+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src0176 started at 06:30:14 on 04-Mar-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0176 in P2(1)/c CELL 0.71073 3.9246 16.0687 17.4699 90.000 90.825 90.000 ZERR 2.00 0.0001 0.0005 0.0004 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H S UNIT 52 24 16 V = 1101.59 F(000) = 592.0 Mu = 0.83 mm-1 Cell Wt = 1161.67 Rho = 1.751 MERG 2 OMIT -3.00 55.00 OMIT -1 0 2 EADP S4 C11' EADP C11 S4' FMAP 2 PLAN 20 SIZE 0.02 0.04 0.12 ACTA BOND WGHT 0.03420 1.41880 L.S. 4 TEMP -153.00 FVAR 0.72892 0.57447 C1 1 0.947572 0.519694 0.468001 11.00000 0.01603 0.01357 = 0.01036 0.00048 -0.00301 0.00012 C2 1 0.695703 0.555439 0.333170 11.00000 0.01325 0.01242 = 0.01149 0.00091 -0.00104 -0.00015 C3 1 0.792536 0.632946 0.365145 11.00000 0.01369 0.01414 = 0.01007 -0.00008 -0.00149 -0.00065 C4 1 0.751283 0.707360 0.324559 11.00000 0.01420 0.01372 = 0.00929 -0.00103 0.00084 0.00002 C5 1 0.613249 0.702093 0.248889 11.00000 0.01303 0.01368 = 0.01307 0.00075 -0.00061 0.00097 C6 1 0.509453 0.624001 0.219556 11.00000 0.01169 0.01710 = 0.00732 0.00066 -0.00157 0.00136 C7 1 0.547681 0.550359 0.260999 11.00000 0.01498 0.01322 = 0.01197 -0.00177 0.00077 -0.00092 AFIX 43 H7 2 0.474639 0.498526 0.240392 11.00000 -1.20000 AFIX 0 C8 1 0.546429 0.769329 0.193085 11.00000 0.01082 0.01439 = 0.00796 -0.00184 0.00025 0.00107 AFIX 43 H8 2 0.598888 0.826326 0.201610 11.00000 -1.20000 AFIX 0 C9 1 0.400687 0.739077 0.128228 11.00000 0.02133 0.02043 = 0.01484 0.00261 -0.00029 0.00535 AFIX 43 H9 2 0.339381 0.773581 0.086074 11.00000 -1.20000 AFIX 0 C10 1 0.829648 0.788480 0.359805 11.00000 0.01364 0.01143 = 0.01043 0.00027 -0.00331 0.00025 C12 1 0.998317 0.929811 0.382486 11.00000 0.01886 0.01529 = 0.03606 0.00869 -0.00203 -0.00041 AFIX 43 H12 2 1.097571 0.982640 0.372864 11.00000 -1.20000 AFIX 0 C13 1 0.840680 0.905751 0.447039 11.00000 0.02136 0.02693 = 0.01780 -0.00945 -0.00430 0.00320 AFIX 43 H13 2 0.814986 0.942960 0.488819 11.00000 -1.20000 AFIX 0 S1 3 0.779192 0.466215 0.388254 11.00000 0.02476 0.01110 = 0.01314 0.00109 -0.00775 -0.00120 S2 3 0.967229 0.628537 0.458683 11.00000 0.02361 0.01203 = 0.01147 0.00070 -0.00712 -0.00174 S3 3 0.334936 0.633170 0.128020 11.00000 0.02136 0.01755 = 0.01142 -0.00014 -0.00390 0.00085 PART 1 S4 3 0.697306 0.811669 0.450886 21.00000 0.02266 0.01345 = 0.01012 -0.00167 -0.00031 -0.00050 C11 1 0.985792 0.854838 0.327460 21.00000 0.01711 0.00951 = 0.01249 0.00256 0.00101 -0.00279 AFIX 43 H11 2 1.075928 0.855060 0.277283 21.00000 -1.20000 AFIX 0 PART 2 C11' 1 0.732953 0.814344 0.431471 -21.00000 0.02266 0.01345 = 0.01012 -0.00167 -0.00031 -0.00050 AFIX 43 H11' 2 0.615061 0.780448 0.466920 -21.00000 -1.20000 AFIX 0 S4' 3 1.039301 0.868563 0.313776 -21.00000 0.01711 0.00951 = 0.01249 0.00256 0.00101 -0.00279 HKLF 4 Covalent radii and connectivity table for 2008src0176 in P2(1)/c C 0.770 H 0.320 S 1.030 C1 - C1_$1 S1 S2 C2 - C7 C3 S1 C3 - C4 C2 S2 C4 - C3 C5 C10 C5 - C6 C4 C8 C6 - C7 C5 S3 C7 - C2 C6 C8 - C9 C5 C9 - C8 S3 C10 - C11_a C11'_b C4 S4_a S4'_b C12 - C13 C11_a S4'_b C13 - C12 C11'_b S4_a S1 - C2 C1 S2 - C1 C3 S3 - C9 C6 S4_a - C13 C10 C11_a - C10 C12 C11'_b - C10 C13 S4'_b - C12 C10 Operators for generating equivalent atoms: $1 -x+2, -y+1, -z+1 14475 Reflections read, of which 343 rejected -5 =< h =< 4, -20 =< k =< 20, -22 =< l =< 22, Max. 2-theta = 54.98 0 Systematic absence violations 0 Inconsistent equivalents 2509 Unique reflections, of which 0 suppressed R(int) = 0.0497 R(sigma) = 0.0425 Friedel opposites merged Maximum memory for data reduction = 1513 / 25215 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 = 1941 / 199878 wR2 = 0.0927 before cycle 1 for 2509 data and 161 / 161 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0342 * P )^2 + 1.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72739 0.00143 -1.067 OSF 2 0.57308 0.00349 -0.399 FVAR 2 Mean shift/esd = 0.228 Maximum = -1.067 for OSF Max. shift = 0.004 A for C11'_b Max. dU = 0.000 for C9 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1941 / 199878 wR2 = 0.0925 before cycle 2 for 2509 data and 161 / 161 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0342 * P )^2 + 1.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72655 0.00142 -0.589 OSF 2 0.57253 0.00348 -0.159 FVAR 2 Mean shift/esd = 0.077 Maximum = -0.589 for OSF Max. shift = 0.001 A for C11'_b Max. dU = 0.000 for C9 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1941 / 199878 wR2 = 0.0924 before cycle 3 for 2509 data and 161 / 161 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0342 * P )^2 + 1.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72655 0.00142 -0.004 OSF 2 0.57249 0.00348 -0.011 FVAR 2 Mean shift/esd = 0.002 Maximum = -0.011 for FVAR 2 Max. shift = 0.000 A for C11'_b Max. dU = 0.000 for C11_a Least-squares cycle 4 Maximum vector length = 511 Memory required = 1941 / 199878 wR2 = 0.0924 before cycle 4 for 2509 data and 161 / 161 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0342 * P )^2 + 1.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72655 0.00142 0.000 OSF 2 0.57248 0.00348 -0.001 FVAR 2 Mean shift/esd = 0.001 Maximum = 0.006 for U23 S4_a Max. shift = 0.000 A for C11'_b Max. dU = 0.000 for C3 Largest correlation matrix elements -0.844 y C11'_b / y S4_a -0.736 U23 S4_a / y S4_a -0.631 U13 S4_a / x S4_a 0.834 y C11'_b / U23 S4_a -0.721 y S4'_b / y C11_a 0.599 z C11'_b / U33 S4_a -0.774 x C11'_b / x S4_a -0.719 x S4'_b / x C11_a -0.568 x C11'_b / U11 S4_a 0.768 x C11'_b / U13 S4_a 0.713 