+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 05src0055 started at 23:00:50 on 22-Jan-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 05src0055 in Pbca CELL 0.71073 14.1438 12.9258 14.7767 90.000 90.000 90.000 ZERR 8.00 0.0015 0.0012 0.0008 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 S UNIT 96 80 48 V = 2701.48 F(000) = 1424.0 Mu = 0.99 mm-1 Cell Wt = 2772.48 Rho = 1.704 MERG 2 OMIT -3.00 55.00 OMIT 1 0 2 OMIT 2 1 0 OMIT 0 2 1 OMIT 8 0 0 FMAP 2 PLAN 20 SIZE 0.15 0.25 0.38 ACTA BOND $H WGHT 0.02690 3.04830 L.S. 4 TEMP -153.00 FVAR 0.37575 C1 1 0.135657 0.622509 0.462994 11.00000 0.01502 0.01342 = 0.01398 -0.00239 0.00046 -0.00001 C2 1 0.154790 0.696878 0.532500 11.00000 0.01372 0.01893 = 0.01417 -0.00345 -0.00003 -0.00071 C3 1 0.112571 0.552095 0.655636 11.00000 0.02313 0.02457 = 0.01582 -0.00112 0.00464 -0.00335 AFIX 23 H3A 2 0.114336 0.528918 0.719470 11.00000 -1.20000 H3B 2 0.046848 0.573042 0.641656 11.00000 -1.20000 AFIX 0 C4 1 0.139864 0.462395 0.595030 11.00000 0.03238 0.02123 = 0.01520 0.00159 0.00147 0.00029 AFIX 23 H4A 2 0.093443 0.406102 0.604497 11.00000 -1.20000 H4B 2 0.202181 0.436249 0.615220 11.00000 -1.20000 AFIX 0 C5 1 0.109656 0.668352 0.382479 11.00000 0.01233 0.01134 = 0.01579 -0.00209 0.00153 0.00064 C6 1 0.143988 0.796256 0.503497 11.00000 0.01658 0.01711 = 0.01734 -0.00648 0.00015 -0.00056 AFIX 43 H6 2 0.153133 0.855250 0.540828 11.00000 -1.20000 AFIX 0 C7 1 0.084968 0.619222 0.296845 11.00000 0.01377 0.00993 = 0.01340 0.00044 0.00189 -0.00066 C8 1 0.080377 0.502723 0.163493 11.00000 0.02135 0.01335 = 0.01108 -0.00134 -0.00025 -0.00053 AFIX 43 H8 2 0.089211 0.451328 0.118320 11.00000 -1.20000 AFIX 0 C9 1 0.013577 0.643949 0.237208 11.00000 0.01358 0.01016 = 0.01581 0.00129 0.00122 -0.00115 C10 1 0.010406 0.575307 0.161046 11.00000 0.01658 0.01231 = 0.01286 0.00107 0.00032 -0.00201 C11 1 -0.116568 0.705549 0.080482 11.00000 0.02256 0.01880 = 0.02410 0.00241 -0.00814 0.00208 AFIX 23 H11A 2 -0.063465 0.751516 0.063504 11.00000 -1.20000 H11B 2 -0.167754 0.715450 0.035612 11.00000 -1.20000 AFIX 0 C12 1 -0.152349 0.735660 0.173263 11.00000 0.01515 0.02189 = 0.02805 -0.00068 -0.00457 0.00210 AFIX 23 H12A 2 -0.196425 0.681620 0.195041 11.00000 -1.20000 H12B 2 -0.188271 0.801144 0.168241 11.00000 -1.20000 AFIX 0 S1 3 0.189527 0.663209 0.642698 11.00000 0.02396 0.02366 = 0.01434 -0.00294 -0.00388 -0.00333 S2 3 0.146832 0.488094 0.475001 11.00000 0.08403 0.01311 = 0.01390 -0.00001 0.00040 0.00669 S5 3 -0.077222 0.572895 0.076944 11.00000 0.02389 0.01855 = 0.01889 -0.00283 -0.00782 0.00091 S6 3 -0.059141 0.752189 0.255649 11.00000 0.01763 0.01528 = 0.02245 -0.00349 -0.00364 0.00474 S3 3 0.112047 0.802293 0.392039 11.00000 0.02252 0.01090 = 0.01776 -0.00271 -0.00151 0.00071 S4 3 0.150298 0.514920 0.257191 11.00000 0.01777 0.01311 = 0.01369 -0.00239 -0.00111 0.00386 HKLF 4 1.0 0.00 1.00 0.00 1.00 0.00 0.00 0.00 0.00 -1.00 Covalent radii and connectivity table for 05src0055 in Pbca C 0.770 H 0.320 S 1.030 C1 - C5 C2 S2 C2 - C6 C1 S1 C3 - C4 S1 C4 - C3 S2 C5 - C1 C7 S3 C6 - C2 S3 C7 - C9 C5 S4 C8 - C10 S4 C9 - C7 C10 S6 C10 - C8 C9 S5 C11 - C12 S5 C12 - C11 S6 S1 - C2 C3 S2 - C1 C4 S5 - C10 C11 S6 - C9 C12 S3 - C6 C5 S4 - C8 C7 h k l Fo^2 Sigma Why rejected 9 0 0 12.96 3.18 observed but should be systematically absent 3 0 1 4.85 1.11 observed but should be systematically absent 0 1 5 0.90 0.22 observed but should be systematically absent 29229 Reflections read, of which 2115 rejected -18 =< h =< 18, -16 =< k =< 16, -17 =< l =< 19, Max. 2-theta = 54.98 3 Systematic absence violations 0 Inconsistent equivalents 3096 Unique reflections, of which 0 suppressed R(int) = 0.0345 R(sigma) = 0.0213 Friedel opposites merged Maximum memory for data reduction = 1605 / 30945 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 = 2032 / 202251 wR2 = 0.0660 before cycle 1 for 3096 data and 163 / 163 parameters GooF = S = 1.019; Restrained GooF = 1.019 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0269 * P )^2 + 3.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.37569 0.00046 -0.127 OSF Mean shift/esd = 0.026 Maximum = -0.127 for OSF Max. shift = 0.000 A for C7 Max. dU = 0.000 for C11 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2032 / 202251 wR2 = 0.0661 before cycle 2 for 3096 data and 163 / 163 parameters GooF = S = 1.020; Restrained GooF = 1.020 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0269 * P )^2 + 3.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.37566 0.00046 -0.078 OSF Mean shift/esd = 0.009 Maximum = -0.078 for OSF Max. shift = 0.000 A for C7 Max. dU = 0.000 for C11 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2032 / 202251 wR2 = 0.0660 before cycle 3 for 3096 data and 163 / 163 parameters GooF = S = 1.020; Restrained GooF = 1.020 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0269 * P )^2 + 3.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.37566 0.00046 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z S1 Max. shift = 0.000 A for H11B Max. dU = 0.000 for C12 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2032 / 202251 wR2 = 0.0661 before cycle 4 for 3096 data and 163 / 163 parameters GooF = S = 1.020; Restrained GooF = 1.020 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0269 * P )^2 + 3.