+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 15:36:03 on 03-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01ESP002 IN P212121 CELL 0.71073 8.4889 11.5350 31.9275 90 90 90 ZERR 4 0.0002 0.0002 0.0006 0 0 0 LATT -1 SYMM 1/2+X, 1/2-Y, -Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2-X, -Y, 1/2+Z SFAC C H N O CL UNIT 104 132 16 48 4 V = 3126.32 F(000) = 1320.0 Mu = 0.19 mm-1 Cell Wt = 2516.06 Rho = 1.336 SHEL 7 0.84 TEMP -153 SIZE 0.1 0.05 0.05 HTAB HTAB N4 O5 FMAP 2 PLAN 55 BOND L.S. 4 WGHT 0.056700 EXTI 0.006684 FVAR 0.24013 N1 3 -0.056282 -0.240854 0.365654 11.00000 0.02388 0.02142 = 0.02283 0.00046 0.00362 0.00593 N2 3 0.005423 -0.351087 0.372333 11.00000 0.02297 0.01693 = 0.02915 -0.00117 0.00018 0.00322 N3 3 0.243604 -0.542574 0.317302 11.00000 0.02435 0.02118 = 0.02601 -0.00346 -0.00027 -0.00001 N4 3 0.325035 -0.644408 0.319501 11.00000 0.02949 0.02445 = 0.02407 -0.00025 0.00641 0.00648 AFIX 43 H4A 2 0.318460 -0.688816 0.341844 11.00000 -1.20000 AFIX 0 O1 4 -0.223954 -0.102283 0.385297 11.00000 0.02992 0.02487 = 0.03321 0.00061 0.00615 0.00623 O2 4 -0.223418 -0.271210 0.421415 11.00000 0.03029 0.02571 = 0.02793 0.00099 0.00451 -0.00042 O3 4 0.431484 -0.621766 0.253865 11.00000 0.03640 0.03746 = 0.02939 0.00090 0.00630 0.00528 O4 4 0.491419 -0.774556 0.296233 11.00000 0.03282 0.02925 = 0.03911 -0.00332 0.01149 0.01083 O5 4 0.159413 -0.686401 0.390002 11.00000 0.02286 0.01578 = 0.03406 0.00023 0.00170 -0.00071 O6 4 -0.101318 -0.705787 0.394931 11.00000 0.02779 0.03394 = 0.15012 -0.00999 -0.00125 -0.00581 O7 4 0.424357 -0.540610 0.405990 11.00000 0.02060 0.02171 = 0.02859 -0.00064 0.00401 0.00054 O8 4 0.442785 -0.358204 0.380550 11.00000 0.03141 0.03383 = 0.04418 0.01063 -0.00111 -0.00745 O9 4 0.107746 -0.539693 0.481317 11.00000 0.02440 0.01917 = 0.02904 -0.00011 0.00623 -0.00074 O10 4 0.040795 -0.724670 0.492589 11.00000 0.04289 0.02135 = 0.11772 0.01584 0.02755 0.00036 O11 4 0.397372 -0.408953 0.492499 11.00000 0.02798 0.01569 = 0.03086 0.00198 -0.00335 -0.00379 O12 4 0.582556 -0.410920 0.542896 11.00000 0.03552 0.03260 = 0.03791 0.00465 -0.01077 -0.00026 CL1 5 0.196005 0.087148 0.239597 11.00000 0.05450 0.04055 = 0.03335 0.01266 0.00360 -0.00614 C1 1 0.161080 -0.129700 0.336600 11.00000 0.02462 0.02838 = 0.02049 0.00115 -0.00396 0.00247 AFIX 43 H1 2 0.226460 -0.158285 0.358430 11.00000 -1.20000 AFIX 0 C2 1 0.221528 -0.053987 0.307055 11.00000 0.02710 0.02621 = 0.02999 -0.00443 0.00179 0.00061 AFIX 43 H2 2 0.328966 -0.031110 0.308081 11.00000 -1.20000 AFIX 0 C3 1 0.122760 -0.011998 0.275905 11.00000 0.04149 0.02403 = 0.01886 0.00230 0.00259 -0.00330 C4 1 -0.031713 -0.046629 0.273347 11.00000 0.03671 0.02420 = 0.02256 0.00111 -0.00183 0.00891 AFIX 43 H4 2 -0.097582 -0.017532 0.251711 11.00000 -1.20000 AFIX 0 C5 1 -0.091094 -0.124320 0.302517 11.00000 0.02467 0.02352 = 0.02664 -0.00259 -0.00176 0.00151 AFIX 43 H5 2 -0.197145 -0.150056 0.300559 11.00000 -1.20000 AFIX 0 C6 1 0.003860 -0.163795 0.334172 11.00000 0.02298 0.01911 = 0.02500 -0.00024 0.00329 -0.00012 C7 1 -0.174549 -0.209514 0.393692 11.00000 0.02730 0.02238 = 0.02092 -0.00552 -0.00063 0.00332 C8 1 -0.366605 -0.067365 0.407778 11.00000 0.02889 0.03668 = 0.02909 -0.00546 0.00510 0.01369 AFIX 23 H8A 2 -0.345200 -0.061213 0.438178 11.00000 -1.20000 H8B 2 -0.451482 -0.124982 0.403431 11.00000 -1.20000 AFIX 0 C9 1 -0.414378 0.048452 0.390364 11.00000 0.04435 0.04569 = 0.05316 0.00680 0.01139 0.02007 AFIX 33 H9A 2 -0.509234 0.075760 0.404812 11.00000 -1.50000 H9B 2 -0.436252 0.040848 0.360351 11.00000 -1.50000 H9C 2 -0.328802 0.104274 0.394573 11.00000 -1.50000 AFIX 0 C10 1 0.092326 -0.393789 0.343328 11.00000 0.01914 0.02258 = 0.02065 -0.00091 -0.00222 -0.00057 AFIX 43 H10 2 0.110059 -0.351747 0.318180 11.00000 -1.20000 AFIX 0 C11 1 0.163624 -0.507564 0.349363 11.00000 