+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 17:32:38 on 04-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01SRC105 in Iba2 CELL 0.71073 9.2463 33.4610 7.2285 90.000 90.000 90.000 ZERR 8.00 0.0018 0.0067 0.0014 0.000 0.000 0.000 LATT -2 SYMM - X, - Y, Z SYMM 1/2 + X, 1/2 - Y, Z SYMM 1/2 - X, 1/2 + Y, Z SFAC C H N O UNIT 112 104 8 8 V = 2236.43 F(000) = 896.0 Mu = 0.08 mm-1 Cell Wt = 1690.03 Rho = 1.255 MERG 2 OMIT -3.00 55.00 OMIT 0 12 6 EXTI 0.02887 FMAP 2 PLAN 10 SIZE 0.08 0.30 0.60 BOND MOVE 1 1 1 -1 WGHT 0.09690 L.S. 4 TEMP -123.00 FVAR 0.60483 MOLE 1 C1 1 0.185522 0.462604 -0.578599 11.00000 0.07191 0.02499 = 0.04218 0.00897 -0.00593 -0.00099 AFIX 137 H1A 2 0.179716 0.435758 -0.632289 11.00000 -1.50000 H1B 2 0.215684 0.481664 -0.674032 11.00000 -1.50000 H1C 2 0.090464 0.470333 -0.530479 11.00000 -1.50000 AFIX 0 C2 1 0.265176 0.436378 -0.289230 11.00000 0.04097 0.01670 = 0.02966 -0.00134 0.00632 0.00250 C3 1 0.151877 0.409171 -0.282426 11.00000 0.03916 0.02217 = 0.02559 -0.00233 0.00089 0.00154 AFIX 43 H3 2 0.083122 0.407950 -0.379923 11.00000 -1.20000 AFIX 0 C4 1 0.140416 0.383733 -0.130956 11.00000 0.03450 0.01825 = 0.03049 -0.00294 0.00332 -0.00160 AFIX 43 H4 2 0.063453 0.364939 -0.127496 11.00000 -1.20000 AFIX 0 C5 1 0.237347 0.384864 0.014967 11.00000 0.03144 0.01778 = 0.02967 -0.00375 0.00461 -0.00022 C6 1 0.350909 0.412959 0.004871 11.00000 0.03358 0.02416 = 0.03444 -0.00413 -0.00005 -0.00248 AFIX 43 H6 2 0.419560 0.414418 0.102417 11.00000 -1.20000 AFIX 0 C7 1 0.363614 0.438316 -0.144553 11.00000 0.03706 0.02107 = 0.03685 -0.00360 0.00582 -0.00637 AFIX 43 H7 2 0.440190 0.457226 -0.148523 11.00000 -1.20000 AFIX 0 C8 1 0.217260 0.357710 0.171047 11.00000 0.03088 0.01748 = 0.03090 -0.00148 0.00428 -0.00031 AFIX 43 H8 2 0.137425 0.339927 0.162877 11.00000 -1.20000 AFIX 0 C9 1 0.297482 0.354914 0.323351 11.00000 0.03065 0.02030 = 0.03160 -0.00402 0.00232 -0.00061 AFIX 43 H9 2 0.379548 0.371848 0.333743 11.00000 -1.20000 AFIX 0 C10 1 0.267109 0.327307 0.476275 11.00000 0.03287 0.01819 = 0.02882 -0.00636 0.00184 0.00540 C11 1 0.108831 0.284541 0.620940 11.00000 0.03667 0.02081 = 0.03515 0.00112 0.00392 0.00182 AFIX 43 H11 2 0.016399 0.272186 0.625655 11.00000 -1.20000 AFIX 0 C12 1 0.206356 0.275355 0.758384 11.00000 0.04790 0.02350 = 0.03168 0.00322 0.00308 0.00975 AFIX 43 H12 2 0.182159 0.257018 0.853825 11.00000 -1.20000 AFIX 0 C13 1 0.339676 0.293453 0.753649 11.00000 0.04622 0.03209 = 0.03145 -0.00155 -0.00800 0.01221 AFIX 43 H13 2 0.409564 0.287881 0.846468 11.00000 -1.20000 AFIX 0 C14 1 0.370919 0.319924 0.611861 11.00000 0.03462 0.02598 = 0.03452 -0.00697 -0.00266 0.00229 AFIX 43 H14 2 0.462192 0.332919 0.607068 11.00000 -1.20000 AFIX 0 N1 3 0.135476 0.309733 0.480946 11.00000 0.03462 0.02068 = 0.02931 0.00013 0.00141 0.00258 O1 4 0.288236 0.462686 -0.431862 11.00000 0.05764 0.02534 = 0.03624 0.00486 0.00182 -0.00612 HKLF 4 1.0 0.00 1.00 0.00 0.00 0.00 1.00 1.00 