z S4'_b / U33 C11_a -0.546 y C11'_b / U12 S4_a -0.738 y S4'_b / U22 C11_a 0.708 U11 C11_a / x C11_a 0.543 U11 S4_a / x S4_a -0.737 U33 C11_a / z C11_a -0.702 x S4'_b / U11 C11_a -0.508 U13 S4_a / U11 S4_a 0.736 U22 C11_a / y C11_a -0.651 z S4'_b / z C11_a Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H7 0.4740 0.4985 0.2404 43 0.950 0.000 C7 C2 C6 H8 0.5989 0.8263 0.2016 43 0.950 0.000 C8 C9 C5 H9 0.3397 0.7735 0.0861 43 0.950 0.000 C9 C8 S3 H12 1.0977 0.9826 0.3729 43 0.950 0.000 C12 C13 C11_a H13 0.8152 0.9429 0.4889 43 0.950 0.000 C13 C12 S4_a H11 1.0751 0.8552 0.2773 43 0.950 0.000 C11_a C10 C12 H11' 0.6156 0.7802 0.4671 43 0.950 0.000 C11'_b C10 C13 2008src0176 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.94772 0.51969 0.46797 1.00000 0.01561 0.01314 0.01012 0.00008 -0.00293 -0.00003 0.01299 0.00371 0.00054 0.00014 0.00012 0.00000 0.00105 0.00101 0.00095 0.00083 0.00079 0.00083 0.00042 C2 0.69582 0.55545 0.33312 1.00000 0.01278 0.01217 0.01075 0.00097 -0.00119 0.00009 0.01191 0.00369 0.00053 0.00013 0.00012 0.00000 0.00103 0.00102 0.00098 0.00081 0.00079 0.00079 0.00043 C3 0.79256 0.63294 0.36520 1.00000 0.01275 0.01403 0.00981 -0.00040 -0.00143 -0.00040 0.01221 0.00369 0.00054 0.00013 0.00012 0.00000 0.00104 0.00106 0.00097 0.00080 0.00080 0.00079 0.00043 C4 0.75116 0.70733 0.32459 1.00000 0.01338 0.01332 0.00901 -0.00099 0.00083 -0.00017 0.01190 0.00365 0.00053 0.00013 0.00012 0.00000 0.00102 0.00104 0.00095 0.00082 0.00078 0.00082 0.00042 C5 0.61300 0.70208 0.24890 1.00000 0.01257 0.01355 0.01229 0.00087 -0.00035 0.00094 0.01281 0.00377 0.00054 0.00013 0.00012 0.00000 0.00101 0.00103 0.00099 0.00084 0.00079 0.00082 0.00043 C6 0.50951 0.62402 0.21955 1.00000 0.01086 0.01656 0.00733 0.00034 -0.00130 0.00113 0.01159 0.00367 0.00053 0.00013 0.00012 0.00000 0.00099 0.00108 0.00093 0.00079 0.00077 0.00080 0.00043 C7 0.54743 0.55036 0.26099 1.00000 0.01464 0.01306 0.01143 -0.00199 0.00093 -0.00079 0.01304 0.00376 0.00054 0.00013 0.00012 0.00000 0.00105 0.00103 0.00100 0.00083 0.00081 0.00082 0.00043 H7 0.47398 0.49855 0.24042 1.00000 0.01565 0.00000 0.00000 C8 0.54648 0.76934 0.19311 1.00000 0.01057 0.01396 0.00767 -0.00184 0.00023 0.00128 0.01073 0.00362 0.00051 0.00013 0.00011 0.00000 0.00099 0.00102 0.00092 0.00079 0.00074 0.00078 0.00041 H8 0.59895 0.82634 0.20163 1.00000 0.01288 0.00000 0.00000 C9 0.40083 0.73900 0.12824 1.00000 0.02096 0.01988 0.01422 0.00268 -0.00063 0.00559 0.01836 0.00421 0.00060 0.00015 0.00013 0.00000 0.00117 0.00118 0.00108 0.00092 0.00089 0.00093 0.00048 H9 0.33970 0.77348 0.08605 1.00000 0.02203 0.00000 0.00000 C10 0.82956 0.78852 0.35984 1.00000 0.01314 0.01149 0.01033 0.00034 -0.00336 0.00034 0.01169 0.00359 0.00053 0.00013 0.00012 0.00000 0.00104 0.00101 0.00097 0.00081 