0.01487 0.02059 = 0.02404 -0.00344 -0.00471 -0.00168 C12 1 0.417188 -0.676020 0.286203 11.00000 0.02199 0.02732 = 0.03347 -0.00747 -0.00760 0.00364 C13 1 0.614818 -0.813787 0.267121 11.00000 0.04455 0.03588 = 0.04759 -0.00713 0.01340 0.01712 AFIX 23 H13A 2 0.592815 -0.784134 0.238617 11.00000 -1.20000 H13B 2 0.616379 -0.899547 0.265979 11.00000 -1.20000 AFIX 0 C14 1 0.770099 -0.769844 0.281861 11.00000 0.04339 0.03528 = 0.04639 0.00091 0.01451 0.00416 AFIX 33 H14A 2 0.852960 -0.795987 0.262689 11.00000 -1.50000 H14B 2 0.791319 -0.799698 0.310039 11.00000 -1.50000 H14C 2 0.768243 -0.684918 0.282559 11.00000 -1.50000 AFIX 0 C15 1 0.146056 -0.561871 0.392167 11.00000 0.02222 0.01329 = 0.03020 -0.00296 0.00279 0.00600 AFIX 13 H15 2 0.039527 -0.541849 0.403411 11.00000 -1.20000 AFIX 0 C16 1 0.024228 -0.749129 0.390954 11.00000 0.03315 0.02116 = 0.03732 -0.00424 -0.00670 -0.00460 C17 1 0.058994 -0.875139 0.387321 11.00000 0.03908 0.02139 = 0.04557 -0.00186 0.00164 -0.00961 AFIX 33 H17A 2 0.172919 -0.886483 0.384520 11.00000 -1.50000 H17B 2 0.005609 -0.906641 0.362600 11.00000 -1.50000 H17C 2 0.021355 -0.915300 0.412450 11.00000 -1.50000 AFIX 0 C18 1 0.270071 -0.516290 0.422382 11.00000 0.01576 0.02160 = 0.02369 -0.00428 0.00247 0.00237 AFIX 13 H18 2 0.257226 -0.430515 0.425385 11.00000 -1.20000 AFIX 0 C19 1 0.499499 -0.453102 0.384847 11.00000 0.02650 0.03461 = 0.02216 0.00131 0.00029 -0.00765 C20 1 0.651931 -0.494233 0.367509 11.00000 0.03112 0.05029 = 0.04089 -0.00703 0.01080 -0.01380 AFIX 33 H20A 2 0.669158 -0.575053 0.375791 11.00000 -1.50000 H20B 2 0.737671 -0.446005 0.378412 11.00000 -1.50000 H20C 2 0.649543 -0.488781 0.336884 11.00000 -1.50000 AFIX 0 C21 1 0.261214 -0.572080 0.465398 11.00000 0.01757 0.01579 = 0.02988 -0.00020 0.00190 0.00233 AFIX 13 H21 2 0.266097 -0.658265 0.462271 11.00000 -1.20000 AFIX 0 C22 1 0.005523 -0.623807 0.492069 11.00000 0.02336 0.02765 = 0.03478 0.00505 -0.00038 -0.00521 C23 1 -0.152640 -0.574007 0.501320 11.00000 0.02757 0.03447 = 0.05772 -0.00006 0.00809 -0.00728 AFIX 33 H23A 2 -0.147974 -0.489344 0.499082 11.00000 -1.50000 H23B 2 -0.184427 -0.595716 0.529767 11.00000 -1.50000 H23C 2 -0.229551 -0.604205 0.481196 11.00000 -1.50000 AFIX 0 C24 1 0.388404 -0.533217 0.495215 11.00000 0.02636 0.01514 = 0.02700 0.00207 0.00139 0.00118 AFIX 23 H24A 2 0.362318 -0.557179 0.524170 11.00000 -1.20000 H24B 2 0.490639 -0.568355 0.487376 11.00000 -1.20000 AFIX 0 C25 1 0.507991 -0.358415 0.517173 11.00000 0.02264 0.02406 = 0.02765 -0.00489 0.00671 -0.00297 C26 1 0.526312 -0.232411 0.507234 11.00000 0.03797 0.02297 = 0.03304 -0.00423 0.00546 -0.00706 AFIX 33 H26A 2 0.451962 -0.210793 0.485090 11.00000 -1.50000 H26B 2 0.634179 -0.217515 0.497712 11.00000 -1.50000 H26C 2 0.504799 -0.186372 0.532389 11.00000 -1.50000 HKLF 4 Covalent radii and connectivity table for 01ESP002 IN P212121 C 0.770 H 0.320 N 0.700 O 0.660 CL 0.990 N1 - N2 C7 C6 N2 - C10 N1 N3 - C11 N4 N4 - N3 C12 O1 - C7 C8 O2 - C7 O3 - C12 O4 - C12 C13 O5 - C16 C15 O6 - C16 O7 - C19 C18 O8 - C19 O9 - C22 C21 O10 - C22 O11 - C25 C24 O12 - C25 Cl1 - C3 C1 - C2 C6 C2 - C1 C3 C3 - C4 C2 Cl1 C4 - C3 C5 C5 - C6 C4 C6 - C5 C1 N1 C7 - O2 O1 N1 C8 - O1 C9 C9 - C8 C10 - N2 C11 C11 - N3 C10 C15 C12 - O3 O4 N4 C13 - O4 C14 C14 - C13 C15 - O5 C11 C18 C16 - O6 O5 C17 C17 - C16 C18 - O7 C21 C15 C19 - O8 O7 C20 C20 - C19 C21 - O9 C24 C18 C22 - O10 O9 C23 C23 - C22 C24 - O11 C21 C25 - O12 O11 C26 C26 - C25 11451 Reflections read, of which 1758 rejected -10 =< h =< 10, -13 =< k =< 13, -35 =< l =< 38, Max. 2-theta = 50.05 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 1 0 824.49 30.08 2 263.40 1 1 1 149.98 3.20 3 90.91 -1 2 1 28.10 0.65 4 4.77 -1 1 2 39.20 0.12 3 209.02 1 1 2 437.87 13.10 3 83.40 -1 2 2 713.31 11.36 3 232.95 -2 4 2 17.44 0.31 4 4.87 -3 7 2 50.32 0.64 3 25.24 -2 4 3 50.87 