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.37566 0.00046 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for y S6 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C2 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 H3A 0.1143 0.5289 0.7195 23 0.990 0.000 C3 C4 S1 H3B 0.0468 0.5730 0.6416 23 0.990 0.000 C3 C4 S1 H4A 0.0934 0.4061 0.6045 23 0.990 0.000 C4 C3 S2 H4B 0.2022 0.4363 0.6152 23 0.990 0.000 C4 C3 S2 H6 0.1531 0.8553 0.5408 43 0.950 0.000 C6 C2 S3 H8 0.0892 0.4513 0.1183 43 0.950 0.000 C8 C10 S4 H11A -0.0635 0.7515 0.0635 23 0.990 0.000 C11 C12 S5 H11B -0.1677 0.7155 0.0356 23 0.990 0.000 C11 C12 S5 H12A -0.1964 0.6816 0.1950 23 0.990 0.000 C12 C11 S6 H12B -0.1883 0.8012 0.1682 23 0.990 0.000 C12 C11 S6 05src0055 in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.13566 0.62251 0.46299 1.00000 0.01499 0.01339 0.01398 -0.00241 0.00045 0.00000 0.01412 0.00286 0.00012 0.00013 0.00011 0.00000 0.00081 0.00080 0.00078 0.00066 0.00062 0.00064 0.00033 C2 0.15478 0.69688 0.53250 1.00000 0.01368 0.01889 0.01414 -0.00345 -0.00004 -0.00069 0.01557 0.00294 0.00012 0.00014 0.00011 0.00000 0.00078 0.00087 0.00078 0.00069 0.00062 0.00067 0.00034 C3 0.11257 0.55210 0.65563 1.00000 0.02310 0.02459 0.01582 -0.00112 0.00467 -0.00336 0.02117 0.00322 0.00013 0.00015 0.00012 0.00000 0.00093 0.00098 0.00083 0.00076 0.00070 0.00078 0.00039 H3A 0.11433 0.52892 0.71947 1.00000 0.02540 0.00000 0.00000 H3B 0.04685 0.57305 0.64165 1.00000 0.02540 0.00000 0.00000 C4 0.13987 0.46240 0.59503 1.00000 0.03234 0.02123 0.01519 0.00160 0.00146 0.00029 0.02292 0.00340 0.00015 0.00015 0.00012 0.00000 0.00105 0.00093 0.00085 0.00076 0.00075 0.00081 0.00040 H4A 0.09345 0.40610 0.60450 1.00000 0.02751 0.00000 0.00000 H4B 0.20218 0.43626 0.61522 1.00000 0.02751 0.00000 0.00000 C5 0.10966 0.66835 0.38248 1.00000 0.01231 0.01132 0.01577 -0.00208 0.00152 0.00064 0.01313 0.00284 0.00011 0.00013 0.00011 0.00000 0.00076 0.00078 0.00079 0.00065 0.00061 0.00063 0.00033 C6 0.14398 0.79626 0.50349 1.00000 0.01656 0.01712 0.01729 -0.00648 0.00014 -0.00056 0.01699 0.00300 0.00012 0.00014 0.00012 0.00000 0.00083 0.00087 0.00082 0.00070 0.00066 0.00067 0.00035 H6 0.15313 0.85526 0.54083 1.00000 0.02039 0.00000 0.00000 C7 0.08498 0.61923 0.29685 1.00000 0.01375 0.00993 0.01337 0.00045 0.00190 -0.00067 0.01235 0.00282 0.00011 0.00013 0.00011 0.00000 0.00073 0.00075 0.00076 0.00064 0.00061 0.00061 0.00032 C8 0.08038 0.50273 0.16349 1.00000 0.02134 0.01330 0.01107 -0.00131 -0.00023 -0.00052 0.01524 0.00296 0.00012 0.00013 0.00011 0.00000 0.00084 0.00080 0.00075 0.00065 0.00065 0.00068 0.00034 H8 0.08923 0.45134 0.11831 1.00000 0.01829 0.00000 0.00000 C9 0.01358 0.64395 0.23721 1.00000 0.01355 0.01013 0.01580 0.00130 0.00119 -0.00114 0.01316 0.00286 0.00012 0.00013 0.00011 0.00000 0.00076 0.00075 0.00079 0.00064 0.00062 0.00061 0.00032 C10 0.01040 0.57530 0.16105 1.00000 0.01659 0.01229 