0.00 0.00 Covalent radii and connectivity table for 01SRC105 in Iba2 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1 C2 - O1 C7 C3 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 C8 C6 - C7 C5 C7 - C6 C2 C8 - C9 C5 C9 - C8 C10 C10 - N1 C14 C9 C11 - N1 C12 C12 - C13 C11 C13 - C12 C14 C14 - C13 C10 N1 - C11 C10 O1 - C2 C1 Floating origin restraints generated h k l Fo^2 Sigma Why rejected 0 3 1 1.33 0.27 observed but should be systematically absent 0 5 -1 2.21 0.44 observed but should be systematically absent 7443 Reflections read, of which 380 rejected -11 =< h =< 11, -41 =< k =< 43, -8 =< l =< 9, Max. 2-theta = 54.98 2 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 5 4 -5 71.06 2.82 4 14.99 4 5 -5 110.27 2.91 5 19.95 4 7 -5 188.23 5.25 5 37.19 4 9 -5 293.35 8.55 5 56.50 3 1 -4 1014.43 23.60 4 184.02 3 5 -4 101.88 3.46 3 41.05 2 8 -4 236.06 8.62 2 50.58 5 11 -4 530.85 20.56 2 136.22 4 16 -4 398.66 17.73 2 101.18 2 1 -3 683.72 15.59 4 147.46 2 3 -3 434.88 10.52 4 103.85 1 1 -2 52.60 1.82 3 19.77 0 2 2 932.38 43.31 2 375.04 1 6 3 624.66 9.17 6 70.84 0 2 4 178.72 7.99 2 43.41 0 4 4 85.25 3.41 2 39.14 0 6 4 143.71 4.10 3 39.53 1 3 6 42.19 2.84 2 24.52 1 5 6 153.56 7.24 2 46.56 2 16 6 99.64 2.20 5 20.93 1 8 7 12.44 1.53 2 8.25 1 9 8 56.75 3.01 2 38.94 22 Inconsistent equivalents 2481 Unique reflections, of which 0 suppressed R(int) = 0.0717 R(sigma) = 0.0714 Friedel opposites not merged Maximum memory for data reduction = 1513 / 28946 Default effective X-H distances for T = -123.0 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 = 1927 / 184401 wR2 = 0.1474 before cycle 1 for 2481 data and 147 / 147 parameters GooF = S = 1.023; Restrained GooF = 1.023 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0969 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60497 0.00262 0.055 OSF 2 0.02901 0.00501 0.028 EXTI Mean shift/esd = 0.149 Maximum = -0.972 for U33 C13 Max. shift = 0.002 A for H1A Max. dU = 0.000 for C13 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1927 / 184401 wR2 = 0.1471 before cycle 2 for 2481 data and 147 / 147 parameters GooF = S = 1.022; Restrained GooF = 1.021 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0969 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60489 0.00261 -0.032 OSF 2 0.02900 0.00501 -0.002 EXTI Mean shift/esd = 0.051 Maximum = -0.344 for U33 C13 Max. shift = 0.001 A for H1A Max. dU = 0.000 for C13 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1927 / 184401 wR2 = 0.1471 before cycle 3 for 2481 data and 147 / 147 parameters GooF = S = 1.022; Restrained GooF = 1.021 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0969 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60487 0.00261 -0.006 OSF 2 0.02897 0.00501 -0.006 EXTI Mean shift/esd = 0.005 Maximum = 0.033 for z C9 Max. shift = 0.000 A for H1B Max. dU = 0.000 for C13 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1927 / 184401 wR2 = 0.1471 