0.33 4 27.04 4 6 3 44.08 0.56 3 33.45 -3 7 3 35.84 0.81 3 13.91 4 7 3 28.66 0.76 3 10.57 -3 8 3 43.15 0.95 3 22.80 -2 2 4 158.40 1.79 3 73.11 -2 4 4 12.73 0.21 4 4.52 -3 8 4 8.19 0.74 3 4.02 -2 2 5 201.28 0.24 4 386.32 -2 3 5 7.55 0.21 4 3.12 -2 3 6 47.25 0.22 5 14.51 -2 4 6 114.87 0.34 5 31.41 -3 3 8 4.13 0.23 4 2.46 -3 3 9 137.71 0.48 3 106.69 -3 4 9 36.11 0.46 3 20.03 -3 7 9 5.74 0.53 3 3.78 -3 4 10 34.11 0.46 3 17.75 -3 5 10 5.09 0.44 3 4.61 -3 6 10 5.44 0.53 3 4.64 -3 6 11 13.31 0.55 3 9.52 -3 7 11 1.91 0.56 2 5.12 -4 5 14 24.97 0.69 3 13.40 30 Inconsistent equivalents 5286 Unique reflections, of which 0 suppressed R(int) = 0.0763 R(sigma) = 0.0996 Friedel opposites not merged Maximum memory for data reduction = 3430 / 53471 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 = 4533 / 498208 wR2 = 0.1224 before cycle 1 for 5286 data and 389 / 389 parameters GooF = S = 0.988; Restrained GooF = 0.988 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0567 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24013 0.00052 0.002 OSF 2 0.00668 0.00097 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.006 for z Cl1 Max. shift = 0.000 A for C6 Max. dU = 0.000 for O8 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4533 / 498208 wR2 = 0.1224 before cycle 2 for 5286 data and 389 / 389 parameters GooF = S = 0.988; Restrained GooF = 0.988 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0567 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24013 0.00052 0.002 OSF 2 0.00668 0.00096 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for z Cl1 Max. shift = 0.000 A for C6 Max. dU = 0.000 for O8 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4533 / 498208 wR2 = 0.1224 before cycle 3 for 5286 data and 389 / 389 parameters GooF = S = 0.988; Restrained GooF = 0.988 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0567 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24013 0.00052 -0.001 OSF 2 0.00668 0.00096 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for C13 Max. dU = 0.000 for C3 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4533 / 498208 wR2 = 0.1224 before cycle 4 for 5286 data and 389 / 389 parameters GooF = S = 0.988; Restrained GooF = 0.988 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0567 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24013 0.00052 0.000 OSF 2 0.00668 0.00096 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O12 Max. shift = 0.000 A for N3 Max. dU = 0.000 for O2 Largest correlation matrix elements 0.559 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H4A 0.3185 -0.6888 0.3418 43 0.880 0.000 N4 N3 C12 H1 0.2265 -0.1583 0.3584 43 0.950 0.000 C1 C2 C6 H2 0.3290 -0.0311 0.3081 43 0.950 0.000 C2 C1 C3 H4 -0.0976 -0.0175 0.2517 43 0.950 0.000 C4 C3 C5 H5 -0.1971 -0.1501 0.3006 43 0.950 0.000 C5 C6 C4 H8A -0.3452 -0.0612 0.4382 23 0.990 0.000 C8 O1 C9 H8B -0.4515 -0.1250 0.4034 23 0.990 0.000 C8 O1 C9 H9A -0.5092 0.0758 0.4048 33 0.980 0.000 C9 C8 H9A H9B -0.4363 0.0408 0.3604 33 0.980 0.000 C9 C8 H9A H9C -0.3288 0.1043 0.3946 33 0.980 0.000 C9 C8 H9A H10 0.1101 -0.3517 0.3182 43 0.950 0.000 C10 N2 C11 H13A 0.5928 -0.7841 0.2386 23 0.990 0.000 C13 O4 C14 H13B 0.6164 -0.8995 0.2660 23 0.990 0.000 C13 O4 C14 H14A 0.8530 -0.7960 0.2627 33 0.980 0.000 C14 C13 H14A H14B 0.7913 -0.7997 0.3100 33 0.980 0.000 C14 C13 H14A H14C 0.7682 -0.6849 0.2826 33 0.980 0.000 C14 C13 H14A H15 0.0395 -0.5418 0.4034 13 1.000 0.000 C15 O5 C11 C18 H17A 0.1729 -0.8865 0.3845 33 0.980 0.000 C17 C16 H17A H17B 0.0056 -0.9066 0.3626 33 0.980 0.000 C17 C16 H17A H17C 0.0214 -0.9153 0.4125 33 0.980 0.000 C17 C16 H17A H18 0.2572 -0.4305 0.4254 13 1.000 0.000 C18 O7 C21 C15 H20A 0.6692 -0.5751 0.3758 33 0.980 0.000 C20 C19 H20A H20B 0.7377 -0.4460 0.3784 33 0.980 0.000 C20 C19 H20A H20C 0.6495 -0.4888 0.3369 