+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0464p21n started at 10:42:26 on 27-Apr-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0464p21n in P2(1)/n CELL 0.71073 8.1049 6.1023 17.6777 90.000 92.219 90.000 ZERR 4.00 0.0002 0.0002 0.0005 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O F UNIT 40 24 12 4 4 V = 873.66 F(000) = 416.0 Mu = 0.12 mm-1 Cell Wt = 812.71 Rho = 1.545 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 DFIX 0.89 0.02 N12 H12a N12 H12b FMAP 2 PLAN 10 ACTA SIZE 0.24 0.13 0.06 EQIV_$1 x, y+1, z HTAB N12 N11_$1 EQIV_$2 -x+3, -y+1, -z+1 HTAB N12 N14_$2 BOND $H WGHT 0.05180 0.39470 L.S. 4 TEMP -153.00 FVAR 0.35382 MOLE 1 C1 1 0.466815 0.242963 0.293821 11.00000 0.01306 0.02724 = 0.02656 -0.00386 -0.00170 -0.00338 C2 1 0.528661 0.450612 0.282161 11.00000 0.01745 0.02382 = 0.02858 0.00165 -0.00359 0.00170 AFIX 43 H2 2 0.466550 0.556513 0.253821 11.00000 -1.20000 AFIX 0 C3 1 0.684490 0.500050 0.313126 11.00000 0.01811 0.01733 = 0.02440 -0.00005 -0.00043 -0.00061 AFIX 43 H3 2 0.729852 0.641852 0.306186 11.00000 -1.20000 AFIX 0 C4 1 0.774749 0.342469 0.354380 11.00000 0.01572 0.01689 = 0.01851 -0.00190 -0.00088 0.00071 C5 1 0.707717 0.134218 0.365019 11.00000 0.02083 0.01792 = 0.02145 0.00065 -0.00105 -0.00106 AFIX 43 H5 2 0.769020 0.027078 0.393150 11.00000 -1.20000 AFIX 0 C6 1 0.551809 0.083294 0.334619 11.00000 0.02043 0.02001 = 0.02567 -0.00084 0.00151 -0.00511 AFIX 43 H6 2 0.504955 -0.057568 0.341711 11.00000 -1.20000 AFIX 0 C7 1 0.939027 0.393418 0.386284 11.00000 0.01571 0.01210 = 0.02032 -0.00022 -0.00051 -0.00120 C9 1 1.138839 0.616669 0.422506 11.00000 0.01478 0.01794 = 0.01891 0.00036 -0.00218 -0.00009 C10 1 1.179731 0.403649 0.440220 11.00000 0.01546 0.01411 = 0.02155 0.00042 -0.00239 -0.00034 C13 1 1.322195 0.323508 0.479790 11.00000 0.01954 0.01208 = 0.02355 -0.00004 -0.00092 -0.00156 N11 3 1.049827 0.263851 0.415737 11.00000 0.01603 0.01446 = 0.02247 -0.00040 -0.00282 -0.00037 N12 3 1.211542 0.810256 0.430438 11.00000 0.01795 0.01505 = 0.03492 0.00150 -0.00776 -0.00078 N14 3 1.436212 0.254449 0.512813 11.00000 0.02172 0.01741 = 0.03282 0.00233 -0.00614 -0.00038 O8 4 0.984804 0.612492 0.387844 11.00000 0.01550 0.01431 = 0.02364 0.00119 -0.00373 -0.00077 F1 5 0.315173 0.193192 0.263240 11.00000 0.01630 0.03846 = 0.04562 -0.00018 -0.00924 -0.00769 H12A 2 1.151152 0.928880 0.422761 11.00000 0.03021 H12B 2 1.311050 0.813716 0.452003 11.00000 0.04175 HKLF 4 Covalent radii and connectivity table for 2009src0464p21n in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 C1 - F1 C6 C2 C2 - C1 C3 C3 - C2 C4 C4 - C3 C5 C7 C5 - C6 C4 C6 - C1 C5 C7 - N11 O8 C4 C9 - N12 O8 C10 C10 - C9 N11 C13 C13 - N14 C10 N11 - C7 C10 N12 - C9 N14 - C13 O8 - C9 C7 F1 - C1 Operators for generating equivalent atoms: $1 x, y+1, z $2 -x+3, -y+1, -z+1 19407 Reflections read, of which 1076 rejected -10 =< h =< 10, -7 =< k =< 7, -22 =< l =< 22, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) -1 5 10 20.66 0.51 4 9.14 1 Inconsistent equivalents 1992 Unique reflections, of which 0 suppressed R(int) = 0.0443 R(sigma) = 0.0274 Friedel opposites merged Maximum memory for data reduction = 1367 / 19686 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 = 1727 / 181913 wR2 = 0.1023 before cycle 1 for 1992 data and 144 / 144 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.023; Restrained GooF = 1.023 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0518 * P )^2 + 0.