+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0189 started at 14:41:22 on 26-Feb-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0189 in P-1 CELL 0.71073 7.7644 8.7396 9.6184 108.028 96.346 107.648 ZERR 2.00 0.0002 0.0003 0.0003 0.001 0.002 0.002 LATT 1 SFAC C H N O UNIT 24 16 4 8 V = 576.19 F(000) = 252.0 Mu = 0.11 mm-1 Cell Wt = 488.41 Rho = 1.408 MERG 2 OMIT -3.00 55.00 OMIT 1 -2 2 OMIT -2 0 2 OMIT 1 -1 1 SHEL 7 0.77 FMAP 2 PLAN 10 ACTA SIZE 0.4 0.37 0.21 BOND $H WGHT 0.05940 0.24160 L.S. 8 TEMP -153.00 FVAR 1.88279 MOLE 1 C1 1 -0.119097 -0.338987 -0.492271 11.00000 0.03204 0.02122 = 0.02282 0.00342 0.00457 0.00447 AFIX 137 H1A 2 -0.240543 -0.329807 -0.517035 11.00000 -1.50000 H1B 2 -0.126782 -0.413479 -0.433381 11.00000 -1.50000 H1C 2 -0.081901 -0.388438 -0.585045 11.00000 -1.50000 AFIX 0 C2 1 0.020438 -0.164810 -0.403259 11.00000 0.02191 0.02136 = 0.01851 0.00551 0.00380 0.01006 C4 1 0.107721 0.052602 -0.160340 11.00000 0.01880 0.01767 = 0.01695 0.00412 0.00731 0.00445 C5 1 0.082689 0.195068 -0.181930 11.00000 0.02134 0.02223 = 0.01881 0.00744 0.00487 0.00780 AFIX 43 H5 2 -0.001006 0.180561 -0.268911 11.00000 -1.20000 AFIX 0 C6 1 0.180130 0.358479 -0.076247 11.00000 0.02211 0.02024 = 0.02282 0.00870 0.00790 0.00937 AFIX 43 H6 2 0.165270 0.456605 -0.091250 11.00000 -1.20000 AFIX 0 C7 1 0.299674 0.377748 0.051767 11.00000 0.01688 0.01641 = 0.02013 0.00424 0.00748 0.00500 C8 1 0.325269 0.236517 0.075379 11.00000 0.01830 0.02143 = 0.01743 0.00709 0.00699 0.00797 C9 1 0.229141 0.070645 -0.033977 11.00000 0.01952 0.01790 = 0.01973 0.00712 0.00931 0.00759 C10 1 0.255436 -0.077705 -0.013560 11.00000 0.02238 0.02118 = 0.02038 0.00664 0.00694 0.00689 C12 1 0.444343 0.259194 0.211412 11.00000 0.02541 0.02149 = 0.02345 0.00744 0.00640 0.00731 C15 1 0.307512 0.627117 0.242866 11.00000 0.02282 0.01969 = 0.01576 0.00722 0.00442 0.00959 C16 1 0.432938 0.803381 0.342572 11.00000 0.02610 0.01987 = 0.02106 0.00148 0.00282 0.00584 AFIX 137 H16A 2 0.364377 0.882388 0.354837 11.00000 -1.50000 H16B 2 0.537483 0.842195 0.297780 11.00000 -1.50000 H16C 2 0.479624 0.801739 0.440818 11.00000 -1.50000 AFIX 0 N11 3 0.278409 -0.194179 0.004920 11.00000 0.03354 0.02456 = 0.03355 0.01268 0.00906 0.01200 N13 3 0.536090 0.275666 0.321005 11.00000 0.04108 0.03624 = 0.02806 0.01116 -0.00269 0.01009 O2 4 0.135629 -0.074791 -0.444764 11.00000 0.02830 0.02541 = 0.02450 0.00581 0.01026 0.00548 O3 4 -0.000443 -0.113740 -0.256556 11.00000 0.02638 0.01750 = 0.01777 0.00357 0.00562 0.00264 O14 4 0.403992 0.540281 0.157071 11.00000 0.01895 0.01659 = 0.02337 0.00231 0.00517 0.00542 O15 4 0.145449 0.560597 0.234566 11.00000 0.02151 0.02400 = 0.02520 0.00496 0.00716 0.00698 HKLF 4 Covalent radii and connectivity table for 2009src0189 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - C2 C2 - O2 O3 C1 C4 - C9 C5 O3 C5 - C6 C4 C6 - C5 C7 C7 - C8 O14 C6 C8 - C7 C9 C12 C9 - C4 C8 C10 C10 - N11 C9 C12 - N13 C8 C15 - O15 O14 C16 C16 - C15 N11 - C10 N13 - C12 O2 - C2 O3 - C2 C4 O14 - C15 C7 O15 - C15 14107 Reflections read, of which 34 rejected -9 =< h =< 10, -11 =< k =< 11, -12 =< l =< 12, Max. 2-theta = 54.95 0 Systematic absence violations 0 Inconsistent equivalents 2622 Unique reflections, of which 0 suppressed R(int) = 0.0400 R(sigma) = 0.0305 Friedel opposites merged Maximum memory for data reduction = 1458 / 26466 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 = 1878 / 205650 wR2 = 0.1206 before cycle 1 for 2622 data and 165 / 165 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0594 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.88277 0.00475 -0.004 OSF Mean shift/su = 0.003 Maximum = -0.010 for U11 O14 Max. shift = 0.000 A for H1A Max. dU = 0.000 for C9 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1878 / 205650 wR2 = 0.1206 before cycle 2 for 2622 data and 165 / 165 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0594 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.88275 0.00475 -0.004 OSF Mean shift/su = 0.001 Maximum = -0.004 for OSF Max. shift = 0.000 A for H16A Max. dU = 0.000 for C9 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1878 / 205650 wR2 = 0.1206 before cycle 3 for 2622 data and 165 / 165 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0594 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.88275 0.00475 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for tors H16A Max. shift = 0.000 A for H16A Max. dU = 0.000 for N13 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1878 / 205650 wR2 = 0.1206 before cycle 4 for 2622 data and 165 / 165 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0594 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.88275 0.00475 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for tors H16A Max. shift = 0.000 A for H16B Max. dU = 0.000 for C15 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1878 / 205650 wR2 = 0.1206 before cycle 5 for 2622 data and 165 / 165 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0594 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.88275 0.00475 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for tors H16A Max. shift = 0.000 A for H16B Max. dU = 0.000 for C7 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1878 / 205650 wR2 = 0.1206 before cycle 6 for 2622 data and 165 / 165 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0594 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.88275 0.00475 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for tors H16A Max. shift = 0.000 A for H16A Max. dU = 0.000 for C15 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1878 / 205650 wR2 = 0.1206 before cycle 7 for 2622 data and 165 / 165 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0594 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.88275 0.00475 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for tors H16A Max. shift = 0.000 A for H16B Max. dU = 0.000 for N11 Least-squares cycle 8 Maximum vector