33 0.980 0.000 C20 C19 H20A H21 0.2661 -0.6583 0.4623 13 1.000 0.000 C21 O9 C24 C18 H23A -0.1480 -0.4893 0.4991 33 0.980 0.000 C23 C22 H23A H23B -0.1844 -0.5957 0.5298 33 0.980 0.000 C23 C22 H23A H23C -0.2296 -0.6042 0.4812 33 0.980 0.000 C23 C22 H23A H24A 0.3623 -0.5572 0.5242 23 0.990 0.000 C24 O11 C21 H24B 0.4906 -0.5684 0.4874 23 0.990 0.000 C24 O11 C21 H26A 0.4520 -0.2108 0.4851 33 0.980 0.000 C26 C25 H26A H26B 0.6342 -0.2175 0.4977 33 0.980 0.000 C26 C25 H26A H26C 0.5048 -0.1864 0.5324 33 0.980 0.000 C26 C25 H26A 01ESP002 IN P212121 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq N1 -0.05628 -0.24085 0.36565 1.00000 0.02388 0.02142 0.02283 0.00046 0.00362 0.00593 0.02271 0.00477 0.00032 0.00023 0.00008 0.00000 0.00161 0.00156 0.00155 0.00126 0.00136 0.00131 0.00068 N2 0.00542 -0.35109 0.37233 1.00000 0.02297 0.01693 0.02915 -0.00117 0.00018 0.00322 0.02302 0.00468 0.00032 0.00022 0.00009 0.00000 0.00157 0.00151 0.00171 0.00129 0.00142 0.00134 0.00068 N3 0.24360 -0.54257 0.31730 1.00000 0.02435 0.02118 0.02601 -0.00346 -0.00027 -0.00001 0.02385 0.00461 0.00033 0.00022 0.00009 0.00000 0.00158 0.00150 0.00162 0.00130 0.00137 0.00140 0.00067 N4 0.32504 -0.64441 0.31950 1.00000 0.02949 0.02445 0.02407 -0.00025 0.00641 0.00648 0.02600 0.00488 0.00034 0.00024 0.00009 0.00000 0.00167 0.00157 0.00164 0.00131 0.00143 0.00141 0.00069 H4A 0.31846 -0.68882 0.34184 1.00000 0.03120 0.00000 0.00000 O1 -0.22395 -0.10228 0.38530 1.00000 0.02992 0.02487 0.03321 0.00061 0.00615 0.00623 0.02933 0.00387 0.00027 0.00018 0.00007 0.00000 0.00135 0.00134 0.00143 0.00113 0.00117 0.00116 0.00059 O2 -0.22342 -0.27121 0.42141 1.00000 0.03029 0.02571 0.02793 0.00099 0.00451 -0.00042 0.02798 0.00389 0.00028 0.00019 0.00007 0.00000 0.00147 0.00128 0.00140 0.00119 0.00122 0.00114 0.00059 O3 0.43148 -0.62177 0.25386 1.00000 0.03640 0.03746 0.02939 0.00090 0.00630 0.00528 0.03442 0.00420 0.00028 0.00021 0.00008 0.00000 0.00152 0.00148 0.00150 0.00128 0.00125 0.00129 0.00064 O4 0.49142 -0.77456 0.29623 1.00000 0.03282 0.02925 0.03911 -0.00332 0.01149 0.01083 0.03373 0.00440 0.00029 0.00021 0.00008 0.00000 0.00150 0.00140 0.00155 0.00120 0.00130 0.00127 0.00065 O5 0.15941 -0.68640 0.39000 1.00000 0.02286 0.01578 0.03406 0.00023 0.00170 -0.00071 0.02423 0.00383 0.00026 0.00018 0.00007 0.00000 0.00129 0.00117 0.00144 0.00106 0.00115 0.00107 0.00056 O6 -0.10132 -0.70579 0.39493 1.00000 0.02779 0.03394 0.15012 -0.00999 -0.00125 -0.00581 0.07062 0.00544 0.00035 0.00023 0.00013 0.00000 0.00165 0.00173 0.00353 0.00195 0.00210 0.00153 0.00111 O7 0.42436 -0.54061 0.40599 1.00000 0.02060 0.02171 0.02859 -0.00064 0.00401 0.00054 0.02363 0.00372 0.00025 0.00018 0.00007 0.00000 0.00126 0.00126 0.00133 0.00106 0.00112 0.00107 0.00056 O8 0.44279 -0.35820 0.38055 1.00000 0.03141 0.03383 0.04418 0.01063 -0.00111 -0.00745 0.03648 0.00443 0.00028 0.00023 0.00008 0.00000 0.00151 0.00154 0.00166 0.00130 0.00130 0.00131 0.00067 O9 0.10775 -0.53969 0.48132 1.00000 0.02439 0.01917 0.02904 -0.00011 0.00623 -0.00074 0.02420 0.00380 0.00026 0.00018 0.00007 0.00000 0.00126 0.00124 0.00133 0.00107 0.00113 0.00108 0.00056 O10 0.04079 -0.72467 0.49259 1.00000 0.04289 0.02135 0.11772 0.01584 0.02755 0.00036 0.06065 0.00591 0.00034 0.00022 0.00012 0.00000 0.00181 0.00155 0.00285 0.00169 0.00189 0.00135 0.00096 O11 0.39737 -0.40895 0.49250 1.00000 0.02798 0.01569 0.03086 0.00198 -0.00335 -0.00379 0.02485 0.00374 0.00026 0.00017 0.00007 0.00000 0.00129 0.00117 0.00135 0.00108 0.00115 0.00107 0.00056 O12 0.58256 -0.41092 0.54290 1.00000 0.03552 0.03260 0.03791 0.00465 -0.01077 -0.00026 0.03534 0.00415 0.00029 0.00021 0.00008 0.00000 0.00151 0.00144 0.00152 0.00131 0.00135 0.00127 0.00064 Cl1 0.19600 0.08715 0.23960 1.00000 0.05450 0.04055 0.03335 0.01266 0.00360 -0.00614 0.04280 0.00181 0.00012 0.00008 0.00003 