02054 -0.00071 0.00205 -0.00820 0.02113 0.00294 0.00037 0.00033 0.00012 0.00000 0.00094 0.00097 0.00095 0.00074 0.00075 0.00076 0.00041 C13 1.27345 0.26523 0.05867 1.00000 0.02383 0.01940 0.02554 -0.00080 0.00063 -0.00890 0.02267 0.00297 0.00038 0.00033 0.00013 0.00000 0.00099 0.00096 0.00103 0.00076 0.00080 0.00079 0.00042 N11 0.88793 0.44451 0.16281 1.00000 0.02002 0.02237 0.02387 -0.00257 0.00266 -0.00749 0.02223 0.00248 0.00031 0.00028 0.00011 0.00000 0.00080 0.00085 0.00086 0.00066 0.00065 0.00066 0.00038 N12 1.04523 -0.14549 0.10050 1.00000 0.02775 0.02031 0.03190 -0.00528 0.01015 -0.01202 0.02638 0.00273 0.00035 0.00030 0.00012 0.00000 0.00094 0.00089 0.00098 0.00072 0.00076 0.00075 0.00041 N14 1.45258 0.26950 0.01375 1.00000 0.02877 0.02472 0.03802 -0.00331 0.00848 -0.01251 0.03030 0.00283 0.00035 0.00031 0.00012 0.00000 0.00094 0.00094 0.00106 0.00076 0.00079 0.00075 0.00043 O8 0.74985 0.14104 0.18575 1.00000 0.02173 0.02071 0.02550 -0.00328 0.00564 -0.00976 0.02242 0.00201 0.00025 0.00023 0.00009 0.00000 0.00069 0.00070 0.00074 0.00055 0.00055 0.00055 0.00033 H12B 0.96796 -0.24190 0.12164 1.00000 0.02506 0.03164 0.00411 0.00347 0.00139 0.00000 0.00576 H12A 1.18828 -0.19642 0.06426 1.00000 0.03699 0.03703 0.00382 0.00415 0.00141 0.00000 0.00677 Final Structure Factor Calculation for 2009src0459 in P-1 Total number of l.s. parameters = 135 Maximum vector length = 511 Memory required = 1830 / 22995 wR2 = 0.1309 before cycle 5 for 2205 data and 0 / 135 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.083; Restrained GooF = 1.082 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 0.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0591 for 1737 Fo > 4sig(Fo) and 0.0797 for all 2205 data wR2 = 0.1309, GooF = S = 1.083, Restrained GooF = 1.082 for all data Occupancy sum of asymmetric unit = 14.00 for non-hydrogen and 13.00 for hydrogen atoms Principal mean square atomic displacements U 0.0271 0.0216 0.0163 C1 0.0334 0.0293 0.0198 C2 0.0443 0.0384 0.0178 C3 0.0507 0.0403 0.0189 C4 0.0478 0.0307 0.0203 C5 0.0360 0.0229 0.0213 C6 0.0241 0.0208 0.0187 C7 0.0237 0.0221 0.0161 C9 0.0256 0.0207 0.0171 C10 0.0279 0.0222 0.0179 C13 0.0276 0.0217 0.0173 N11 0.0442 0.0189 0.0160 N12 0.0469 0.0247 0.0193 N14 0.0326 0.0192 0.0155 O8 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.010 0.018 0.027 0.037 0.048 0.062 0.079 0.105 0.145 1.000 Number in group 238. 205. 232. 216. 225. 212. 222. 216. 218. 221. GooF 1.092 1.198 1.117 1.175 1.120 1.064 0.996 0.949 0.980 1.113 K 2.885 1.611 1.120 1.037 1.006 1.014 0.996 1.005 1.003 1.000 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.31 1.66 inf Number in group 227. 221. 218. 225. 212. 220. 219. 222. 219. 