0.00078 0.00081 0.00042 C12 0.99830 0.92979 0.38254 1.00000 0.01842 0.01498 0.03588 0.00853 -0.00172 -0.00055 0.02311 0.00455 0.00061 0.00015 0.00015 0.00000 0.00118 0.00114 0.00141 0.00105 0.00101 0.00092 0.00053 H12_a 1.09770 0.98260 0.37292 1.00000 0.02774 0.00000 0.00000 C13 0.84079 0.90571 0.44709 1.00000 0.02136 0.02634 0.01770 -0.00958 -0.00432 0.00301 0.02184 0.00414 0.00061 0.00016 0.00013 0.00000 0.00120 0.00131 0.00113 0.00101 0.00092 0.00101 0.00052 H13_a 0.81524 0.94290 0.48889 1.00000 0.02621 0.00000 0.00000 S1 0.77919 0.46624 0.38828 1.00000 0.02441 0.01083 0.01280 0.00105 -0.00774 -0.00120 0.01609 0.00093 0.00015 0.00003 0.00003 0.00000 0.00031 0.00027 0.00027 0.00020 0.00022 0.00021 0.00015 S2 0.96729 0.62853 0.45867 1.00000 0.02326 0.01178 0.01110 0.00075 -0.00720 -0.00175 0.01546 0.00093 0.00015 0.00003 0.00003 0.00000 0.00031 0.00028 0.00027 0.00020 0.00021 0.00021 0.00015 S3 0.33487 0.63315 0.12803 1.00000 0.02095 0.01737 0.01105 -0.00014 -0.00395 0.00086 0.01650 0.00098 0.00015 0.00004 0.00003 0.00000 0.00031 0.00029 0.00027 0.00021 0.00021 0.00022 0.00015 S4_a 0.69732 0.81168 0.45090 0.57248 0.02229 0.01319 0.00959 -0.00181 -0.00024 -0.00044 0.01503 0.00305 0.00045 0.00011 0.00007 0.00348 0.00065 0.00047 0.00075 0.00062 0.00055 0.00040 0.00037 C11_a 0.98529 0.85490 0.32756 0.57248 0.01689 0.00952 0.01231 0.00254 0.00094 -0.00276 0.01290 0.01567 0.00216 0.00052 0.00047 0.00348 0.00101 0.00098 0.00107 0.00060 0.00064 0.00061 0.00050 H11_a 1.07506 0.85517 0.27734 0.57248 0.01548 0.00348 0.00000 C11'_b 0.73297 0.81413 0.43164 0.42752 0.02229 0.01319 0.00959 -0.00181 -0.00024 -0.00044 0.01503 0.02074 0.00302 0.00076 0.00052 0.00348 0.00065 0.00047 0.00075 0.00062 0.00055 0.00040 0.00037 H11'_b 0.61559 0.78015 0.46711 0.42752 0.01804 0.00348 0.00000 S4'_b 1.03929 0.86855 0.31381 0.42752 0.01689 0.00952 0.01231 0.00254 0.00094 -0.00276 0.01290 0.00414 0.00058 0.00014 0.00012 0.00348 0.00101 0.00098 0.00107 0.00060 0.00064 0.00061 0.00050 Final Structure Factor Calculation for 2008src0176 in P2(1)/c Total number of l.s. parameters = 161 Maximum vector length = 511 Memory required = 1780 / 21973 wR2 = 0.0924 before cycle 5 for 2509 data and 0 / 161 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0342 * P )^2 + 1.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0356 for 2113 Fo > 4sig(Fo) and 0.0464 for all 2509 data wR2 = 0.0924, GooF = S = 1.049, Restrained GooF = 1.049 for all data Occupancy sum of asymmetric unit = 17.00 for non-hydrogen and 6.00 for hydrogen atoms Principal mean square atomic displacements U 0.0171 0.0131 0.0088 C1 0.0136 0.0124 0.0097 C2 0.0141 0.0134 0.0091 C3 0.0138 0.0132 0.0087 C4 0.0143 0.0130 0.0112 C5 0.0168 0.0112 0.0068 C6 0.0156 0.0134 0.0101 C7 0.0148 0.0103 0.0071 