0.00000 0.00066 0.00058 0.00057 0.00047 0.00050 0.00052 0.00030 C1 0.16108 -0.12970 0.33660 1.00000 0.02462 0.02838 0.02049 0.00115 -0.00396 0.00247 0.02450 0.00578 0.00040 0.00029 0.00011 0.00000 0.00193 0.00193 0.00191 0.00161 0.00159 0.00171 0.00082 H1 0.22646 -0.15829 0.35843 1.00000 0.02940 0.00000 0.00000 C2 0.22153 -0.05399 0.30705 1.00000 0.02710 0.02621 0.02999 -0.00443 0.00179 0.00061 0.02777 0.00600 0.00043 0.00028 0.00011 0.00000 0.00195 0.00195 0.00217 0.00164 0.00171 0.00173 0.00086 H2 0.32897 -0.03111 0.30808 1.00000 0.03332 0.00000 0.00000 C3 0.12276 -0.01200 0.27591 1.00000 0.04149 0.02403 0.01886 0.00230 0.00259 -0.00330 0.02812 0.00615 0.00046 0.00030 0.00011 0.00000 0.00231 0.00195 0.00191 0.00155 0.00175 0.00182 0.00089 C4 -0.03171 -0.04663 0.27335 1.00000 0.03671 0.02420 0.02256 0.00111 -0.00183 0.00891 0.02782 0.00609 0.00043 0.00029 0.00011 0.00000 0.00218 0.00194 0.00196 0.00156 0.00169 0.00183 0.00087 H4 -0.09758 -0.01753 0.25171 1.00000 0.03339 0.00000 0.00000 C5 -0.09109 -0.12432 0.30252 1.00000 0.02467 0.02352 0.02664 -0.00259 -0.00176 0.00151 0.02494 0.00592 0.00043 0.00029 0.00010 0.00000 0.00190 0.00182 0.00199 0.00157 0.00170 0.00167 0.00082 H5 -0.19715 -0.15006 0.30056 1.00000 0.02993 0.00000 0.00000 C6 0.00386 -0.16380 0.33417 1.00000 0.02298 0.01911 0.02500 -0.00024 0.00329 -0.00012 0.02236 0.00581 0.00040 0.00028 0.00011 0.00000 0.00196 0.00180 0.00194 0.00151 0.00164 0.00161 0.00081 C7 -0.17455 -0.20951 0.39369 1.00000 0.02730 0.02238 0.02092 -0.00552 -0.00063 0.00332 0.02353 0.00566 0.00042 0.00028 0.00011 0.00000 0.00201 0.00197 0.00194 0.00164 0.00172 0.00168 0.00081 C8 -0.36660 -0.06737 0.40778 1.00000 0.02889 0.03668 0.02909 -0.00546 0.00510 0.01369 0.03155 0.00654 0.00042 0.00031 0.00011 0.00000 0.00205 0.00215 0.00211 0.00178 0.00172 0.00185 0.00092 H8A -0.34520 -0.06121 0.43818 1.00000 0.03786 0.00000 0.00000 H8B -0.45148 -0.12498 0.40343 1.00000 0.03786 0.00000 0.00000 C9 -0.41438 0.04845 0.39036 1.00000 0.04435 0.04569 0.05316 0.00680 0.01139 0.02007 0.04773 0.00794 0.00049 0.00034 0.00013 0.00000 0.00256 0.00258 0.00276 0.00224 0.00230 0.00221 0.00115 H9A -0.50923 0.07576 0.40481 1.00000 0.07160 0.00000 0.00000 H9B -0.43625 0.04085 0.36035 1.00000 0.07160 0.00000 0.00000 H9C -0.32880 0.10427 0.39457 1.00000 0.07160 0.00000 0.00000 C10 0.09233 -0.39379 0.34333 1.00000 0.01914 0.02258 0.02065 -0.00091 -0.00222 -0.00057 0.02079 0.00540 0.00038 0.00028 0.00010 0.00000 0.00173 0.00188 0.00185 0.00150 0.00158 0.00158 0.00077 H10 0.11006 -0.35175 0.31818 1.00000 0.02495 0.00000 0.00000 C11 0.16362 -0.50756 0.34936 1.00000 0.01487 0.02059 0.02404 -0.00344 -0.00471 -0.00168 0.01983 0.00536 0.00037 0.00027 0.00010 0.00000 0.00172 0.00179 0.00193 0.00152 0.00157 0.00152 0.00077 C12 0.41719 -0.67602 0.28620 1.00000 0.02199 0.02732 0.03347 -0.00747 -0.00760 0.00364 0.02759 0.00597 0.00041 0.00032 0.00012 0.00000 0.00201 0.00203 0.00228 0.00180 0.00185 0.00174 0.00086 C13 0.61482 -0.81379 0.26712 1.00000 0.04455 0.03588 0.04759 -0.00713 0.01340 0.01712 0.04267 0.00738 0.00046 0.00035 0.00013 0.00000 0.00253 0.00226 0.00257 0.00209 0.00223 0.00211 0.00108 H13A 0.59281 -0.78413 0.23862 1.00000 0.05121 0.00000 0.00000 H13B 0.61638 -0.89955 0.26598 1.00000 0.05121 0.00000 0.00000 C14 0.77010 -0.76984 0.28186 1.00000 0.04339 0.03528 0.04639 0.00091 0.01451 0.00416 0.04169 0.00704 0.00048 0.00034 0.00013 0.00000 0.00258 0.00219 0.00256 0.00198 0.00220 0.00208 0.00105 H14A 0.85296 -0.79599 0.26269 1.00000 0.06253 0.00000 0.00000 H14B 0.79132 -0.79970 0.31004 1.00000 0.06253 0.00000 0.00000 H14C 0.76824 -0.68492 0.28256 1.00000 0.06253 0.00000 0.00000 C15 0.14606 -0.56187 0.39217 1.00000 0.02222 0.01330 0.03020 -0.00296 0.00279 0.00600 0.02191 0.00549 0.00039 0.00026 0.00011 0.00000 0.00185 0.00173 0.00200 0.00154 0.00159 