+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 16:09:31 on 08-Apr-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02SRC141 in P2(1)/c CELL 0.71073 19.3799 13.2761 13.0097 90.000 91.600 90.000 ZERR 8.00 0.0020 0.0011 0.0011 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 112 192 24 40 V = 3345.95 F(000) = 1352.0 Mu = 0.09 mm-1 Cell Wt = 2514.90 Rho = 1.248 ACTA SIZE 0.2 0.2 0.15 HTAB O1 N3_$1 EQIV $1[ -x, -y+1, -z+1 HTAB O1 O3_$1 HTAB O6 N6_$2 EQIV $2 -x+1, -y+1, -z+2 HTAB O6 O8_$2 FMAP 2 PLAN 20 HTAB SHEL 7 0.84 BOND L.S. 4 WGHT 0.141300 FVAR 0.14233 MOLE 1 N1 3 0.035399 0.426927 0.338867 11.00000 0.03977 0.03098 = 0.03662 0.00229 -0.00286 -0.00206 N2 3 0.034318 0.573304 0.257785 11.00000 0.04625 0.03823 = 0.02585 0.00243 -0.00348 -0.00340 N3 3 0.096863 0.562841 0.418291 11.00000 0.03829 0.02673 = 0.03381 0.00096 0.00000 -0.00465 O1 4 -0.101013 0.501559 0.368315 11.00000 0.06173 0.03462 = 0.03747 -0.00272 0.00732 0.00460 AFIX 147 H1 2 -0.096690 0.488154 0.429685 11.00000 -1.50000 AFIX 0 O2 4 0.026006 0.262050 0.379562 11.00000 0.04457 0.03425 = 0.04231 0.00025 -0.00358 -0.00574 O3 4 0.112199 0.356369 0.451159 11.00000 0.03903 0.03135 = 0.03608 -0.00127 -0.00128 0.00133 O4 4 0.104183 0.719595 0.337583 11.00000 0.04996 0.03392 = 0.03386 0.00596 -0.00344 -0.00596 O5 4 0.156115 0.686783 0.491700 11.00000 0.04517 0.02748 = 0.03695 0.00045 -0.00215 -0.00767 C1 1 -0.090544 0.413923 0.309987 11.00000 0.04300 0.03000 = 0.03550 -0.00318 0.00096 -0.00425 AFIX 23 H1A 2 -0.126734 0.408158 0.257291 11.00000 -1.20000 H1B 2 -0.092919 0.355266 0.354200 11.00000 -1.20000 AFIX 0 C2 1 -0.021537 0.417030 0.260472 11.00000 0.04380 0.02795 = 0.03063 -0.00141 0.00034 -0.00063 AFIX 13 H2 2 -0.014978 0.356126 0.219318 11.00000 -1.20000 AFIX 0 C3 1 -0.011496 0.510482 0.194351 11.00000 0.05578 0.03789 = 0.03288 -0.00202 -0.00117 -0.00535 AFIX 23 H3A 2 0.009558 0.493308 0.129889 11.00000 -1.20000 H3B 2 -0.055119 0.544152 0.179923 11.00000 -1.20000 AFIX 0 C4 1 0.058528 0.526466 0.341565 11.00000 0.02824 0.03238 = 0.03017 0.00160 0.00737 -0.00198 C5 1 0.056443 0.341094 0.392561 11.00000 0.03756 0.03312 = 0.03741 -0.00745 0.00374 0.00250 C6 1 0.140464 0.273626 0.516260 11.00000 0.04135 0.03031 = 0.03328 0.00756 -0.00289 0.00344 C7 1 0.089149 0.245290 0.595492 11.00000 0.05403 0.04786 = 0.04490 0.00890 0.00577 0.00166 AFIX 137 H7A 2 0.078273 0.303453 0.635782 11.00000 -1.50000 H7B 2 0.108468 0.193927 0.639541 11.00000 -1.50000 H7C 2 0.047865 0.220356 0.561859 11.00000 -1.50000 AFIX 0 C8 1 0.161148 0.185635 0.450732 11.00000 0.04916 0.03597 = 0.05430 -0.00798 -0.00178 0.00664 AFIX 137 H8A 2 0.120516 0.151339 0.425390 11.00000 -1.50000 H8B 2 0.189055 0.139993 0.491250 11.00000 -1.50000 H8C 2 0.187050 0.209522 0.393816 11.00000 -1.50000 AFIX 0 C9 1 0.204205 0.320617 0.565197 11.00000 0.05583 0.04066 = 0.03896 -0.00569 -0.00623 0.01042 AFIX 137 H9A 2 0.233867 0.344277 0.512474 11.00000 -1.50000 H9B 2 0.228230 0.271302 0.606602 11.00000 -1.50000 H9C 2 0.191072 0.376170 0.607650 11.00000 -1.50000 AFIX 0 C10 1 0.117238 0.661629 0.408106 11.00000 0.03178 0.03041 = 0.03593 -0.00219 -0.00099 0.00391 C11 1 0.183230 0.790754 0.503923 11.00000 0.05124 0.02805 = 0.03401 0.00050 -0.00166 -0.00594 C12 1 0.123223 0.864864 0.505029 11.00000 0.06522 