length = 511 Memory required = 1878 / 205650 wR2 = 0.1206 before cycle 8 for 2622 data and 165 / 165 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0594 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.88275 0.00475 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for tors H16A Max. shift = 0.000 A for H16C Max. dU = 0.000 for O15 Largest correlation matrix elements 0.503 U23 C6 / U22 C6 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A -0.2405 -0.3298 -0.5170 137 0.980 0.000 C1 C2 H1A H1B -0.1268 -0.4135 -0.4334 137 0.980 0.000 C1 C2 H1A H1C -0.0819 -0.3884 -0.5850 137 0.980 0.000 C1 C2 H1A H5 -0.0010 0.1806 -0.2689 43 0.950 0.000 C5 C6 C4 H6 0.1653 0.4566 -0.0912 43 0.950 0.000 C6 C5 C7 H16A 0.3644 0.8824 0.3548 137 0.980 0.000 C16 C15 H16A H16B 0.5375 0.8422 0.2978 137 0.980 0.000 C16 C15 H16A H16C 0.4796 0.8017 0.4408 137 0.980 0.000 C16 C15 H16A 2009src0189 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.11910 -0.33899 -0.49227 1.00000 0.03204 0.02122 0.02282 0.00342 0.00457 0.00447 0.02787 0.00358 0.00022 0.00019 0.00017 0.00000 0.00082 0.00073 0.00073 0.00060 0.00061 0.00062 0.00034 H1A -0.24054 -0.32981 -0.51703 1.00000 0.04181 0.00000 0.00000 H1B -0.12678 -0.41348 -0.43338 1.00000 0.04181 0.00000 0.00000 H1C -0.08190 -0.38844 -0.58505 1.00000 0.04181 0.00000 0.00000 C2 0.02044 -0.16481 -0.40326 1.00000 0.02191 0.02136 0.01850 0.00550 0.00380 0.01006 0.02051 0.00338 0.00019 0.00018 0.00015 0.00000 0.00069 0.00070 0.00066 0.00055 0.00053 0.00056 0.00030 C4 0.10772 0.05260 -0.16034 1.00000 0.01880 0.01766 0.01694 0.00412 0.00731 0.00445 0.01856 0.00325 0.00019 0.00017 0.00015 0.00000 0.00066 0.00066 0.00064 0.00053 0.00051 0.00052 0.00029 C5 0.08269 0.19507 -0.18193 1.00000 0.02134 0.02222 0.01881 0.00744 0.00487 0.00780 0.02075 0.00343 0.00019 0.00018 0.00016 0.00000 0.00069 0.00071 0.00066 0.00056 0.00053 0.00056 0.00030 H5 -0.00101 0.18056 -0.26891 1.00000 0.02491 0.00000 0.00000 C6 0.18013 0.35848 -0.07625 1.00000 0.02210 0.02023 0.02282 0.00870 0.00790 0.00937 0.02080 0.00345 0.00019 0.00018 0.00016 0.00000 0.00070 0.00069 0.00070 0.00057 0.00055 0.00055 0.00030 H6 0.16527 0.45661 -0.09125 1.00000 0.02497 0.00000 0.00000 C7 0.29967 0.37775 0.05177 1.00000 0.01688 0.01640 0.02013 0.00424 0.00748 0.00500 0.01835 0.00328 0.00018 0.00017 0.00015 0.00000 0.00064 0.00064 0.00065 0.00053 0.00051 0.00051 0.00029 C8 0.32527 0.23652 0.07538 1.00000 0.01829 0.02143 0.01743 0.00709 0.00699 0.00797 0.01857 0.00330 0.00018 0.00018 0.00015 0.00000 0.00065 0.00069 0.00065 0.00055 0.00052 0.00054 0.00029 C9 0.22914 0.07065 -0.03398 1.00000 0.01951 0.01790 0.01972 0.00712 0.00931 0.00759 0.01832 0.00331 0.00018 0.00017 0.00015 0.00000 0.00067 0.00066 0.00067 0.00054 0.00053 0.00053 0.00029 C10 0.25544 -0.07770 -0.01356 1.00000 0.02238 0.02118 0.02037 0.00664 0.00694 0.00689 0.02157 0.00343 0.00020 0.00018 0.00016 0.00000 0.00070 0.00070 0.00068 0.00057 0.00054 0.00056 0.00030 C12 0.44434 0.25919 0.21141 1.00000 