C8 0.0261 0.0170 0.0119 C9 0.0156 0.0115 0.0079 C10 0.0392 0.0182 0.0119 C12 0.0346 0.0199 0.0110 C13 0.0287 0.0108 0.0087 S1 0.0271 0.0115 0.0077 S2 0.0227 0.0172 0.0096 S3 0.0223 0.0139 0.0088 S4_a 0.0178 0.0137 0.0072 C11_a 0.0223 0.0139 0.0088 C11'_b 0.0178 0.0137 0.0072 S4'_b Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.020 0.038 0.058 0.080 0.105 0.133 0.166 0.212 0.293 1.000 Number in group 257. 251. 254. 244. 249. 249. 254. 248. 252. 251. GooF 1.064 1.055 1.115 1.194 1.063 0.949 1.025 1.050 1.027 0.927 K 1.376 0.965 0.922 0.939 0.978 0.995 0.996 1.007 1.017 1.007 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.31 1.65 inf Number in group 258. 245. 249. 256. 251. 249. 247. 252. 249. 253. GooF 1.038 0.914 1.011 0.868 0.946 0.969 0.930 0.896 1.108 1.605 K 1.023 0.992 1.015 1.008 1.023 1.019 1.020 1.011 1.005 0.990 R1 0.092 0.082 0.071 0.048 0.050 0.041 0.034 0.028 0.028 0.033 Recommended weighting scheme: WGHT 0.0285 1.5499 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) 1 7 3 204.09 115.36 5.28 0.078 1.87 -1 0 4 770.12 1045.12 5.22 0.234 2.94 0 7 5 1313.14 1017.54 4.79 0.231 1.92 -2 1 2 743.37 558.05 4.59 0.171 1.91 0 5 5 57.18 15.16 4.46 0.028 2.37 1 5 3 92.61 48.22 3.90 0.050 2.28 0 4 17 -6.95 15.32 3.65 0.028 1.00 2 0 2 31.97 7.57 3.53 0.020 1.91 1 5 5 82.55 134.90 3.52 0.084 2.02 0 1 7 47.61 21.84 3.49 0.034 2.47 1 1 5 277.27 203.49 3.46 0.103 2.56 0 6 0 480.71 616.58 3.41 0.180 2.68 1 1 6 839.72 687.64 3.37 0.190 2.30 -1 3 4 8.13 0.21 3.34 0.003 2.58 -1 7 7 495.77 618.69 3.20 0.180 1.56 -3 13 3 43.54 90.52 3.07 0.069 0.89 -1 0 8 55.15 91.61 3.07 0.069 1.92 0 11 14 60.91 118.44 2.99 0.079 0.95 -2 17 3 -1.58 24.68 2.99 0.036 0.84 -1 3 22 256.63 375.98 2.98 0.141 0.77 -2 3 4 32.97 12.56 2.96 0.026 1.71 -1 4 2 127.18 180.89 2.95 0.098 2.68 2 5 2 14.34 0.78 2.92 0.006 1.64 4 12 4 10.97 94.67 2.88 0.071 0.78 0 10 0 955.77 1132.62 2.86 0.244 1.61 -3 9 8 42.15 79.77 2.83 0.065 0.95 4 12 5 36.88 108.82 2.83 0.076 0.77 1 14 5 211.03 152.60 2.81 0.090 1.05 0 4 0 3361.25 3849.59 2.79 0.450 4.02 0 7 4 895.13 762.18 2.78 0.200 2.03 2 7 4 13.18 33.28 2.76 0.042 1.41 1 6 0 369.84 296.86 2.73 0.125 2.21 0 7 6 462.53 371.62 2.71 0.140 1.80 0 3 2 697.53 586.41 2.70 0.176 4.57 1 1 4 463.22 554.77 2.63 0.171 2.85 -2 3 6 87.07 56.35 2.63 0.054 1.57 -4 7 8 -15.35 14.54 2.62 0.028 0.84 1 8 2 411.61 335.59 2.60 0.133 1.75 0 4 9 87.23 56.26 2.60 0.054 1.75 1 7 6 46.04 24.04 2.60 0.036 1.63 -3 2 5 8.03 24.08 2.60 0.036 1.22 1 5 4 491.36 410.20 2.57 0.147 2.15 1 2 11 92.20 129.02 2.55 0.082 1.44 -4 8 3 14.21 33.37 2.53 0.042 0.87 1 7 4 524.91 434.60 2.53 0.151 1.80 0 13 7 420.51 508.64 2.52 0.164 1.11 1 0 2 7331.10 8192.76 2.50 0.656 3.56 -1 4 6 151.34 112.76 2.49 0.077 2.03 0 7 9 312.31 383.76 2.48 0.142 1.48 0 