0.01282 0.00107 0.00033 -0.00200 0.01390 0.00285 0.00012 0.00013 0.00011 0.00000 0.00079 0.00077 0.00074 0.00065 0.00062 0.00064 0.00033 C11 -0.11657 0.70555 0.08049 1.00000 0.02251 0.01879 0.02404 0.00240 -0.00814 0.00210 0.02178 0.00326 0.00014 0.00015 0.00013 0.00000 0.00091 0.00092 0.00094 0.00076 0.00074 0.00075 0.00039 H11A -0.06346 0.75152 0.06351 1.00000 0.02614 0.00000 0.00000 H11B -0.16775 0.71546 0.03561 1.00000 0.02614 0.00000 0.00000 C12 -0.15235 0.73567 0.17326 1.00000 0.01510 0.02189 0.02806 -0.00070 -0.00458 0.00209 0.02168 0.00321 0.00013 0.00015 0.00013 0.00000 0.00081 0.00093 0.00098 0.00080 0.00072 0.00073 0.00039 H12A -0.19643 0.68163 0.19504 1.00000 0.02602 0.00000 0.00000 H12B -0.18826 0.80116 0.16824 1.00000 0.02602 0.00000 0.00000 S1 0.18953 0.66321 0.64270 1.00000 0.02392 0.02364 0.01432 -0.00294 -0.00388 -0.00333 0.02063 0.00076 0.00003 0.00004 0.00003 0.00000 0.00023 0.00024 0.00021 0.00018 0.00017 0.00019 0.00011 S2 0.14683 0.48809 0.47500 1.00000 0.08399 0.01310 0.01388 -0.00001 0.00039 0.00668 0.03699 0.00105 0.00005 0.00004 0.00003 0.00000 0.00047 0.00024 0.00023 0.00019 0.00025 0.00026 0.00016 S5 -0.07722 0.57289 0.07694 1.00000 0.02386 0.01853 0.01886 -0.00283 -0.00783 0.00092 0.02042 0.00076 0.00003 0.00004 0.00003 0.00000 0.00023 0.00023 0.00022 0.00018 0.00017 0.00018 0.00011 S6 -0.05914 0.75219 0.25565 1.00000 0.01760 0.01525 0.02243 -0.00349 -0.00364 0.00474 0.01843 0.00076 0.00003 0.00003 0.00003 0.00000 0.00021 0.00021 0.00022 0.00018 0.00017 0.00017 0.00011 S3 0.11205 0.80229 0.39204 1.00000 0.02249 0.01087 0.01774 -0.00271 -0.00152 0.00071 0.01703 0.00074 0.00003 0.00003 0.00003 0.00000 0.00022 0.00020 0.00021 0.00017 0.00017 0.00017 0.00010 S4 0.15030 0.51492 0.25719 1.00000 0.01774 0.01308 0.01367 -0.00239 -0.00111 0.00386 0.01483 0.00073 0.00003 0.00003 0.00003 0.00000 0.00020 0.00020 0.00020 0.00016 0.00015 0.00016 0.00010 Final Structure Factor Calculation for 05src0055 in Pbca Total number of l.s. parameters = 163 Maximum vector length = 511 Memory required = 1869 / 21973 wR2 = 0.0660 before cycle 5 for 3096 data and 0 / 163 parameters GooF = S = 1.020; Restrained GooF = 1.020 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0269 * P )^2 + 3.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0266 for 2684 Fo > 4sig(Fo) and 0.0340 for all 3096 data wR2 = 0.0660, GooF = S = 1.020, Restrained GooF = 1.020 for all data Occupancy sum of asymmetric unit = 18.00 for non-hydrogen and 10.00 for hydrogen atoms Principal mean square atomic displacements U 0.0162 0.0149 0.0112 C1 0.0208 0.0137 0.0122 C2 0.0285 0.0215 0.0135 C3 0.0325 0.0216 0.0147 C4 0.0169 0.0126 0.0099 C5 0.0237 0.0165 0.0107 C6 0.0155 0.0119 0.0096 C7 0.0214 0.0139 0.0105 C8 0.0164 0.0137 0.0094 C9 0.0174 0.0135 0.0109 C10 0.0315 0.0206 0.0133 C11 0.0297 0.0220 0.0133 C12 0.0272 0.0230 0.0117 S1 0.0846 0.0139 0.0125 S2 0.0301 0.0186 0.0126 S5 0.0269 0.0168 0.0115 S6 0.0231 0.0180 0.0099 S3 0.0206 0.0138 0.0101 S4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.017 0.033 0.052 0.074 0.095 0.121 0.155 0.194 0.265 1.000 Number in group 312. 