0.00151 0.00080 H15 0.03953 -0.54185 0.40341 1.00000 0.02629 0.00000 0.00000 C16 0.02423 -0.74913 0.39095 1.00000 0.03315 0.02116 0.03732 -0.00424 -0.00670 -0.00460 0.03054 0.00610 0.00047 0.00030 0.00012 0.00000 0.00236 0.00197 0.00229 0.00175 0.00191 0.00184 0.00091 C17 0.05899 -0.87514 0.38732 1.00000 0.03908 0.02139 0.04557 -0.00186 0.00164 -0.00961 0.03535 0.00606 0.00043 0.00028 0.00012 0.00000 0.00233 0.00190 0.00248 0.00180 0.00199 0.00180 0.00097 H17A 0.17292 -0.88648 0.38452 1.00000 0.05302 0.00000 0.00000 H17B 0.00561 -0.90664 0.36260 1.00000 0.05302 0.00000 0.00000 H17C 0.02136 -0.91530 0.41245 1.00000 0.05302 0.00000 0.00000 C18 0.27007 -0.51629 0.42238 1.00000 0.01576 0.02160 0.02369 -0.00428 0.00247 0.00237 0.02035 0.00540 0.00036 0.00028 0.00010 0.00000 0.00173 0.00174 0.00189 0.00151 0.00152 0.00150 0.00077 H18 0.25723 -0.43052 0.42538 1.00000 0.02442 0.00000 0.00000 C19 0.49950 -0.45310 0.38485 1.00000 0.02650 0.03461 0.02216 0.00131 0.00029 -0.00765 0.02776 0.00603 0.00042 0.00033 0.00011 0.00000 0.00200 0.00221 0.00197 0.00174 0.00173 0.00188 0.00085 C20 0.65193 -0.49423 0.36751 1.00000 0.03112 0.05029 0.04089 -0.00703 0.01080 -0.01380 0.04077 0.00665 0.00043 0.00034 0.00012 0.00000 0.00223 0.00261 0.00255 0.00206 0.00195 0.00206 0.00107 H20A 0.66916 -0.57505 0.37579 1.00000 0.06115 0.00000 0.00000 H20B 0.73767 -0.44601 0.37841 1.00000 0.06115 0.00000 0.00000 H20C 0.64954 -0.48878 0.33688 1.00000 0.06115 0.00000 0.00000 C21 0.26121 -0.57208 0.46540 1.00000 0.01757 0.01579 0.02988 -0.00020 0.00190 0.00233 0.02108 0.00557 0.00036 0.00028 0.00010 0.00000 0.00176 0.00165 0.00199 0.00148 0.00152 0.00152 0.00078 H21 0.26610 -0.65826 0.46227 1.00000 0.02530 0.00000 0.00000 C22 0.00552 -0.62381 0.49207 1.00000 0.02336 0.02765 0.03478 0.00505 -0.00038 -0.00521 0.02860 0.00606 0.00041 0.00031 0.00012 0.00000 0.00194 0.00206 0.00222 0.00173 0.00179 0.00176 0.00085 C23 -0.15264 -0.57401 0.50132 1.00000 0.02757 0.03447 0.05772 -0.00006 0.00809 -0.00728 0.03992 0.00662 0.00039 0.00031 0.00014 0.00000 0.00208 0.00205 0.00277 0.00211 0.00203 0.00186 0.00101 H23A -0.14797 -0.48934 0.49908 1.00000 0.05988 0.00000 0.00000 H23B -0.18443 -0.59572 0.52977 1.00000 0.05988 0.00000 0.00000 H23C -0.22955 -0.60421 0.48120 1.00000 0.05988 0.00000 0.00000 C24 0.38840 -0.53322 0.49521 1.00000 0.02636 0.01514 0.02700 0.00207 0.00139 0.00118 0.02284 0.00550 0.00039 0.00026 0.00011 0.00000 0.00187 0.00165 0.00197 0.00152 0.00169 0.00154 0.00078 H24A 0.36232 -0.55718 0.52417 1.00000 0.02740 0.00000 0.00000 H24B 0.49064 -0.56835 0.48738 1.00000 0.02740 0.00000 0.00000 C25 0.50799 -0.35842 0.51717 1.00000 0.02264 0.02406 0.02766 -0.00489 0.00671 -0.00297 0.02478 0.00610 0.00041 0.00029 0.00012 0.00000 0.00195 0.00192 0.00206 0.00165 0.00177 0.00172 0.00082 C26 0.52631 -0.23241 0.50723 1.00000 0.03797 0.02297 0.03303 -0.00423 0.00546 -0.00706 0.03133 0.00608 0.00044 0.00027 0.00012 0.00000 0.00234 0.00189 0.00220 0.00170 0.00191 0.00173 0.00093 H26A 0.45196 -0.21079 0.48509 1.00000 0.04699 0.00000 0.00000 H26B 0.63418 -0.21751 0.49771 1.00000 0.04699 0.00000 0.00000 H26C 0.50480 -0.18637 0.53239 1.00000 0.04699 0.00000 0.00000 Final Structure Factor Calculation for 01ESP002 IN P212121 Total number of l.s. parameters = 389 Maximum vector length = 511 Memory required = 4146 / 26068 wR2 = 0.1224 before cycle 5 for 5286 data and 2 / 389 parameters GooF = S = 0.988; Restrained GooF = 0.988 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0567 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0498 for 3997 Fo > 4sig(Fo) and 0.0784 for all 5286 data wR2 = 0.1224, GooF = S = 0.988, Restrained GooF = 0.988 for all data Flack x parameter = -0.1050 with esd 0.0930 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 Occupancy sum of asymmetric unit = 43.00 for