0.02541 0.02148 0.02345 0.00744 0.00640 0.00731 0.02380 0.00357 0.00020 0.00019 0.00017 0.00000 0.00074 0.00071 0.00073 0.00058 0.00059 0.00058 0.00032 C15 0.30751 0.62712 0.24287 1.00000 0.02282 0.01968 0.01576 0.00722 0.00442 0.00959 0.01872 0.00329 0.00019 0.00017 0.00015 0.00000 0.00071 0.00067 0.00063 0.00054 0.00051 0.00055 0.00029 C16 0.43294 0.80338 0.34257 1.00000 0.02610 0.01986 0.02106 0.00148 0.00282 0.00584 0.02462 0.00344 0.00021 0.00019 0.00016 0.00000 0.00074 0.00070 0.00070 0.00057 0.00056 0.00058 0.00032 H16A 0.36437 0.88239 0.35484 1.00000 0.03693 0.00000 0.00000 H16B 0.53748 0.84220 0.29778 1.00000 0.03693 0.00000 0.00000 H16C 0.47963 0.80174 0.44082 1.00000 0.03693 0.00000 0.00000 N11 0.27841 -0.19418 0.00492 1.00000 0.03354 0.02456 0.03355 0.01268 0.00906 0.01200 0.02948 0.00333 0.00019 0.00017 0.00016 0.00000 0.00073 0.00068 0.00073 0.00058 0.00057 0.00057 0.00031 N13 0.53609 0.27567 0.32100 1.00000 0.04108 0.03624 0.02806 0.01115 -0.00269 0.01009 0.03706 0.00347 0.00021 0.00020 0.00016 0.00000 0.00083 0.00082 0.00075 0.00063 0.00062 0.00065 0.00036 O2 0.13563 -0.07479 -0.44476 1.00000 0.02830 0.02541 0.02450 0.00581 0.01026 0.00548 0.02751 0.00253 0.00015 0.00014 0.00012 0.00000 0.00057 0.00057 0.00055 0.00045 0.00044 0.00045 0.00027 O3 -0.00044 -0.11374 -0.25656 1.00000 0.02638 0.01750 0.01777 0.00356 0.00562 0.00264 0.02247 0.00234 0.00014 0.00013 0.00011 0.00000 0.00053 0.00050 0.00050 0.00040 0.00039 0.00040 0.00024 O14 0.40399 0.54028 0.15707 1.00000 0.01894 0.01659 0.02337 0.00231 0.00517 0.00542 0.02106 0.00229 0.00013 0.00012 0.00011 0.00000 0.00049 0.00049 0.00052 0.00040 0.00039 0.00039 0.00024 O15 0.14545 0.56060 0.23457 1.00000 0.02150 0.02400 0.02520 0.00496 0.00716 0.00698 0.02467 0.00245 0.00014 0.00013 0.00012 0.00000 0.00053 0.00054 0.00054 0.00043 0.00041 0.00042 0.00025 Final Structure Factor Calculation for 2009src0189 in P-1 Total number of l.s. parameters = 165 Maximum vector length = 511 Memory required = 1713 / 22995 wR2 = 0.1206 before cycle 9 for 2622 data and 0 / 165 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0594 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0439 for 2173 Fo > 4sig(Fo) and 0.0544 for all 2622 data wR2 = 0.1206, GooF = S = 1.049, Restrained GooF = 1.049 for all data Occupancy sum of asymmetric unit = 18.00 for non-hydrogen and 8.00 for hydrogen atoms Principal mean square atomic displacements U 0.0373 0.0279 0.0185 C1 0.0250 0.0190 0.0175 C2 0.0256 0.0167 0.0135 C4 0.0224 0.0213 0.0186 C5 0.0248 0.0197 0.0179 C6 0.0253 0.0160 0.0137 C7 0.0216 0.0202 0.0140 C8 0.0240 0.0177 0.0133 C9 0.0254 0.0209 0.0184 C10 0.0270 0.0229 0.0214 C12 0.0234 0.0177 0.0150 C15 0.0300 0.0278 0.0161 C16 0.0348 0.0316 0.0220 N11 0.0509 0.0368 0.0235 N13 0.0385 0.0236 0.0204 O2 0.0327 0.0192 0.0155 O3 0.0292 0.0188 0.0152 O14 0.0322 0.0220 0.0198 O15 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.032 0.048 0.066 0.087 0.113 0.141 0.186 0.277 1.000 Number in group 266. 