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.35370 0.00089 -0.140 OSF Mean shift/su = 0.037 Maximum = -0.140 for OSF Max. shift = 0.001 A for H12A Max. dU = 0.000 for H12A Least-squares cycle 2 Maximum vector length = 511 Memory required = 1727 / 181913 wR2 = 0.1022 before cycle 2 for 1992 data and 144 / 144 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.023; Restrained GooF = 1.023 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0518 * P )^2 + 0.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.35363 0.00089 -0.073 OSF Mean shift/su = 0.013 Maximum = -0.073 for OSF Max. shift = 0.000 A for H12A Max. dU = 0.000 for H12A Least-squares cycle 3 Maximum vector length = 511 Memory required = 1727 / 181913 wR2 = 0.1023 before cycle 3 for 1992 data and 144 / 144 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.023; Restrained GooF = 1.023 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0518 * P )^2 + 0.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.35363 0.00089 -0.001 OSF Mean shift/su = 0.000 Maximum = -0.002 for U13 C3 Max. shift = 0.000 A for H12A Max. dU = 0.000 for H12B Least-squares cycle 4 Maximum vector length = 511 Memory required = 1727 / 181913 wR2 = 0.1023 before cycle 4 for 1992 data and 144 / 144 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.023; Restrained GooF = 1.023 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0518 * P )^2 + 0.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.35363 0.00089 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for U12 C2 Max. shift = 0.000 A for H12A Max. dU = 0.000 for H12B 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 0.4666 0.5565 0.2538 43 0.950 0.000 C2 C1 C3 H3 0.7298 0.6419 0.3062 43 0.950 0.000 C3 C2 C4 H5 0.7690 0.0271 0.3932 43 0.950 0.000 C5 C6 C4 H6 0.5050 -0.0576 0.3417 43 0.950 0.000 C6 C1 C5 2009src0464p21n in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.46683 0.24297 0.29382 1.00000 0.01299 0.02721 0.02648 -0.00386 -0.00171 -0.00340 0.02229 0.00229 0.00016 0.00024 0.00008 0.00000 0.00057 0.00073 0.00066 0.00053 0.00046 0.00050 0.00029 C2 0.52866 0.45059 0.28216 1.00000 0.01741 0.02377 0.02850 0.00163 -0.00356 0.00168 0.02334 0.00237 0.00016 0.00024 0.00008 0.00000 0.00061 0.00070 0.00070 0.00054 0.00050 0.00052 0.00030 H2 0.46655 0.55648 0.25382 1.00000 0.02801 0.00000 0.00000 C3 0.68449 0.50006 0.31313 1.00000 0.01803 0.01727 0.02436 -0.00007 -0.00043 -0.00057 0.01992 0.00224 0.00015 0.00021 0.00007 0.00000 0.00060 0.00065 0.00063 0.00049 0.00048 0.00046 0.00028 H3 0.72985 0.64186 0.30619 1.00000 0.02390 0.00000 0.00000 C4 0.77475 0.34245 0.35438 1.00000 0.01569 0.01680 0.01846 -0.00192 -0.00089 0.00069 0.01702 0.00214 0.00015 0.00021 0.00007 0.00000 0.00059 0.00063 0.00058 0.00047 0.00045 0.00046 0.00027 C5 0.70772 0.13423 0.36502 1.00000 0.02078 