310. 309. 325. 299. 312. 300. 311. 306. 312. GooF 0.950 1.037 1.085 1.060 0.998 1.009 1.046 1.003 1.014 0.992 K 0.931 0.891 0.950 0.967 0.976 0.989 0.994 1.010 1.012 0.999 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 317. 305. 310. 309. 307. 314. 306. 308. 310. 310. GooF 1.070 1.005 0.960 0.951 0.932 0.895 0.926 0.927 0.976 1.443 K 0.980 0.999 1.015 1.018 1.018 1.010 1.008 0.998 1.003 0.990 R1 0.078 0.055 0.045 0.046 0.039 0.031 0.027 0.019 0.019 0.024 Recommended weighting scheme: WGHT 0.0266 3.0700 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) 4 1 1 1.88 43.05 4.28 0.025 3.32 1 3 6 1261.79 974.66 4.25 0.120 2.11 10 10 8 86.98 224.80 3.83 0.058 0.85 13 4 12 103.74 212.42 3.66 0.056 0.79 6 4 1 641.26 482.33 3.65 0.085 1.89 18 0 2 332.39 522.19 3.42 0.088 0.78 7 3 11 206.45 126.30 3.41 0.043 1.08 7 2 3 721.08 911.05 3.40 0.116 1.80 17 5 1 198.59 329.16 3.23 0.070 0.79 2 5 1 61.73 119.35 3.20 0.042 2.40 15 7 1 400.10 554.13 3.18 0.091 0.84 14 2 8 119.88 210.90 3.18 0.056 0.88 1 5 7 114.15 187.08 3.16 0.053 1.62 4 6 2 99.33 51.36 3.11 0.028 1.79 2 4 0 28.48 3.76 3.07 0.007 2.94 12 9 8 73.90 167.70 3.06 0.050 0.82 0 6 5 -11.04 17.45 3.03 0.016 1.74 17 1 5 41.45 124.40 2.95 0.043 0.80 6 0 0 2600.20 2274.87 2.92 0.184 2.36 2 5 5 9918.34 10896.49 2.85 0.402 1.88 0 4 6 5249.16 5837.22 2.84 0.294 1.96 15 3 3 307.86 423.34 2.83 0.079 0.91 17 3 5 280.55 399.68 2.81 0.077 0.79 10 0 16 962.84 1237.31 2.81 0.135 0.77 14 2 12 51.86 125.67 2.81 0.043 0.78 6 9 0 1102.35 916.14 2.79 0.116 1.23 10 2 1 390.64 503.27 2.79 0.086 1.38 1 5 4 1843.48 2111.09 2.75 0.177 2.09 3 4 5 5430.95 6001.49 2.75 0.298 1.98 17 0 6 1924.57 2275.67 2.71 0.184 0.79 2 2 0 174.97 250.54 2.70 0.061 4.77 4 0 6 3493.31 3899.73 2.70 0.240 2.02 8 0 12 1181.02 990.28 2.69 0.121 1.01 13 2 10 461.82 590.09 2.69 0.093 0.87 4 4 5 4612.65 4165.34 2.68 0.248 1.86 2 3 6 1574.68 1367.96 2.67 0.142 2.05 6 3 3 726.93 599.26 2.67 0.094 1.91 10 11 2 156.24 244.07 2.66 0.060 0.90 13 3 13 850.16 1049.63 2.66 0.125 0.77 4 2 3 1310.51 1128.45 2.66 0.129 2.62 0 4 5 -3.87 9.48 2.64 0.012 2.18 7 1 2 503.06 622.72 2.63 0.096 1.93 6 8 0 2847.41 3211.50 2.63 0.218 1.33 14 6 0 2372.01 2031.68 2.62 0.173 0.91 2 4 2 1262.42 1459.93 2.61 0.147 2.73 1 7 7 819.80 976.20 2.60 0.120 1.38 11 1 7 1380.09 1188.92 2.59 0.133 1.09 1 4 1 710.04 588.40 2.58 0.093 3.08 15 4 4 