12 5 50.60 27.86 2.47 0.038 1.25 Bond lengths and angles C1 - Distance Angles C1_$1 1.3446 (0.0042) S1 1.7570 (0.0022) 122.43 (0.23) S2 1.7583 (0.0022) 122.13 (0.23) 115.43 (0.12) C1 - C1_$1 S1 C2 - Distance Angles C7 1.3829 (0.0030) C3 1.4152 (0.0030) 121.33 (0.20) S1 1.7554 (0.0021) 121.64 (0.17) 117.02 (0.16) C2 - C7 C3 C3 - Distance Angles C4 1.3983 (0.0030) C2 1.4152 (0.0029) 121.51 (0.19) S2 1.7634 (0.0021) 123.03 (0.16) 115.46 (0.16) C3 - C4 C2 C4 - Distance Angles C3 1.3983 (0.0030) C5 1.4243 (0.0030) 117.40 (0.19) C10 1.4733 (0.0029) 121.52 (0.19) 120.99 (0.19) C4 - C3 C5 C5 - Distance Angles C6 1.4125 (0.0030) C4 1.4243 (0.0030) 119.56 (0.19) C8 1.4761 (0.0029) 111.30 (0.18) 129.11 (0.19) C5 - C6 C4 C6 - Distance Angles C7 1.3943 (0.0029) C5 1.4125 (0.0030) 122.50 (0.19) S3 1.7367 (0.0021) 125.98 (0.17) 111.52 (0.16) C6 - C7 C5 C7 - Distance Angles C2 1.3829 (0.0030) C6 1.3943 (0.0029) 117.60 (0.20) C7 - C2 C8 - Distance Angles C9 1.3529 (0.0031) C5 1.4761 (0.0029) 110.97 (0.20) C8 - C9 C9 - Distance Angles C8 1.3529 (0.0031) S3 1.7205 (0.0025) 114.82 (0.18) C9 - C8 C10 - Distance Angles C11_a 1.3561 (0.0070) C11'_b 1.3785 (0.0096) 105.97 (0.66) C4 1.4733 (0.0029) 127.97 (0.42) 125.88 (0.53) S4_a 1.7212 (0.0023) 110.98 (0.41) 5.02 (0.55) 120.92 (0.17) S4'_b 1.7311 (0.0026) 4.02 (0.45) 109.87 (0.52) 124.16 (0.17) 114.87 (0.15) C10 - C11_a C11'_b C4 S4_a C12 - Distance Angles C13 1.3504 (0.0035) C11_a 1.5402 (0.0094) 106.59 (0.31) S4'_b 1.5626 (0.0037) 120.98 (0.21) 14.42 (0.24) C12 - C13 C11_a C13 - Distance Angles C12 1.3504 (0.0035) C11'_b 1.5538 (0.0125) 104.66 (0.37) S4_a 1.6142 (0.0032) 117.83 (0.20) 13.18 (0.33) C13 - C12 C11'_b S1 - Distance Angles C2 1.7554 (0.0021) C1 1.7570 (0.0022) 95.79 (0.10) S1 - C2 S2 - Distance Angles C1 1.7583 (0.0022) C3 1.7634 (0.0022) 96.24 (0.10) S2 - C1 S3 - Distance Angles C9 1.7205 (0.0025) C6 1.7367 (0.0021) 91.39 (0.11) S3 - C9 S4_a - Distance Angles C13 1.6142 (0.0032) C10 1.7212 (0.0023) 93.11 (0.13) S4_a - C13 C11_a - Distance Angles C10 1.3561 (0.0069) C12 1.5402 (0.0094) 111.49 (0.53) C11_a - C10 C11'_b - Distance Angles C10 1.3785 (0.0096) C13 1.5538 (0.0125) 111.28 (0.68) C11'_b - C10 S4'_b - Distance Angles C12 1.5626 (0.0037) C10 1.7311 (0.0026) 93.21 (0.14) S4'_b - C12 FMAP and GRID set by program FMAP 2 1 12 GRID -5.556 -2 -1 5.556 2 1 R1 = 0.0460 for 2509 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.45 at 0.2442 0.2996 0.1101 [ 0.63 A from C10 ] Deepest hole -0.39 at 0.4027 0.6540 0.1465 [ 0.53 A from S3 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 2467 / 26025 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7558 0.7996 0.3899 1.00000 0.05 0.45 0.63 C10 0.77 C11' 1.11 S4 1.50 H11' Q2 1 0.7247 0.5956 0.3510 1.00000 0.05 0.40 0.70 C3 