0.01789 0.02139 0.00065 -0.00102 -0.00104 0.02007 0.00226 0.00016 0.00022 0.00007 0.00000 0.00063 0.00065 0.00061 0.00048 0.00048 0.00049 0.00028 H5 0.76902 0.02709 0.39315 1.00000 0.02408 0.00000 0.00000 C6 0.55181 0.08331 0.33462 1.00000 0.02041 0.01999 0.02562 -0.00086 0.00156 -0.00511 0.02199 0.00228 0.00016 0.00023 0.00007 0.00000 0.00063 0.00066 0.00066 0.00052 0.00050 0.00050 0.00029 H6 0.50496 -0.05755 0.34171 1.00000 0.02638 0.00000 0.00000 C7 0.93902 0.39340 0.38628 1.00000 0.01571 0.01201 0.02027 -0.00022 -0.00050 -0.00120 0.01603 0.00213 0.00015 0.00020 0.00007 0.00000 0.00059 0.00060 0.00058 0.00044 0.00045 0.00043 0.00027 C9 1.13884 0.61666 0.42251 1.00000 0.01475 0.01785 0.01887 0.00036 -0.00219 -0.00007 0.01723 0.00215 0.00015 0.00021 0.00007 0.00000 0.00057 0.00064 0.00059 0.00046 0.00045 0.00045 0.00027 C10 1.17973 0.40364 0.44022 1.00000 0.01545 0.01409 0.02149 0.00041 -0.00239 -0.00029 0.01709 0.00212 0.00015 0.00020 0.00007 0.00000 0.00057 0.00061 0.00060 0.00046 0.00045 0.00045 0.00027 C13 1.32221 0.32351 0.47980 1.00000 0.01948 0.01204 0.02351 -0.00005 -0.00091 -0.00157 0.01839 0.00217 0.00015 0.00020 0.00007 0.00000 0.00062 0.00059 0.00063 0.00048 0.00049 0.00047 0.00027 N11 1.04983 0.26385 0.41574 1.00000 0.01602 0.01444 0.02241 -0.00039 -0.00279 -0.00038 0.01771 0.00182 0.00012 0.00018 0.00006 0.00000 0.00051 0.00055 0.00055 0.00040 0.00040 0.00038 0.00025 N12 1.21154 0.81027 0.43043 1.00000 0.01792 0.01497 0.03487 0.00147 -0.00775 -0.00081 0.02281 0.00200 0.00014 0.00019 0.00007 0.00000 0.00055 0.00058 0.00065 0.00046 0.00046 0.00043 0.00027 N14 1.43622 0.25444 0.51281 1.00000 0.02172 0.01736 0.03273 0.00233 -0.00611 -0.00037 0.02412 0.00200 0.00014 0.00019 0.00007 0.00000 0.00057 0.00056 0.00064 0.00046 0.00046 0.00045 0.00027 O8 0.98481 0.61249 0.38784 1.00000 0.01544 0.01423 0.02359 0.00119 -0.00375 -0.00078 0.01787 0.00148 0.00010 0.00014 0.00005 0.00000 0.00044 0.00047 0.00046 0.00034 0.00034 0.00033 0.00022 F1 0.31517 0.19319 0.26324 1.00000 0.01625 0.03845 0.04557 -0.00017 -0.00923 -0.00769 0.03369 0.00147 0.00010 0.00016 0.00005 0.00000 0.00041 0.00054 0.00053 0.00041 0.00035 0.00035 0.00025 H12A 1.15112 0.92894 0.42281 1.00000 0.03010 0.02930 0.00193 0.00260 0.00091 0.00000 0.00436 H12B 1.31112 0.81370 0.45200 1.00000 0.04181 0.02953 0.00197 0.00329 0.00105 0.00000 0.00515 Final Structure Factor Calculation for 2009src0464p21n in P2(1)/n Total number of l.s. parameters = 144 Maximum vector length = 511 Memory required = 1583 / 24017 wR2 = 0.1023 before cycle 5 for 1992 data and 0 / 144 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.023; Restrained GooF = 1.023 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0518 * P )^2 + 0.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0396 for 1732 Fo > 4sig(Fo) and 0.0466 for all 1992 data wR2 = 0.1023, GooF = S = 1.023, Restrained GooF = 1.023 for all data Occupancy sum of asymmetric unit = 15.00 for non-hydrogen and 6.00 for hydrogen atoms Principal mean square atomic displacements U 0.0307 0.0245 0.0116 C1 0.0304 0.0242 0.0155 C2 0.0246 0.0182 0.0169 C3 0.0204 0.0156 0.0150 C4 0.0233 0.0194 0.0176 C5 0.0265 0.0244 0.0151 C6 0.0206 0.0158 0.0116 C7 0.0205 0.0178 0.0134 C9 0.0230 0.0143 0.0140 C10 0.0243 0.0192 0.0117 C13 0.0241 0.0150 0.0140 N11 0.0391 0.0149 0.0144 N12 0.0368 0.0187 0.0168 N14 0.0260 0.0142 0.0135 O8 0.0499 0.0399 0.0113 F1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.025 0.039 0.054 0.070 0.089 0.115 0.153 0.224 1.000 Number in group 206. 