55.46 120.47 2.58 0.042 0.88 2 0 2 13148.97 14503.51 2.57 0.463 5.11 Bond lengths and angles C1 - Distance Angles C5 1.3791 (0.0024) C2 1.4325 (0.0024) 112.37 (0.15) S2 1.7536 (0.0018) 122.48 (0.13) 125.12 (0.13) C1 - C5 C2 C2 - Distance Angles C6 1.3627 (0.0026) C1 1.4325 (0.0024) 112.70 (0.16) S1 1.7557 (0.0018) 123.83 (0.14) 123.46 (0.14) C2 - C6 C1 C3 - Distance Angles C4 1.5151 (0.0026) S1 1.8122 (0.0019) 113.02 (0.13) H3A 0.9900 108.98 108.98 H3B 0.9900 108.98 108.98 107.77 C3 - C4 S1 H3A C4 - Distance Angles C3 1.5151 (0.0026) S2 1.8071 (0.0019) 116.96 (0.14) H4A 0.9900 108.06 108.06 H4B 0.9900 108.06 108.06 107.28 C4 - C3 S2 H4A C5 - Distance Angles C1 1.3791 (0.0024) C7 1.4581 (0.0023) 128.72 (0.15) S3 1.7375 (0.0017) 110.66 (0.13) 120.61 (0.12) C5 - C1 C7 C6 - Distance Angles C2 1.3627 (0.0025) S3 1.7096 (0.0018) 112.06 (0.13) H6 0.9500 123.97 123.97 C6 - C2 S3 C7 - Distance Angles C9 1.3779 (0.0023) C5 1.4581 (0.0023) 129.01 (0.15) S4 1.7363 (0.0017) 110.75 (0.12) 120.24 (0.12) C7 - C9 C5 C8 - Distance Angles C10 1.3642 (0.0024) S4 1.7087 (0.0017) 112.21 (0.13) H8 0.9500 123.90 123.90 C8 - C10 S4 C9 - Distance Angles C7 1.3779 (0.0023) C10 1.4339 (0.0023) 112.42 (0.15) S6 1.7577 (0.0017) 120.95 (0.13) 126.58 (0.13) C9 - C7 C10 C10 - Distance Angles C8 1.3642 (0.0024) C9 1.4339 (0.0023) 112.46 (0.15) S5 1.7554 (0.0017) 121.25 (0.13) 126.07 (0.13) C10 - C8 C9 C11 - Distance Angles C12 1.5123 (0.0027) S5 1.8035 (0.0019) 111.98 (0.13) H11A 0.9900 109.22 109.22 H11B 0.9900 109.22 109.22 107.91 C11 - C12 S5 H11A C12 - Distance Angles C11 1.5123 (0.0027) S6 1.8071 (0.0019) 113.39 (0.13) H12A 0.9900 108.89 108.89 H12B 0.9900 108.89 108.89 107.73 C12 - C11 S6 H12A S1 - Distance Angles C2 1.7557 (0.0018) C3 1.8122 (0.0019) 97.25 (0.09) S1 - C2 S2 - Distance Angles C1 1.7536 (0.0018) C4 1.8071 (0.0019) 106.05 (0.09) S2 - C1 S5 - Distance Angles C10 1.7554 (0.0017) C11 1.8035 (0.0019) 100.40 (0.08) S5 - C10 S6 - Distance Angles C9 1.7577 (0.0017) C12 1.8071 (0.0019) 103.20 (0.08) S6 - C9 S3 - Distance Angles C6 1.7096 (0.0018) C5 1.7375 (0.0017) 92.18 (0.09) S3 - C6 S4 - Distance Angles C8 1.7087 (0.0017) C7 1.7363 (0.0017) 92.13 (0.08) S4 - C8 FMAP and GRID set by program FMAP 2 1 18 GRID -1.667 -2 -1 1.667 2 1 R1 = 0.0339 for 3096 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.81 at 0.1005 0.4999 0.4931 [ 0.72 A from S2 ] Deepest hole -0.78 at 0.2025 0.4834 0.4653 [ 0.80 A from S2 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2271 / 26367 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1005 0.4999 0.4931 1.00000 0.05 0.81 0.72 S2 1.68 C4 1.72 C1 2.05 H4A Q2 1 0.1810 0.5068 0.5013 1.00000 0.05 0.50 0.67 S2 1.61 C4 1.72 C1 1.94 H4B Q3 1 0.1454 0.6573 0.5005 1.00000 0.05 