270. 263. 251. 262. 269. 256. 263. 258. 264. GooF 0.976 0.951 1.105 1.072 1.157 1.085 1.094 1.047 0.983 1.005 K 2.307 1.094 0.961 0.942 0.971 0.994 0.997 1.016 1.017 0.999 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.31 1.64 inf Number in group 272. 260. 261. 258. 262. 264. 258. 261. 265. 261. GooF 0.885 0.862 1.013 0.907 0.945 0.912 0.889 1.073 1.307 1.501 K 1.013 1.010 0.998 1.022 1.017 1.018 1.026 1.028 1.018 0.976 R1 0.110 0.093 0.093 0.070 0.060 0.044 0.037 0.041 0.043 0.039 Recommended weighting scheme: WGHT 0.0596 0.2415 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) 2 -3 4 4.52 0.29 5.65 0.010 1.88 4 -3 1 5.31 12.39 4.07 0.068 1.79 1 5 4 34.87 52.73 3.83 0.141 1.03 0 -3 5 110.66 81.98 3.78 0.176 1.80 -3 0 3 72.45 99.91 3.73 0.194 2.12 1 0 5 4.76 10.67 3.70 0.063 1.65 -3 1 5 129.34 97.53 3.66 0.192 1.56 -2 2 4 39.44 26.79 3.64 0.100 1.76 -1 4 2 51.08 35.94 3.58 0.116 1.68 -1 2 4 103.60 77.84 3.56 0.171 1.78 -5 3 0 4.61 1.48 3.54 0.024 1.51 4 6 1 14.14 6.04 3.52 0.048 0.87 -8 -1 5 21.66 38.07 3.43 0.120 0.87 2 -10 5 7.51 16.33 3.41 0.078 0.86 -4 1 5 3.09 0.62 3.38 0.015 1.41 2 6 2 53.73 75.20 3.36 0.168 0.98 -9 2 3 21.37 39.06 3.32 0.121 0.85 -2 3 3 3.83 8.79 3.31 0.058 1.78 1 -5 3 20.20 30.72 3.24 0.107 1.70 -6 1 0 4.42 1.62 3.16 0.025 1.26 5 -3 3 7.09 3.32 3.15 0.035 1.33 0 -2 4 155.55 197.16 3.14 0.272 2.33 -7 -1 4 35.13 52.04 3.12 0.140 0.99 1 -4 6 69.29 90.89 3.09 0.185 1.45 -4 2 5 29.97 20.85 2.98 0.089 1.35 -3 0 6 14.18 8.76 2.97 0.057 1.41 -2 -3 1 46.62 34.77 2.95 0.114 1.92 -4 2 4 18.70 27.40 2.95 0.102 1.50 3 -7 2 27.39 18.72 2.91 0.084 1.23 -7 -4 4 4.49 9.43 2.90 0.060 0.84 2 1 3 17.25 11.14 2.88 0.065 1.81 -1 -1 1 1888.96 2275.46 2.82 0.925 4.78 4 -8 3 2.10 5.74 2.75 0.046 1.05 -2 0 5 6.62 3.50 2.74 0.036 1.76 3 -9 4 18.36 27.10 2.74 0.101 0.96 1 0 1 1129.32 1350.13 2.73 0.713 5.07 -3 5 0 1.65 0.00 2.70 0.001 1.59 1 -9 5 25.29 35.84 2.70 0.116 0.94 6 -2 2 8.78 14.07 2.70 0.073 1.20 -3 -2 4 1.46 3.96 2.66 0.039 1.69 -4 2 0 274.15 330.57 2.66 0.353 1.92 3 5 3 9.23 14.94 2.64 0.075 0.95 3 -1 6 8.79 13.96 2.62 0.072 1.22 1 -2 6 5.62 9.84 2.61 0.061 1.52 3 -2 3 188.02 155.62 2.61 0.242 1.90 5 -3 1 28.31 20.56 2.59 0.088 1.48 -1 -1 3 91.75 113.33 2.58 0.206 3.02 -1 7 3 2.00 6.38 2.57 0.049 0.97 -2 1 0 783.99 927.38 2.57 0.591 3.83 -3 2 5 18.62 12.95 2.54 0.070 1.45 Bond lengths and angles C1 - Distance Angles C2 1.4874 (0.0020) H1A 0.9800 109.47 H1B 0.9800 109.47 109.47 H1C 0.9800 109.47 109.47 109.47 C1 - C2 H1A H1B C2 - Distance Angles O2 1.1937 (0.0018) O3 1.3861 (0.0017) 121.91 (0.13) C1 1.4874 (0.0020) 128.14 (0.13) 109.95 (0.12) C2 - O2 O3 C4 - Distance Angles C9 1.3888 (0.0019) C5 1.3889 (0.0020) 121.10 (0.13) O3 1.3894 (0.0016) 117.43 (0.12) 121.19 (0.12) C4 - C9 C5 C5 - Distance Angles C6 1.3862 (0.0020) C4 1.3889 (0.0020) 119.84 (0.13) H5 0.9500 120.08 120.08 C5 - C6 C4 C6 - Distance Angles C5 1.3862 (0.0020) C7 1.3893 (0.0020) 119.54 (0.13) H6 0.9500 120.23 120.23 C6 - C5 C7 C7 - Distance