before cycle 4 for 2481 data and 147 / 147 parameters GooF = S = 1.022; Restrained GooF = 1.021 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0969 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60487 0.00261 -0.001 OSF 2 0.02896 0.00500 -0.001 EXTI Mean shift/esd = 0.002 Maximum = 0.010 for z C8 Max. shift = 0.000 A for H1A Max. dU = 0.000 for C2 Largest correlation matrix elements 0.581 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.8201 0.5642 1.6326 137 0.980 0.000 C1 O1 H1A H1B 0.9095 0.5297 1.5307 137 0.980 0.000 C1 O1 H1A H1C 0.7843 0.5183 1.6741 137 0.980 0.000 C1 O1 H1A H3 0.9168 0.5921 1.3803 43 0.950 0.000 C3 C2 C4 H4 0.9366 0.6350 1.1270 43 0.950 0.000 C4 C5 C3 H6 0.5804 0.5856 0.8978 43 0.950 0.000 C6 C7 C5 H7 0.5598 0.5428 1.1482 43 0.950 0.000 C7 C6 C2 H8 0.8626 0.6601 0.8371 43 0.950 0.000 C8 C9 C5 H9 0.6204 0.6282 0.6664 43 0.950 0.000 C9 C8 C10 H11 0.9835 0.7278 0.3745 43 0.950 0.000 C11 N1 C12 H12 0.8179 0.7429 0.1461 43 0.950 0.000 C12 C13 C11 H13 0.5904 0.7122 0.1538 43 0.950 0.000 C13 C12 C14 H14 0.5378 0.6671 0.3926 43 0.950 0.000 C14 C13 C10 01SRC105 in Iba2 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.81442 0.53740 1.57878 1.00000 0.07241 0.02480 0.04106 0.00882 -0.00555 -0.00110 0.04609 0.00443 0.00033 0.00007 0.00035 0.00000 0.00166 0.00119 0.00129 0.00099 0.00126 0.00117 0.00064 H1A 0.82012 0.56424 1.63256 1.00000 0.06914 0.00000 0.00000 H1B 0.90953 0.52970 1.53071 1.00000 0.06914 0.00000 0.00000 H1C 0.78427 0.51832 1.67413 1.00000 0.06914 0.00000 0.00000 C2 0.73483 0.56362 1.28926 1.00000 0.04106 0.01671 0.02923 -0.00082 0.00622 0.00257 0.02900 0.00360 0.00022 0.00006 0.00028 0.00000 0.00116 0.00091 0.00114 0.00081 0.00099 0.00080 0.00050 C3 0.84813 0.59083 1.28269 1.00000 0.03909 0.02200 0.02660 -0.00274 0.00091 0.00148 0.02923 0.00347 0.00022 0.00006 0.00029 0.00000 0.00110 0.00093 0.00098 0.00082 0.00095 0.00083 0.00047 H3 0.91678 0.59210 1.38030 1.00000 0.03507 0.00000 0.00000 C4 0.85956 0.61626 1.13067 1.00000 0.03458 0.01832 0.02994 -0.00345 0.00328 -0.00164 0.02762 0.00350 0.00021 0.00006 0.00029 0.00000 0.00112 0.00095 0.00106 0.00078 0.00088 0.00079 0.00048 H4 0.93662 0.63502 1.12699 1.00000 0.03314 0.00000 0.00000 C5 0.76262 0.61513 0.98491 1.00000 0.03130 0.01784 0.03014 -0.00400 0.00467 -0.00025 0.02643 0.00339 0.00021 0.00006 0.00028 0.00000 0.00103 0.00093 0.00109 0.00078 0.00091 0.00079 0.00047 C6 0.64913 0.58705 0.99524 1.00000 0.03393 0.02425 0.03324 -0.00415 -0.00011 -0.00244 0.03047 0.00358 0.00022 0.00006 0.00031 0.00000 0.00106 0.00098 0.00112 0.00087 0.00094 0.00083 0.00049 H6 0.58041 0.58560 0.89776 1.00000 0.03657 0.00000 0.00000 C7 0.63636 0.56169 1.14436 1.00000 0.03692 0.02105 0.03717 -0.00294 0.00569 -0.00633 0.03172 0.00370 0.00023 0.00006 0.00031 0.00000 0.00120 0.00098 0.00115 0.00091 0.00097 0.00085 0.00051 H7 0.55980 0.54277 1.14818 1.00000 0.03806 0.00000 0.00000 C8 0.78273 0.64231 0.82890 1.00000 