222. GooF 1.204 1.125 1.169 1.185 1.029 1.023 0.925 0.947 0.920 1.231 K 1.052 1.089 1.089 1.055 1.025 0.988 0.981 0.989 1.024 0.993 R1 0.212 0.177 0.146 0.127 0.097 0.075 0.048 0.050 0.039 0.035 Recommended weighting scheme: WGHT 0.0253 0.4899 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) 6 1 1 25.29 10.28 3.79 0.040 0.89 -1 1 0 6.10 0.71 3.76 0.011 3.32 1 6 9 11.64 1.21 3.58 0.014 0.88 5 7 0 1.14 8.75 3.43 0.037 0.78 -4 2 9 8.47 0.95 3.40 0.012 0.87 -2 0 5 1032.13 894.80 3.32 0.373 1.89 0 2 19 24.67 7.35 3.23 0.034 0.78 6 0 6 7.53 0.20 3.18 0.006 0.83 4 5 12 -4.08 7.13 3.12 0.033 0.85 6 3 6 9.01 1.76 2.90 0.017 0.87 3 -3 14 6.03 0.43 2.88 0.008 0.80 4 7 1 -2.11 3.11 2.87 0.022 0.83 0 -1 1 716.12 816.79 2.83 0.357 5.41 -4 1 6 13.96 6.32 2.83 0.031 1.03 -3 4 9 118.87 89.76 2.82 0.118 0.82 0 0 14 -1.49 2.46 2.81 0.020 1.10 0 1 2 709.62 810.81 2.79 0.355 4.65 1 6 3 49.25 34.58 2.71 0.073 1.00 -3 1 10 2.37 8.11 2.71 0.036 1.04 0 3 1 391.78 329.98 2.71 0.227 1.92 -2 -7 1 21.65 11.07 2.69 0.042 0.87 -2 1 3 688.76 603.43 2.69 0.307 1.89 -2 -1 2 124.31 100.88 2.68 0.125 2.47 1 -4 12 14.03 4.28 2.68 0.026 0.92 -4 -6 5 6.87 1.54 2.67 0.016 0.88 3 0 14 13.01 1.69 2.66 0.016 0.97 5 -3 1 14.31 27.72 2.65 0.066 0.80 -1 -7 8 5.52 13.31 2.62 0.046 0.78 3 -3 5 4.90 0.02 2.61 0.002 1.06 0 -1 4 324.82 374.00 2.60 0.241 3.20 -3 5 7 37.37 55.35 2.56 0.093 0.77 1 4 1 812.67 723.44 2.55 0.336 1.53 -1 5 8 9.84 1.70 2.53 0.016 0.92 -1 1 5 1210.06 1085.24 2.53 0.411 2.20 -5 -5 3 -1.32 2.43 2.52 0.019 0.91 1 0 2 2264.80 2517.82 2.51 0.626 4.45 -3 1 14 63.34 44.85 2.49 0.084 0.86 4 -4 8 49.03 28.75 2.48 0.067 0.78 0 2 12 17.79 27.80 2.44 0.066 1.18 -4 -3 1 29.29 40.81 2.43 0.080 1.26 0 -5 2 58.70 75.23 2.40 0.108 1.14 1 1 4 96.49 117.75 2.39 0.135 3.12 2 -4 14 39.50 22.13 2.39 0.059 0.80 0 -6 6 -1.11 2.18 2.38 0.018 0.90 -3 2 7 2.76 7.36 2.35 0.034 1.09 -5 0 1 3.65 0.01 2.34 0.001 1.01 -2 -2 2 439.85 392.07 2.31 0.247 2.19 -2 -3 17 32.50 19.30 2.30 0.055 0.79 5 -2 6 3.64 0.04 2.30 0.003 0.85 -1 -6 10 65.32 46.48 2.30 0.085 0.84 Bond lengths and angles C1 - Distance Angles C7 1.4870 (0.0025) C6 1.5242 (0.0027) 111.78 (0.16) C2 1.5364 (0.0028) 111.70 (0.16) 110.58 (0.16) H1 1.0000 107.52 107.52 107.52 C1 - C7 C6 C2 C2 - Distance Angles C3 1.5312 (0.0027) C1 1.5364 (0.0028) 110.29 (0.17) H2A 0.9900 109.60 109.60 H2B 0.9900 109.60 109.60 108.13 C2 - C3 C1 H2A C3 - Distance Angles C4 1.5237 (0.0033) C2 1.5312 (0.0027) 111.71 (0.18) H3A 0.9900 109.28 109.28 H3B 0.9900 109.28 109.28 107.94 C3 - C4 C2 H3A C4 - Distance Angles C5 1.5220 (0.0034) C3 1.5237 (0.0033) 111.40 (0.18) H4A 0.9900 109.35 109.35 H4B 0.9900 109.35 109.35 107.98 C4 - C5 C3 H4A C5 - Distance Angles C4 1.5220 (0.0034) C6 1.5286 (0.0028) 111.65 (0.18) H5A 0.9900 109.29 109.29 H5B 0.9900 109.29 109.29 107.95 C5 - C4 C6 H5A C6 - Distance Angles C1 1.5242 (0.0027) C5 1.5286 (0.0028) 109.95 (0.16) H6A 0.9900 109.67 109.67 H6B 0.9900 109.67 109.67 108.17 C6 - C1 C5 H6A C7 - Distance Angles N11 1.2838 (0.0024) O8 1.3884 (0.0023) 113.56 (0.16) C1 1.4870 (0.0025) 130.52 (0.18) 115.92 (0.15) C7 - N11 O8 C9 - Distance Angles N12 1.3270 (0.0025) O8 1.3640 (0.0022) 117.89 (0.16) C10 1.3727 (0.0027) 135.01 (0.18) 107.10 (0.16) C9 - N12 O8 C10 - Distance Angles C9 1.3727 (0.0027) N11 1.4115 (0.0024) 109.11 (0.16) C13 1.4142 (0.0026) 127.88 (0.18) 123.00 (0.17) C10 - C9 N11 C13 - Distance Angles N14 1.1493 (0.0025) C10 1.4142 (0.0026) 178.74 (0.21) C13 - N14 N11 - Distance Angles C7 1.2838 (0.0024) C10 1.4115 (0.0024) 104.81 (0.16) N11 - C7 N12 - Distance Angles C9 1.3270 (0.0025) H12B 0.8716 (0.0156) 120.72 (1.49) H12A 0.8868 (0.0162) 119.51 (1.62) 119.44 (2.21) N12 - C9 H12B N14 - Distance Angles C13 1.1493 (0.0025) N14 - O8 - Distance Angles C9 1.3640 (0.0022) C7 1.3884 (0.0023) 105.42 (0.14) O8 - C9 Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.872(16) 2.172(17) 3.017(2) 163(2) N12-H12B...N11_$1 0.887(16) 2.118(17) 2.995(2) 170(2) N12-H12A...N14_$2 FMAP and GRID set by program FMAP 2 1 29 GRID -3.846 -2 -1 3.846 2 1 R1 = 0.0795 for 2205 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.29 at 0.4774 0.6198 0.2683 [ 0.73 A from C6 ] Deepest hole -0.28 at 0.7606 0.4895 0.2392 [ 1.05 A from C7 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 1926 / 22892 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4774 0.6198 0.2683 1.00000 0.05 0.29 0.73 C6 0.80 C1 1.37 H6B 1.43 H6A Q2 1 0.5395 0.4213 0.3078 1.00000 0.05 0.27 0.80 C2 0.82 C1 1.30 H2B 1.46 H2A Q3 1 1.1151 0.1433 0.1582 1.00000 0.05 0.23 0.95 C10 1.18 C9 1.85 N11 1.94 C13 Q4 1 0.0756 0.8656 0.4996 1.00000 0.05 0.20 0.86 H4A 1.46 C4 1.51 H4B 1.95 H4A Q5 1 0.3538 0.7978 0.3082 1.00000 0.05 0.20 0.73 C6 0.85 C5 1.28 H6B 1.47 H5A Q6 1 1.3144 0.4197 0.0397 1.00000 0.05 0.20 1.04 N14 1.07 C13 2.21 C10 2.26 H12A Q7 1 1.1085 -0.1185 0.1516 1.00000 0.05 0.19 0.94 N12 1.22 C9 1.36 H12B 1.43 H12A Q8 1 -0.0005 0.9487 0.2372 1.00000 0.05 0.19 1.14 H5B 1.71 O8 1.82 C9 1.84 C5 Q9 1 0.1599 0.6637 0.2030 1.00000 0.05 0.18 1.32 H1 1.68 H12B 1.91 H5B 1.96 N12 Q10 1 1.0412 -0.2438 0.1442 1.00000 0.05 0.18 0.55 H12B 0.89 N12 1.48 H12A 1.85 C9 Shortest distances between peaks (including symmetry equivalents) 7 10 0.97 9 10 1.18 1 5 1.23 1 2 1.30 7 8 1.42 7 9 1.49 4 4 1.58 3 7 1.63 8 9 1.75 8 10 1.85 3 8 1.89 1 9 2.02 2 5 2.19 5 8 2.22 5 9 2.34 3 10 2.56 6 10 2.62 6 6 2.71 2 9 2.75 1 8 2.78 5 7 2.83 3 6 2.84 1 7 2.87 6 9 2.90 3 9 2.93 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. 0.41: 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 0.20: Structure factors and derivatives 0.33: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.05: Solve l.s. equations 0.00: Generate HTAB table 0.08: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0459 finished at 12:03:08 Total CPU time: 1.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++