201. 198. 203. 190. 197. 203. 195. 199. 200. GooF 1.039 1.047 1.001 0.997 1.016 1.107 1.013 0.983 1.013 1.010 K 2.125 1.113 0.972 0.995 0.980 0.997 1.006 1.005 1.015 0.990 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.64 inf Number in group 206. 201. 193. 197. 205. 197. 196. 201. 196. 200. GooF 1.055 1.047 0.944 1.021 0.957 0.886 0.841 0.842 1.033 1.459 K 1.003 1.053 1.031 1.035 1.012 0.993 1.006 1.005 1.031 0.968 R1 0.100 0.088 0.084 0.064 0.050 0.039 0.029 0.028 0.031 0.037 Recommended weighting scheme: WGHT 0.0506 0.4040 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) 3 1 3 10.77 3.49 4.47 0.021 2.25 2 2 6 72.63 50.48 3.87 0.079 1.86 -10 0 4 3.94 12.41 3.73 0.039 0.80 -1 1 7 60.29 41.36 3.71 0.071 2.26 0 1 1 2454.73 2981.93 3.49 0.604 5.77 -3 2 3 42.15 28.29 3.42 0.059 1.93 -5 2 6 3.02 0.12 3.38 0.004 1.30 4 2 1 6.18 2.28 3.10 0.017 1.67 0 4 0 221.95 178.96 3.05 0.148 1.53 8 1 7 0.55 6.98 2.96 0.029 0.92 0 3 2 3.92 0.94 2.95 0.011 1.98 -3 6 2 48.65 34.73 2.88 0.065 0.95 -1 1 4 6903.33 8168.67 2.87 1.000 3.31 2 3 1 83.44 106.76 2.87 0.114 1.80 6 3 12 96.16 73.54 2.84 0.095 0.88 6 1 8 82.16 105.71 2.84 0.114 1.11 -2 1 2 9.57 4.85 2.81 0.024 3.19 -4 1 2 11.45 19.00 2.80 0.048 1.89 -3 5 1 10.95 18.75 2.79 0.048 1.11 8 0 12 292.76 216.41 2.77 0.163 0.82 3 5 6 5.66 11.80 2.76 0.038 1.03 -4 3 19 40.97 57.58 2.74 0.084 0.79 -1 1 6 8.52 4.08 2.70 0.022 2.55 4 5 9 99.01 124.53 2.67 0.123 0.92 -3 3 4 29.89 41.47 2.66 0.071 1.54 4 7 0 444.43 360.17 2.65 0.210 0.80 3 6 7 6.85 0.88 2.62 0.010 0.89 3 3 3 85.66 68.08 2.62 0.091 1.56 1 1 0 1882.21 2179.72 2.61 0.517 4.87 6 2 11 37.89 50.92 2.59 0.079 0.96 3 3 1 220.35 185.20 2.59 0.151 1.61 1 1 4 445.01 521.62 2.58 0.253 3.24 -1 4 5 232.63 195.86 2.53 0.155 1.38 -4 6 7 74.65 57.41 2.51 0.084 0.86 -3 5 4 14.37 8.54 2.50 0.032 1.08 6 1 5 193.46 230.47 2.49 0.168 1.22 4 2 0 77.27 61.88 2.47 0.087 1.69 8 0 10 68.18 48.89 2.47 0.077 0.86 3 7 5 265.56 212.02 2.47 0.161 0.81 3 6 12 19.38 31.42 2.46 0.062 0.79 8 0 8 7.71 0.00 2.45 0.001 0.91 2 1 6 492.97 425.81 2.44 0.228 2.18 -4 1 7 19.59 13.03 2.44 0.040 1.56 -4 6 6 -2.46 1.79 2.42 0.015 0.87 1 3 1 2.54 0.40 2.42 0.007 1.96 6 0 6 60.48 46.67 2.42 0.076 1.21 0 7 8 10.98 19.84 2.41 0.049 0.81 2 5 17 11.53 20.04 2.39 0.050 0.77 2 6 3 5.04 1.73 2.39 0.015 0.97 0 4 5 131.07 157.40 2.39 0.139 1.40 Bond lengths and angles C1 - Distance Angles F1 1.3579 (0.0015) C6 1.3803 (0.0020) 118.41 (0.12) C2 1.3809 (0.0020) 118.29 (0.12) 123.30 (0.12) C1 - F1 C6 C2 - Distance Angles C1 1.3809 (0.0020) C3 1.3901 (0.0018) 118.03 (0.13) H2 0.9500 120.99 120.99 C2 - C1 C3 C3 - Distance Angles C2 1.3901 (0.0018) C4 1.3966 (0.0018) 120.37 (0.12) H3 0.9500 119.81 119.81 C3 - C2 C4 C4 - Distance Angles C3 1.3966 (0.0018) C5 1.3975 (0.0018) 119.86 (0.11) C7 1.4592 (0.0017) 120.44 (0.12) 119.69 (0.11) C4 - C3 C5 C5 - Distance Angles C6 1.3891 (0.0018) C4 1.3975 (0.0018) 120.26 (0.12) H5 0.9500 119.87 119.87 C5 - C6 C4 C6 - Distance Angles C1 1.3803 (0.0020) C5 1.3891 (0.0018) 118.18 (0.12) H6 0.9500 120.91 120.91 C6 - C1 C5 C7 - Distance Angles N11 1.2909 (0.0016) O8 1.3875 (0.0015) 113.62 (0.10) C4 1.4592 (0.0017) 129.46 (0.12) 116.89 (0.10) C7 - N11 O8 C9 - Distance Angles N12 1.3253 (0.0017) O8 1.3695 (0.0015) 117.24 (0.11) C10 1.3746 (0.0018) 135.79 (0.12) 106.97 (0.10) C9 - N12 O8 C10 - Distance Angles C9 1.3746 (0.0018) N11 1.4100 (0.0016) 109.37 (0.11) C13 1.4141 (0.0017) 128.66 (0.12) 121.90 (0.11) C10 - C9 N11 C13 - Distance Angles N14 1.1534 (0.0017) C10 1.4141 (0.0017) 178.42 (0.14) C13 - N14 N11 - Distance Angles C7 1.2909 (0.0016) C10 1.4100 (0.0016) 104.64 (0.11) N11 - C7 N12 - Distance Angles C9 1.3253 (0.0017) H12A 0.8816 (0.0142) 118.29 (1.12) H12B 0.8793 (0.0148) 117.64 (1.33) 122.81 (1.78) N12 - C9 H12A N14 - Distance Angles C13 1.1534 (0.0017) N14 - O8 - Distance Angles C9 1.3695 (0.0015) C7 1.3875 (0.0015) 105.38 (0.09) O8 - C9 F1 - Distance Angles C1 1.3579 (0.0015) F1 - Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.882(14) 2.204(15) 3.0692(16) 166.8(15) N12-H12A...N11_$1 0.879(15) 2.157(16) 3.0151(16) 164.9(18) N12-H12B...N14_$2 FMAP and GRID set by program FMAP 2 2 10 GRID -3.571 -2 -2 3.571 2 2 R1 = 0.0466 for 1992 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.23 at 0.0193 0.1105 0.6142 [ 1.52 A from H12A ] Deepest hole -0.26 at 0.5123 0.0572 0.8983 [ 0.69 A from C7 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 1874 / 16070 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9807 0.8895 0.3858 1.00000 0.05 0.23 1.52 H12A 1.69 O8 1.92 H5 2.06 N12 Q2 1 0.8619 0.3595 0.3674 1.00000 0.05 0.20 0.73 C7 0.74 C4 1.81 N11 1.86 C5 Q3 1 0.5329 0.1675 0.3009 1.00000 0.05 0.19 0.71 C1 0.80 C6 1.57 H6 1.76 C2 Q4 1 0.6450 0.1077 0.3442 1.00000 0.05 0.19 0.64 C5 0.78 C6 1.39 H5 1.52 H6 Q5 1 1.0514 0.1096 0.4192 1.00000 0.05 0.18 0.94 N11 1.37 H12A 2.03 C7 2.10 C10 Q6 1 1.1881 1.1275 0.4366 1.00000 0.05 0.18 1.27 H12A 1.43 N11 1.69 C10 1.77 C13 Q7 1 1.1779 0.5099 0.4188 1.00000 0.05 0.17 0.73 C9 0.75 C10 1.75 O8 1.83 N11 Q8 1 1.1269 0.3132 0.4256 1.00000 0.05 0.17 0.71 N11 0.74 C10 1.72 C7 1.82 C13 Q9 1 0.6877 -0.0097 0.3115 1.00000 0.05 0.17 1.30 C5 1.32 C6 1.58 H5 1.62 H6 Q10 1 0.7735 0.2099 0.3399 1.00000 0.05 0.17 0.84 C5 0.85 C4 1.46 H5 1.91 C7 Shortest distances between peaks (including symmetry equivalents) 4 9 0.99 5 6 1.14 4 10 1.22 3 4 1.22 2 10 1.25 6 8 1.25 7 8 1.28 5 8 1.39 1 5 1.57 9 10 1.58 3 9 1.66 3 10 2.06 2 5 2.33 6 7 2.36 2 4 2.36 2 8 2.36 1 6 2.37 5 7 2.65 5 10 2.68 1 10 2.68 1 9 2.74 2 9 2.82 2 7 2.84 1 7 2.86 1 8 2.92 Time profile in seconds ----------------------- 0.02: 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. 0.89: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.30: Structure factors and derivatives 0.27: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0464p21n finished at 10:42:28 Total CPU time: 1.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++