0.03091 0.01741 0.03089 -0.00141 0.00408 -0.00029 0.02640 0.00349 0.00023 0.00006 0.00028 0.00000 0.00099 0.00095 0.00110 0.00077 0.00085 0.00078 0.00046 H8 0.86257 0.66009 0.83711 1.00000 0.03168 0.00000 0.00000 C9 0.70253 0.64512 0.67665 1.00000 0.03057 0.02031 0.03170 -0.00410 0.00235 -0.00066 0.02753 0.00358 0.00023 0.00006 0.00029 0.00000 0.00108 0.00095 0.00114 0.00081 0.00088 0.00078 0.00048 H9 0.62040 0.62820 0.66635 1.00000 0.03304 0.00000 0.00000 C10 0.73290 0.67269 0.52360 1.00000 0.03311 0.01818 0.02804 -0.00621 0.00183 0.00538 0.02644 0.00351 0.00022 0.00006 0.00028 0.00000 0.00106 0.00092 0.00104 0.00077 0.00088 0.00081 0.00046 C11 0.89115 0.71546 0.37914 1.00000 0.03682 0.02074 0.03506 0.00077 0.00392 0.00168 0.03087 0.00378 0.00023 0.00006 0.00030 0.00000 0.00115 0.00096 0.00112 0.00086 0.00097 0.00084 0.00048 H11 0.98355 0.72784 0.37449 1.00000 0.03705 0.00000 0.00000 C12 0.79365 0.72462 0.24167 1.00000 0.04784 0.02349 0.03163 0.00289 0.00281 0.00977 0.03432 0.00414 0.00024 0.00006 0.00033 0.00000 0.00135 0.00097 0.00111 0.00090 0.00098 0.00094 0.00053 H12 0.81789 0.74293 0.14611 1.00000 0.04119 0.00000 0.00000 C13 0.66032 0.70655 0.24651 1.00000 0.04664 0.03217 0.02985 -0.00157 -0.00771 0.01229 0.03622 0.00407 0.00026 0.00007 0.00031 0.00000 0.00133 0.00110 0.00118 0.00096 0.00105 0.00102 0.00055 H13 0.59038 0.71216 0.15382 1.00000 0.04347 0.00000 0.00000 C14 0.62909 0.68008 0.38794 1.00000 0.03458 0.02594 0.03466 -0.00630 -0.00275 0.00229 0.03172 0.00364 0.00023 0.00006 0.00030 0.00000 0.00112 0.00099 0.00113 0.00087 0.00091 0.00089 0.00049 H14 0.53784 0.66707 0.39260 1.00000 0.03807 0.00000 0.00000 N1 0.86453 0.69026 0.51912 1.00000 0.03464 0.02062 0.02969 0.00018 0.00142 0.00260 0.02832 0.00285 0.00018 0.00005 0.00023 0.00000 0.00096 0.00082 0.00091 0.00070 0.00080 0.00070 0.00042 O1 0.71173 0.53731 1.43189 1.00000 0.05801 0.02528 0.03573 0.00491 0.00173 -0.00616 0.03967 0.00278 0.00018 0.00004 0.00023 0.00000 0.00104 0.00080 0.00083 0.00065 0.00078 0.00071 0.00045 Final Structure Factor Calculation for 01SRC105 in Iba2 Total number of l.s. parameters = 147 Maximum vector length = 511 Memory required = 1782 / 25046 wR2 = 0.1471 before cycle 5 for 2481 data and 2 / 147 parameters GooF = S = 1.022; Restrained GooF = 1.021 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0969 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0576 for 2017 Fo > 4sig(Fo) and 0.0722 for all 2481 data wR2 = 0.1471, GooF = S = 1.022, Restrained GooF = 1.021 for all data Flack x parameter = 0.1038 with esd 1.8656 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 16.00 for non-hydrogen and 13.00 for hydrogen atoms Principal mean square atomic displacements U 0.0735 0.0439 0.0209 C1 0.0439 0.0269 0.0163 C2 0.0393 0.0279 0.0206 C3 0.0368 0.0287 0.0173 C4 0.0359 0.0268 0.0166 C5 0.0354 0.0338 0.0222 C6 0.0446 0.0318 0.0188 C7 0.0351 0.0269 0.0173 C8 0.0345 0.0291 0.0190 C9 0.0348 0.0309 0.0136 C10 0.0401 0.0319 0.0206 C11 0.0519 0.0313 0.0198 C12 0.0558 0.0291 0.0237 C13 0.0402 0.0324 0.0226 C14 0.0355 0.0293 0.0201 N1 0.0592 0.0377 0.0222 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.027 0.042 0.056 0.072 0.088 0.107 0.134 0.173 0.247 1.000 Number in group 248. 