0.36 0.71 C2 0.73 C1 1.80 C6 1.82 C5 Q4 1 0.1041 0.6392 0.4307 1.00000 0.05 0.34 0.69 C1 0.81 C5 1.83 C2 2.01 C7 Q5 1 0.1502 0.4713 0.4540 1.00000 0.05 0.31 0.38 S2 1.97 C1 2.09 C4 2.51 H4A Q6 1 0.0115 0.6123 0.2002 1.00000 0.05 0.31 0.68 C9 0.75 C10 1.77 C7 1.80 C8 Q7 1 0.1435 0.8046 0.4473 1.00000 0.05 0.29 0.84 C6 0.93 S3 1.54 H6 1.88 C2 Q8 1 0.1127 0.5779 0.2866 1.00000 0.05 0.27 0.68 C7 1.06 S4 1.80 C9 1.84 C5 Q9 1 0.0327 0.5299 0.1706 1.00000 0.05 0.27 0.68 C10 0.77 C8 1.51 H8 1.79 C9 Q10 1 0.1449 0.4772 0.5532 1.00000 0.05 0.26 0.65 C4 1.16 S2 1.33 H4B 1.40 H4A Q11 1 0.1238 0.5063 0.6247 1.00000 0.05 0.26 0.75 C4 0.76 C3 1.40 H4A 1.41 H3B Q12 1 0.0325 0.6143 0.2770 1.00000 0.05 0.26 0.75 C9 0.80 C7 1.81 C10 2.03 C5 Q13 1 0.1181 0.5197 0.1885 1.00000 0.05 0.25 0.69 C8 1.11 S4 1.42 H8 1.73 C10 Q14 1 0.0987 0.6465 0.3400 1.00000 0.05 0.25 0.71 C5 0.75 C7 1.92 C1 1.94 C9 Q15 1 0.1475 0.7383 0.5192 1.00000 0.05 0.24 0.58 C2 0.79 C6 1.55 H6 1.72 C1 Q16 1 0.0594 0.6452 0.2620 1.00000 0.05 0.23 0.71 C7 0.74 C9 1.88 C10 1.94 C5 Q17 1 0.1340 0.5792 0.4686 1.00000 0.05 0.23 0.57 C1 1.20 S2 1.75 C5 1.81 C2 Q18 1 0.1649 0.6837 0.5755 1.00000 0.05 0.23 0.67 C2 1.09 S1 1.83 C6 1.89 C1 Q19 1 -0.0115 0.5804 0.1319 1.00000 0.05 0.22 0.53 C10 1.24 S5 1.71 C8 1.79 C9 Q20 1 0.1793 0.7543 0.5056 1.00000 0.05 0.21 0.74 C6 0.91 C2 1.45 H6 1.92 C1 Shortest distances between peaks (including symmetry equivalents) 15 20 0.53 12 16 0.59 2 5 0.94 1 5 0.98 2 10 1.00 4 17 1.05 9 19 1.07 3 15 1.08 15 18 1.12 1 10 1.13 3 17 1.13 6 19 1.14 1 2 1.15 10 11 1.16 6 12 1.17 1 17 1.18 6 9 1.19 3 18 1.19 7 20 1.19 8 14 1.20 8 16 1.21 3 4 1.21 6 16 1.21 8 12 1.24 9 13 1.24 2 17 1.24 14 16 1.28 3 20 1.34 4 14 1.35 7 15 1.37 12 14 1.38 18 20 1.39 5 17 1.43 5 10 1.47 8 13 1.63 10 17 1.82 9 12 1.91 4 15 1.93 6 13 1.93 6 8 1.97 1 11 1.97 2 11 2.00 2 3 2.01 1 4 2.02 9 16 2.05 3 7 2.06 13 16 2.12 17 18 2.12 1 3 2.13 4 20 2.14 8 9 2.14 14 17 2.15 12 13 2.16 13 19 2.16 15 17 2.20 4 7 2.22 12 19 2.28 4 8 2.28 2 4 2.28 4 5 2.29 16 19 2.32 4 18 2.38 17 20 2.41 6 14 2.45 3 10 2.46 3 14 2.47 7 18 2.47 11 18 2.47 11 17 2.50 3 5 2.50 4 12 2.51 2 18 2.55 4 16 2.57 5 11 2.59 7 14 2.66 3 11 2.70 10 18 2.70 8 17 2.71 13 14 2.79 1 18 2.82 4 10 2.83 1 1 2.85 5 8 2.88 8 19 2.88 5 14 2.91 7 17 2.93 1 14 2.95 14 15 2.98 Time profile in seconds ----------------------- 0.08: 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. 1.16: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.72: Structure factors and derivatives 0.41: 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 0.02: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 05src0055 finished at 23:00:52 Total CPU time: 2.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++