0.72 C2 1.86 C4 1.86 C7 Q3 1 0.5921 0.7925 0.1935 1.00000 0.05 0.37 0.41 C8 0.56 H8 1.61 C9 1.75 C5 Q4 1 0.5886 0.7421 0.2165 1.00000 0.05 0.37 0.62 C8 0.86 C5 1.38 H8 1.70 C9 Q5 1 0.7259 0.6993 0.2803 1.00000 0.05 0.36 0.70 C5 0.79 C4 1.81 C6 1.84 C3 Q6 1 0.7782 0.7477 0.3434 1.00000 0.05 0.35 0.73 C4 0.74 C10 1.88 C3 1.89 C11' Q7 1 0.5961 0.6638 0.2347 1.00000 0.05 0.33 0.67 C5 0.77 C6 1.82 C4 1.85 C8 Q8 1 0.3588 0.7006 0.1290 1.00000 0.05 0.33 0.64 C9 1.09 S3 1.39 H9 1.73 C8 Q9 1 0.7187 0.5143 0.3571 1.00000 0.05 0.33 0.79 C2 0.97 S1 1.89 C7 1.93 C3 Q10 1 0.7954 0.6657 0.3418 1.00000 0.05 0.32 0.67 C3 0.75 C4 1.82 C2 1.86 C5 Q11 1 0.4123 0.7612 0.1740 1.00000 0.05 0.32 0.63 C8 0.88 C9 1.36 H8 1.57 H9 Q12 1 0.5487 0.5847 0.2372 1.00000 0.05 0.29 0.69 C7 0.72 C6 1.42 H7 1.83 C2 Q13 1 0.8508 0.8217 0.3290 1.00000 0.05 0.29 0.75 C11 0.76 C10 1.09 S4' 1.38 H11 Q14 1 0.9050 0.9168 0.4075 1.00000 0.05 0.28 0.61 C12 0.76 C13 1.44 H12 1.53 H13 Q15 1 0.7868 0.8661 0.4496 1.00000 0.05 0.28 0.67 C13 0.92 C11' 0.94 S4 1.42 H13 Q16 1 1.0000 0.5000 0.5000 0.50000 0.05 0.28 0.67 C1 2.19 S2 2.19 S1 3.26 C2 Q17 1 0.9851 1.0604 0.4176 1.00000 0.05 0.27 1.54 H12 1.80 H13 1.88 S3 2.19 C12 Q18 1 0.6223 0.9843 0.4645 1.00000 0.05 0.27 1.09 H13 1.56 C13 2.24 H13 2.25 C12 Q19 1 1.0072 0.8943 0.3543 1.00000 0.05 0.26 0.76 C12 0.79 C11 0.83 S4' 1.50 H12 Q20 1 0.4553 0.6230 0.1904 1.00000 0.05 0.25 0.55 C6 1.19 S3 1.73 C7 1.74 C5 Shortest distances between peaks (including symmetry equivalents) 3 4 0.90 3 11 0.93 4 11 1.05 14 19 1.08 12 20 1.08 5 7 1.10 7 20 1.15 1 6 1.17 2 10 1.17 1 13 1.19 14 15 1.19 5 10 1.23 6 13 1.25 8 11 1.27 7 12 1.28 4 7 1.30 2 9 1.31 6 10 1.32 5 6 1.36 13 19 1.39 4 5 1.41 1 15 1.50 18 18 1.66 8 20 1.68 14 18 1.85 4 8 1.89 1 19 1.92 15 19 1.94 1 14 1.99 7 10 2.02 7 11 2.02 15 18 2.02 4 20 2.03 17 18 2.06 13 14 2.06 3 8 2.06 2 5 2.07 2 12 2.10 5 12 2.10 7 8 2.14 3 5 2.19 3 7 2.19 5 13 2.20 13 15 2.24 11 20 2.25 5 20 2.25 1 10 2.32 4 6 2.33 14 17 2.34 2 7 2.36 5 11 2.43 6 7 2.43 10 12 2.43 2 6 2.46 9 12 2.46 9 10 2.47 1 5 2.50 10 13 2.53 6 19 2.53 4 13 2.55 4 12 2.56 3 13 2.60 4 10 2.63 17 18 2.65 6 15 2.66 9 16 2.73 17 20 2.73 15 17 2.74 8 17 2.74 8 12 2.75 3 20 2.78 3 6 2.80 18 19 2.86 17 19 2.89 6 14 2.98 5 8 2.99 Time profile in seconds ----------------------- 0.08: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: Generate connectivity array 0.03: 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. 2.48: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.36: Structure factors and derivatives 0.47: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 0.23: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src0176 finished at 06:30:18 Total CPU time: 3.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++