272. 238. 248. 251. 232. 250. 244. 248. 250. GooF 0.889 0.979 0.990 1.049 1.055 0.951 1.062 0.972 1.077 1.161 K 1.083 1.030 1.023 1.039 0.988 1.006 0.993 1.002 1.043 1.037 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 256. 246. 242. 256. 252. 242. 244. 245. 252. 246. GooF 1.113 0.951 1.062 0.932 0.873 0.884 1.009 1.019 1.169 1.151 K 0.987 0.999 0.989 0.994 1.014 1.037 1.085 1.066 1.070 1.000 R1 0.174 0.142 0.126 0.080 0.060 0.052 0.055 0.048 0.054 0.049 Recommended weighting scheme: WGHT 0.0950 0.0000 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 11 8 323.35 163.95 4.39 0.097 0.86 7 12 7 161.40 76.90 3.53 0.066 0.78 1 42 -1 347.07 546.30 3.38 0.177 0.79 3 35 -2 141.54 257.97 3.30 0.122 0.89 0 22 -2 1988.01 1412.59 3.22 0.284 1.40 0 8 6 227.20 334.31 3.15 0.138 1.16 2 39 -1 275.33 412.35 3.09 0.154 0.84 2 6 0 88.85 124.39 3.02 0.084 3.56 1 2 -5 14.77 4.86 2.99 0.017 1.42 1 1 6 4.41 23.33 2.97 0.037 1.19 1 7 0 22.12 30.89 2.90 0.042 4.25 5 3 6 161.28 235.10 2.89 0.116 1.01 0 42 2 98.53 1.41 2.89 0.009 0.78 2 35 -3 46.82 102.04 2.89 0.076 0.87 5 17 -4 1729.45 1179.13 2.89 0.260 1.08 0 24 0 48.43 27.97 2.87 0.040 1.39 4 11 7 81.14 39.51 2.86 0.048 0.90 10 1 3 -4.45 44.64 2.84 0.051 0.86 5 11 -8 170.04 85.77 2.82 0.070 0.78 4 18 0 725.26 543.63 2.81 0.176 1.45 4 34 -4 140.84 208.09 2.80 0.109 0.81 3 36 3 5.59 52.81 2.79 0.055 0.83 2 24 0 159.91 108.64 2.78 0.079 1.33 3 33 -4 44.99 91.04 2.75 0.072 0.85 5 19 0 425.19 312.24 2.74 0.134 1.28 3 41 0 175.62 261.63 2.73 0.122 0.79 5 12 -7 44.47 102.26 2.73 0.077 0.86 2 8 0 242.01 321.99 2.73 0.136 3.10 1 42 1 390.04 545.78 2.71 0.177 0.79 0 22 2 1880.32 1411.50 2.71 0.284 1.40 9 2 5 427.55 302.94 2.69 0.132 0.84 1 14 -7 7.42 21.01 2.67 0.035 0.94 2 2 0 1059.49 1390.98 2.65 0.282 4.46 2 1 -1 725.59 953.95 2.65 0.234 3.87 2 1 1 723.94 953.38 2.64 0.234 3.87 10 18 2 30.80 71.74 2.55 0.064 0.81 1 20 3 229.51 178.90 2.54 0.101 1.36 3 1 -6 80.70 49.59 2.53 0.053 1.12 3 24 -5 725.59 552.32 2.53 0.178 0.95 4 39 1 217.36 316.55 2.52 0.135 0.80 4 6 -4 14.90 8.12 2.52 0.022 1.38 3 21 -4 1978.79 1427.81 2.50 0.286 1.11 3 3 0 334.00 431.61 2.50 0.157 2.97 2 41 -1 138.42 204.75 2.50 0.108 0.80 3 11 -8 620.72 440.58 2.49 0.159 0.83 4 11 3 132.82 174.78 2.49 0.100 1.46 1 29 -6 -13.34 21.57 2.47 0.035 0.83 2 0 -2 11.34 6.72 2.44 0.020 2.85 1 16 -3 691.85 541.37 2.44 0.176 1.56 3 7 0 239.33 308.10 2.43 0.133 2.59 Bond lengths and angles C1 - Distance Angles O1 1.4245 (0.0031) C1 - C2 - Distance Angles O1 1.3723 (0.0025) C7 1.3893 (0.0030) 115.76 (0.17) C3 1.3890 (0.0028) 124.31 (0.19) 119.93 (0.18) C2 - O1 C7 C3 - Distance Angles C2 1.3890 (0.0028) C4 1.3937 (0.0030) 