Angles C8 1.3881 (0.0020) O14 1.3893 (0.0016) 117.83 (0.12) C6 1.3893 (0.0020) 121.29 (0.13) 120.82 (0.12) C7 - C8 O14 C8 - Distance Angles C7 1.3881 (0.0020) C9 1.4112 (0.0019) 119.08 (0.12) C12 1.4377 (0.0020) 120.21 (0.13) 120.69 (0.12) C8 - C7 C9 C9 - Distance Angles C4 1.3888 (0.0019) C8 1.4112 (0.0019) 119.13 (0.12) C10 1.4389 (0.0020) 120.62 (0.12) 120.25 (0.12) C9 - C4 C8 C10 - Distance Angles N11 1.1466 (0.0020) C9 1.4389 (0.0020) 178.87 (0.16) C10 - N11 C12 - Distance Angles N13 1.1477 (0.0020) C8 1.4377 (0.0020) 178.53 (0.16) C12 - N13 C15 - Distance Angles O15 1.1972 (0.0017) O14 1.3827 (0.0017) 121.64 (0.12) C16 1.4868 (0.0019) 127.58 (0.13) 110.76 (0.11) C15 - O15 O14 C16 - Distance Angles C15 1.4868 (0.0019) H16A 0.9800 109.47 H16B 0.9800 109.47 109.47 H16C 0.9800 109.47 109.47 109.47 C16 - C15 H16A H16B N11 - Distance Angles C10 1.1466 (0.0020) N11 - N13 - Distance Angles C12 1.1477 (0.0020) N13 - O2 - Distance Angles C2 1.1937 (0.0018) O2 - O3 - Distance Angles C2 1.3861 (0.0017) C4 1.3894 (0.0016) 117.84 (0.10) O3 - C2 O14 - Distance Angles C15 1.3827 (0.0016) C7 1.3893 (0.0016) 116.35 (0.10) O14 - C15 O15 - Distance Angles C15 1.1972 (0.0017) O15 - FMAP and GRID set by program FMAP 2 1 21 GRID -2.778 -2 -2 2.778 2 2 R1 = 0.0544 for 2622 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.38 at 0.4384 0.1990 0.6281 [ 0.92 A from H16B ] Deepest hole -0.33 at 0.3591 0.8920 0.3597 [ 0.11 A from H16A ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 1771 / 17535 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5616 0.8010 0.3719 1.00000 0.05 0.38 0.92 H16B 0.97 H16C 1.02 C16 1.89 H16A Q2 1 0.3774 0.8506 0.4415 1.00000 0.05 0.32 0.96 H16A 1.01 H16C 1.10 C16 1.96 H16B Q3 1 0.4455 0.8775 0.2766 1.00000 0.05 0.26 0.89 H16B 1.03 C16 1.03 H16A 1.91 H16C Q4 1 0.2027 0.3621 -0.0025 1.00000 0.05 0.23 0.70 C6 0.82 C7 1.42 H6 1.80 C5 Q5 1 0.0810 0.1237 -0.1526 1.00000 0.05 0.23 0.70 C4 0.76 C5 1.51 H5 1.79 C9 Q6 1 0.1430 0.2748 -0.1198 1.00000 0.05 0.20 0.67 C6 0.74 C5 1.48 H6 1.53 H5 Q7 1 0.1460 -0.3695 -0.1122 1.00000 0.05 0.19 1.55 N11 1.64 H6 2.27 C10 2.28 O15 Q8 1 0.1964 0.0647 -0.1155 1.00000 0.05 0.19 0.73 C4 0.78 C9 1.84 O3 1.85 C5 Q9 1 0.2809 0.3032 0.0765 1.00000 0.05 0.19 0.74 C7 0.76 C8 1.85 C6 1.86 O14 Q10 1 0.2470 -0.0130 -0.0246 1.00000 0.05 0.15 0.63 C10 0.81 C9 1.77 N11 1.93 C4 Shortest distances between peaks (including symmetry equivalents) 4 6 1.10 5 6 1.18 5 8 1.23 4 9 1.24 8 10 1.35 1 3 1.63 1 2 1.76 2 3 1.79 6 9 1.97 4 5 1.99 6 8 2.01 8 9 2.17 5 9 2.31 5 10 2.47 4 8 2.47 2 2 2.53 9 10 2.55 7 10 2.79 2 3 2.85 1 2 2.88 4 7 2.98 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. 0.63: 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 0.61: Structure factors and derivatives 0.97: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.23: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0189 finished at 14:41:25 Total CPU time: 2.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++