non-hydrogen and 33.00 for hydrogen atoms Principal mean square atomic displacements U 0.0301 0.0221 0.0160 N1 0.0293 0.0243 0.0154 N2 0.0278 0.0243 0.0194 N3 0.0363 0.0245 0.0172 N4 0.0393 0.0288 0.0199 O1 0.0338 0.0263 0.0239 O2 0.0440 0.0339 0.0253 O3 0.0489 0.0368 0.0155 O4 0.0343 0.0227 0.0157 O5 0.1510 0.0369 0.0240 O6 0.0303 0.0219 0.0187 O7 0.0521 0.0345 0.0229 O8 0.0334 0.0203 0.0189 O9 0.1289 0.0351 0.0179 O10 0.0339 0.0261 0.0146 O11 0.0484 0.0329 0.0247 O12 0.0569 0.0491 0.0224 Cl1 0.0297 0.0262 0.0176 C1 0.0331 0.0274 0.0227 C2 0.0423 0.0247 0.0174 C3 0.0414 0.0234 0.0187 C4 0.0292 0.0236 0.0219 C5 0.0274 0.0205 0.0191 C6 0.0303 0.0245 0.0158 C7 0.0471 0.0328 0.0148 C8 0.0733 0.0454 0.0245 C9 0.0230 0.0220 0.0174 C10 0.0271 0.0205 0.0119 C11 0.0420 0.0226 0.0182 C12 0.0619 0.0498 0.0162 C13 0.0600 0.0359 0.0292 C14 0.0312 0.0250 0.0095 C15 0.0423 0.0318 0.0175 C16 0.0470 0.0419 0.0171 C17 0.0271 0.0206 0.0134 C18 0.0393 0.0229 0.0211 C19 0.0634 0.0375 0.0214 C20 0.0302 0.0190 0.0141 C21 0.0380 0.0284 0.0194 C22 0.0599 0.0382 0.0216 C23 0.0285 0.0253 0.0147 C24 0.0352 0.0212 0.0179 C25 0.0446 0.0295 0.0198 C26 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.024 0.036 0.048 0.060 0.072 0.086 0.106 0.131 0.173 1.000 Number in group 550. 528. 507. 566. 518. 508. 542. 507. 528. 532. GooF 0.815 0.900 0.909 0.989 1.034 0.937 1.020 1.003 1.108 1.121 K 1.023 1.009 0.998 1.008 1.013 0.994 0.995 1.010 1.010 0.992 Resolution(A) 0.84 0.87 0.91 0.95 1.01 1.07 1.15 1.27 1.45 1.83 inf Number in group 543. 528. 529. 513. 535. 533. 524. 525. 531. 525. GooF 0.827 0.864 0.845 0.843 0.899 0.827 0.984 1.001 1.281 1.344 K 1.013 1.019 1.022 1.023 0.998 1.012 1.015 0.997 1.022 0.980 R1 0.210 0.172 0.129 0.099 0.075 0.054 0.056 0.048 0.047 0.045 Recommended weighting scheme: WGHT 0.0563 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) 5 2 0 109.47 175.44 5.00 0.062 1.63 -1 2 3 22535.40 34729.86 4.54 0.869 4.35 2 5 2 2483.06 1885.21 4.52 0.202 2.01 4 0 18 478.08 756.84 4.43 0.128 1.36 -1 3 14 1603.14 1245.46 4.02 0.165 1.91 2 4 0 481.51 368.24 3.99 0.089 2.39 1 3 14 1636.95 1258.77 3.93 0.165 1.91 2 0 18 2199.30 1706.55 3.92 0.193 1.64 0 2 12 1551.36 1971.79 3.87 0.207 2.42 0 6 14 151.17 226.40 3.72 0.070 1.47 -1 6 19 -3.82 112.76 3.69 0.050 1.25 -2 1 18 156.81 241.82 3.67 0.073 1.62 1 4 3 449.88 360.39 3.59 0.089 2.64 3 5 6 716.75 548.11 3.58 0.109 1.69 -1 5 12 1490.87 1173.93 3.54 0.160 1.71 -3 2 14 725.73 569.73 3.53 0.111 1.70 -2 3 8 1722.78 2138.39 3.52 0.216 2.32 4 0 0 162.21 222.54 3.46 0.070 2.12 -2 2 21 642.54 828.45 3.28 0.134 1.39 0 6 1 916.85 747.91 3.26 0.128 1.92 1 12 4 31.22 166.54 3.22 0.060 0.95 4 3 0 368.09 458.30 3.22 0.100 1.86 -7 8 14 170.46 9.50 3.21 0.014 0.86 0 11 7 -1.23 60.15 3.19 0.036 1.02 2 6 26 -30.88 115.51 3.17 0.050 1.01 3 5 0 147.59 210.76 3.15 0.068 1.79 3 4 30 443.07 199.88 3.14 0.066 0.94 -3 5 20 237.97 148.15 3.12 0.057 1.19 4 4 7 97.68 153.59 3.05 0.058 1.60 2 3 18 415.15 534.98 3.05 0.108 1.51 0 1 9 10283.33 8634.42 3.03 0.433 3.39 0 4 12 89.67 54.25 3.02 0.034 1.96 6 7 9 215.79 129.35 3.01 0.053 1.03 -1 7 20 278.25 139.26 3.01 0.055 1.14 1 6 20 42.55 102.70 3.01 0.047 1.22 2 3 0 171.37 244.11 3.00 0.073 2.85 4 0 9 189.52 133.67 3.00 0.054 1.82 2 2 12 9.74 32.80 2.95 0.027 2.10 1 0 5 1013.83 1218.06 2.89 0.163 5.10 -1 9 4 42.39 94.64 2.88 0.045 1.25 4 3 4 569.10 691.50 2.87 0.123 1.81 4 4 4 1013.38 823.28 2.87 0.134 1.67 2 1 29 203.97 322.66 2.82 0.084 1.06 -3 4 7 1687.35 2015.57 2.82 0.209 1.85 3 5 9 1252.14 1033.55 2.81 0.150 1.60 -4 4 25 89.93 181.56 2.81 0.063 1.02 -4 5 8 378.88 493.01 2.81 0.104 1.45 1 6 13 218.93 286.62 2.81 0.079 1.49 3 0 4 2855.00 2367.92 2.80 0.227 2.67 3 2 5 505.22 422.41 2.80 0.096 2.36 Bond lengths and angles N1 - Distance Angles N2 1.3916 (0.0036) C7 1.3928 (0.0042) 114.20 (0.27) C6 1.4357 (0.0042) 122.62 (0.26) 123.07 (0.27) N1 - N2 C7 N2 - Distance Angles C10 1.2824 (0.0040) N1 1.3916 (0.0036) 117.18 (0.28) N2 - C10 N3 - Distance Angles C11 1.2930 (0.0041) N4 1.3648 (0.0037) 119.61 (0.28) N3 - C11 N4 - Distance Angles N3 1.3648 (0.0037) C12 1.3694 (0.0044) 118.60 (0.30) N4 - N3 O1 - Distance Angles C7 1.3333 (0.0038) C8 1.4642 (0.0038) 114.63 (0.28) O1 - C7 O2 - Distance Angles C7 1.2091 (0.0039) O2 - O3 - Distance Angles C12 1.2134 (0.0042) O3 - O4 - Distance Angles C12 1.3385 (0.0042) C13 1.4717 (0.0041) 116.43 (0.29) O4 - C12 O5 - Distance Angles C16 1.3570 (0.0041) C15 1.4426 (0.0035) 117.61 (0.26) O5 - C16 O6 - Distance Angles C16 1.1840 (0.0043) O6 - O7 - Distance Angles C19 1.3717 (0.0040) C18 1.4381 (0.0036) 117.33 (0.25) O7 - C19 O8 - Distance Angles C19 1.2037 (0.0041) O8 - O9 - Distance Angles C22 1.3462 (0.0039) C21 1.4474 (0.0036) 118.93 (0.25) O9 - C22 O10 - Distance Angles C22 1.2015 (0.0041) O10 - O11 - Distance Angles C25 1.3573 (0.0040) C24 1.4380 (0.0035) 115.45 (0.25) O11 - C25 O12 - Distance Angles C25 1.2008 (0.0041) O12 - Cl1 - Distance Angles C3 1.7431 (0.0035) Cl1 - C1 - Distance Angles C2 1.3842 (0.0047) C6 1.3935 (0.0046) 119.68 (0.33) C1 - C2 C2 - Distance Angles C1 1.3842 (0.0047) C3 1.3880 (0.0048) 118.98 (0.34) C2 - C1 C3 - Distance Angles C4 1.3732 (0.0050) C2 1.3880 (0.0048) 121.19 (0.33) Cl1 1.7431 (0.0035) 119.47 (0.28) 119.34 (0.29) C3 - C4 C2 C4 - Distance Angles C3 1.3732 (0.0050) C5 1.3873 (0.0047) 119.67 (0.34) C4 - C3 C5 - Distance Angles C6 1.3706 (0.0046) C4 1.3873 (0.0047) 119.73 (0.33) C5 - C6 C6 - Distance Angles C5 1.3706 (0.0046) C1 1.3935 (0.0046) 120.70 (0.32) N1 1.4357 (0.0041) 120.85 (0.30) 118.45 (0.31) C6 - C5 C1 C7 - Distance Angles O2 1.2091 (0.0039) O1 1.3333 (0.0038) 125.82 (0.31) N1 1.3928 (0.0042) 124.40 (0.30) 109.77 (0.30) C7 - O2 O1 C8 - Distance Angles O1 1.4642 (0.0038) C9 1.5028 (0.0050) 106.64 (0.30) C8 - O1 C9 - Distance Angles C8 1.5028 (0.0050) C9 - C10 - Distance Angles N2 1.2824 (0.0040) C11 1.4580 (0.0044) 119.28 (0.31) C10 - N2 C11 - Distance Angles N3 1.2930 (0.0041) C10 1.4580 (0.0044) 113.23 (0.30) C15 1.5107 (0.0046) 129.68 (0.29) 116.86 (0.28) C11 - N3 C10 C12 - Distance Angles O3 1.2134 (0.0042) O4 1.3385 (0.0042) 126.47 (0.34) N4 1.3694 (0.0044) 125.48 (0.34) 108.02 (0.32) C12 - O3 O4 C13 - Distance Angles O4 1.4717 (0.0041) C14 1.4886 (0.0054) 109.02 (0.31) C13 - O4 C14 - Distance Angles C13 1.4886 (0.0054) C14 - C15 - Distance Angles O5 1.4426 (0.0035) C11 1.5107 (0.0046) 111.21 (0.26) C18 1.5216 (0.0044) 108.67 (0.26) 111.22 (0.27) C15 - O5 C11 C16 - Distance Angles O6 1.1840 (0.0043) O5 1.3570 (0.0041) 122.58 (0.32) C17 1.4877 (0.0047) 126.83 (0.35) 110.58 (0.31) C16 - O6 O5 C17 - Distance Angles C16 1.4877 (0.0047) C17 - C18 - Distance Angles O7 1.4381 (0.0036) C21 1.5185 (0.0046) 106.95 (0.24) C15 1.5216 (0.0044) 109.39 (0.25) 113.12 (0.27) C18 - O7 C21 C19 - Distance Angles O8 1.2037 (0.0041) O7 1.3717 (0.0040) 122.64 (0.32) C20 1.4852 (0.0051) 126.62 (0.34) 110.70 (0.31) C19 - O8 O7 C20 - Distance Angles C19 1.4852 (0.0050) C20 - C21 - Distance Angles O9 1.4474 (0.0036) C24 1.5076 (0.0044) 110.25 (0.26) C18 1.5185 (0.0046) 104.64 (0.25) 114.18 (0.27) C21 - O9 C24 C22 - Distance Angles O10 1.2015 (0.0041) O9 1.3462 (0.0039) 122.74 (0.33) C23 1.4899 (0.0047) 126.53 (0.33) 110.70 (0.30) C22 - O10 O9 C23 - Distance Angles C22 1.4899 (0.0047) C23 - C24 - Distance Angles O11 1.4380 (0.0035) C21 1.5076 (0.0044) 107.23 (0.26) C24 - O11 C25 - Distance Angles O12 1.2008 (0.0041) O11 1.3573 (0.0040) 123.03 (0.31) C26 1.4958 (0.0047) 125.48 (0.34) 111.48 (0.31) C25 - O12 O11 C26 - Distance Angles C25 1.4958 (0.0047) C26 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.05 2.698(4) 130.0 N4-H4A...O5 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)