118.97 (0.19) C3 - C2 C4 - Distance Angles C5 1.3839 (0.0029) C3 1.3937 (0.0030) 122.32 (0.18) C4 - C5 C5 - Distance Angles C4 1.3839 (0.0029) C6 1.4107 (0.0027) 117.36 (0.19) C8 1.4605 (0.0027) 119.24 (0.18) 123.39 (0.19) C5 - C4 C6 C6 - Distance Angles C7 1.3768 (0.0030) C5 1.4107 (0.0027) 121.05 (0.20) C6 - C7 C7 - Distance Angles C6 1.3768 (0.0030) C2 1.3893 (0.0030) 120.36 (0.18) C7 - C6 C8 - Distance Angles C9 1.3304 (0.0028) C5 1.4605 (0.0027) 127.71 (0.18) C8 - C9 C9 - Distance Angles C8 1.3304 (0.0028) C10 1.4677 (0.0028) 124.14 (0.18) C9 - C8 C10 - Distance Angles N1 1.3520 (0.0026) C14 1.3943 (0.0029) 121.72 (0.19) C9 1.4677 (0.0028) 117.62 (0.19) 120.66 (0.18) C10 - N1 C14 C11 - Distance Angles N1 1.3400 (0.0026) C12 1.3763 (0.0032) 124.40 (0.21) C11 - N1 C12 - Distance Angles C13 1.3737 (0.0034) C11 1.3763 (0.0032) 118.13 (0.20) C12 - C13 C13 - Distance Angles C12 1.3737 (0.0034) C14 1.3831 (0.0030) 119.22 (0.20) C13 - C12 C14 - Distance Angles C13 1.3831 (0.0031) C10 1.3943 (0.0029) 119.32 (0.20) C14 - C13 N1 - Distance Angles C11 1.3400 (0.0026) C10 1.3520 (0.0026) 117.20 (0.18) N1 - C11 O1 - Distance Angles C2 1.3723 (0.0025) C1 1.4245 (0.0031) 117.06 (0.18) O1 - C2 FMAP and GRID set by program FMAP 2 1 13 GRID -2.500 -1 -2 2.500 1 2 R1 = 0.0623 for 1381 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.21 at 0.0994 0.0397 0.9008 [ 1.07 A from O1 ] Deepest hole -0.27 at 0.2330 0.0395 0.7788 [ 0.81 A from C2 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2371 / 24946 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5994 0.5397 1.4008 1.00000 0.05 0.21 1.07 O1 1.69 C2 1.87 H7 2.02 C7 Q2 1 0.7374 0.7187 0.2905 1.00000 0.05 0.19 0.66 C12 0.88 C13 1.52 H12 1.56 C11 Q3 1 0.6644 0.5664 1.2448 1.00000 0.05 0.18 0.73 C2 0.79 C7 1.43 H7 1.72 O1 Q4 1 0.8004 0.5354 1.4495 1.00000 0.05 0.17 0.83 O1 0.95 C1 1.18 H1B 1.61 C2 Q5 1 0.6030 0.6408 0.6841 1.00000 0.05 0.17 0.47 H9 0.93 C9 1.96 C8 1.98 C10 Q6 1 0.8324 0.6095 1.0370 1.00000 0.05 0.17 0.76 C4 0.77 C5 1.44 H4 1.88 C6 Q7 1 0.6948 0.6451 0.8204 1.00000 0.05 0.16 0.82 C8 1.04 C9 1.43 H9 1.63 H8 Q8 1 0.7114 0.5609 1.2210 1.00000 0.05 0.16 0.55 C2 0.89 C7 1.62 H7 1.67 C3 Q9 1 0.7324 0.7193 0.5368 1.00000 0.05 0.16 1.56 C10 1.56 H12 1.57 N1 1.86 C11 Q10 1 0.7846 0.6390 0.7184 1.00000 0.05 0.16 0.81 C8 0.84 C9 1.32 H8 1.61 H9 Shortest distances between peaks (including symmetry equivalents) 3 8 0.50 7 10 1.13 5 7 1.31 1 3 1.56 5 10 1.70 2 9 1.78 1 8 1.81 1 4 1.90 4 8 2.03 3 4 2.20 6 7 2.34 6 8 2.38 6 10 2.54 3 6 2.60 2 9 2.78 Time profile in seconds ----------------------- 0.19: 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. 1.06: 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 0.86: Structure factors and derivatives 0.58: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.08: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 17:32:42 Total CPU time: 3.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++