0.03345 = 0.04385 -0.00763 0.00200 0.00079 AFIX 137 H1C 2 0.102506 0.869594 0.437308 11.00000 -1.50000 H1D 2 0.139873 0.929939 0.526225 11.00000 -1.50000 H1E 2 0.089482 0.841750 0.552252 11.00000 -1.50000 AFIX 0 C13 1 0.234084 0.812875 0.421792 11.00000 0.05593 0.05525 = 0.05094 0.00233 0.00546 -0.01558 AFIX 137 H1F 2 0.268526 0.760916 0.421393 11.00000 -1.50000 H1G 2 0.255807 0.876647 0.435486 11.00000 -1.50000 H1H 2 0.210406 0.815193 0.356027 11.00000 -1.50000 AFIX 0 C14 1 0.218646 0.787874 0.607898 11.00000 0.07608 0.04318 = 0.04329 0.00363 -0.01493 -0.01327 AFIX 137 H1I 2 0.185821 0.770336 0.658838 11.00000 -1.50000 H1J 2 0.237913 0.852894 0.623511 11.00000 -1.50000 H1K 2 0.254867 0.738547 0.607882 11.00000 -1.50000 AFIX 0 MOLE 2 N4 3 0.448985 0.660376 0.935304 11.00000 0.04234 0.02911 = 0.02771 0.00060 0.00613 -0.00364 N5 3 0.449244 0.729048 1.089049 11.00000 0.04646 0.02824 = 0.04420 -0.00834 0.00115 -0.00534 N6 3 0.391947 0.571567 1.067607 11.00000 0.04402 0.03325 = 0.02894 0.00680 0.00292 -0.00037 O6 4 0.586121 0.628410 1.013986 11.00000 0.06560 0.03704 = 0.04016 0.00089 -0.00177 0.00667 AFIX 147 H6 2 0.594396 0.570866 0.995026 11.00000 -1.50000 AFIX 0 O7 4 0.458454 0.630940 0.765400 11.00000 0.05235 0.03927 = 0.03158 0.00612 0.00958 -0.00103 O8 4 0.378077 0.548251 0.855384 11.00000 0.04078 0.02989 = 0.03158 0.00030 0.00385 -0.00590 O9 4 0.385775 0.636007 1.233621 11.00000 0.11454 0.07429 = 0.04278 -0.01185 0.02924 -0.05164 O10 4 0.338310 0.490114 1.189874 11.00000 0.08712 0.04348 = 0.03414 -0.00299 0.02507 -0.02239 C15 1 0.573790 0.690399 0.927338 11.00000 0.04378 0.04544 = 0.03483 0.00834 -0.00180 -0.00514 AFIX 23 H1L 2 0.576848 0.650465 0.865193 11.00000 -1.20000 H1M 2 0.608749 0.742605 0.925449 11.00000 -1.20000 AFIX 0 C16 1 0.503254 0.738211 0.931221 11.00000 0.04317 0.03230 = 0.03422 0.00253 0.00338 -0.00742 AFIX 13 H16 2 0.495253 0.781856 0.871317 11.00000 -1.20000 AFIX 0 C17 1 0.491629 0.796539 1.029701 11.00000 0.05135 0.03288 = 0.04149 -0.00124 0.00528 -0.00920 AFIX 23 H1N 2 0.535043 0.810775 1.065696 11.00000 -1.20000 H1O 2 0.467795 0.859476 1.015492 11.00000 -1.20000 AFIX 0 C18 1 0.426895 0.649573 1.035928 11.00000 0.03746 0.03190 = 0.03208 0.00173 -0.00097 0.00297 C19 1 0.429685 0.611545 0.844628 11.00000 0.04112 0.03426 = 0.03039 0.00017 -0.00188 0.00336 C20 1 0.352414 0.488690 0.765744 11.00000 0.05339 0.03724 = 0.02686 -0.00879 -0.00383 -0.00512 C21 1 0.322737 0.558127 0.684057 11.00000 0.05885 0.05153 = 0.03370 0.00188 -0.00015 -0.00511 AFIX 137 H2A 2 0.291732 0.604996 0.714800 11.00000 -1.50000 H2B 2 0.298113 0.519242 0.632772 11.00000 -1.50000 H2C 2 0.359479 0.594329 0.652617 11.00000 -1.50000 AFIX 0 C22 1 0.295329 0.426197 0.812609 11.00000 0.06019 0.03933 = 0.03716 -0.00697 -0.00878 -0.00864 AFIX 137 H2D 2 0.313793 0.389289 0.870567 11.00000 -1.50000 H2E 2 0.277016 0.379929 0.762126 11.00000 -1.50000 H2F 2 0.259213 0.469999 0.834662 11.00000 -1.50000 AFIX 0 C23 1 0.408428 0.422037 0.727542 11.00000 0.07043 0.04027 = 0.04658 -0.01049 0.01040 -0.00062 AFIX 137 H2G 2 0.443692 0.462606 0.697803 11.00000 -1.50000 H2H 2 0.389546 0.376868 0.676458 11.00000 -1.50000 H2I 2 0.427985 0.383870 0.783853 11.00000 -1.50000 AFIX 0 C24 1 0.373695 0.572021 1.168766 11.00000 0.04107 0.03195 = 0.03846 -0.00246 0.00587 -0.00054 C25 1 0.315829 0.468217 1.295355 11.00000 0.08955 0.03868 = 0.04005 -0.00380 0.02377 -0.01481 C26 1 0.263135 0.536741 1.325926 11.00000 0.07681 0.19816 = 0.07969 0.06855 0.04775 0.07213 AFIX 137 H2J 2 0.282270 0.603164 1.332941 11.00000 -1.50000 H2K 2 0.245342 0.515537 1.390569 11.00000 -1.50000 H2L 2 0.226473 0.537452 1.274759 11.00000 -1.50000 AFIX 0 C27 1 0.288992 0.364672 1.281736 11.00000 0.69537 0.18513 = 0.12207 -0.09119 0.24433 -0.29509 AFIX 137 H2M 2 0.272913 0.340067 1.346194 11.00000 -1.50000 H2N 2 0.325138 0.321694 1.258248 11.00000 -1.50000 H2O 2 0.251500 0.365030 1.231925 11.00000 -1.50000 AFIX 0 C28 1 0.374154 0.468582 1.367862 11.00000 0.09894 0.34852 = 0.08758 0.13873 0.05117 0.11317 AFIX 137 H2P 2 0.388375 0.536749 1.381011 11.00000 -1.50000 H2Q 2 0.411708 0.431627 1.339493 11.00000 -1.50000 H2R 2 0.360945 0.437610 1.431026 11.00000 -1.50000 HKLF 4 1.0 0.00 0.00 1.00 0.00 -1.00 0.00 1.00 0.00 0.00 Covalent radii and connectivity table for 02SRC141 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 N1 - C5 C4 C2 N2 - C4 C3 N3 - C4 C10 O1 - C1 O2 - C5 O3 - C5 C6 O4 - C10 O5 - C10 C11 C1 - O1 C2 C2 - N1 C1 C3 C3 - N2 C2 C4 - N3 N2 N1 C5 - O2 O3 N1 C6 - O3 C7 C8 C9 C7 - C6 C8 - C6 C9 - C6 C10 - O4 O5 N3 C11 - O5 C14 C13 C12 C12 - C11 C13 - C11 C14 - C11 N4 - C19 C18 C16 N5 - C18 C17 N6 - C18 C24 O6 - C15 O7 - C19 O8 - C19 C20 O9 - C24 O10 - C24 C25 C15 - O6 C16 C16 - N4 C15 C17 C17 - N5 C16 C18 - N6 N5 N4 C19 - O7 O8 N4 C20 - O8 C23 C21 C22 C21 - C20 C22 - C20 C23 - C20 C24 - O9 O10 N6 C25 - C26 C28 C27 O10 C26 - C25 C27 - C25 C28 - C25 Operators for generating equivalent atoms: $1 -x, -y+1, -z+1 $2 -x+1, -y+1, -z+2 h k l Fo^2 Sigma Why rejected -3 0 3 33.00 3.89 observed but should be systematically absent -4 0 3 5.93 0.99 observed but should be systematically absent -6 0 3 4.00 1.00 observed but should be systematically absent -9 0 3 5.04 1.01 observed but should be systematically absent 8 0 1 8.92 0.99 observed but should be systematically absent 6 0 1 6.93 0.99 observed but should be systematically absent 4 0 1 16.83 2.97 observed but should be systematically absent -4 0 1 18.92 2.00 observed but should be systematically absent -6 0 1 6.98 1.00 observed but should be systematically absent -8 0 1 10.97 1.00 observed but should be systematically absent -8 0 1 7.98 1.00 observed but should be systematically absent -6 0 1 5.99 1.00 observed but should be systematically absent -4 0 1 16.91 2.99 observed but should be systematically absent -3 0 1 3.96 0.99 observed but should be systematically absent 3 0 1 3.96 0.99 observed but should be systematically absent 4 0 1 20.77 2.97 observed but should be systematically absent 6 0 1 5.94 0.99 observed but should be systematically absent 8 0 1 9.92 1.98 observed but should be systematically absent -3 0 3 12.19 2.82 observed but should be systematically absent 17467 Reflections read, of which 1483 rejected -23 =< h =< 20, -15 =< k =< 15, -15 =< l =< 15, Max. 2-theta = 50.05 19 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -3 2 1 25.91 0.97 3 19.45 -1 2 1 36.95 1.09 3 7.71 4 1 2 14.39 0.81 3 4.82 -6 3 2 28.49 1.35 3 7.16 -2 3 2 25.25 0.91 3 11.27 3 3 2 14.25 0.82 3 4.18 -1 5 2 23.93 0.89 2 20.32 7 1 3 16.34 0.96 2 6.39 5 2 3 13.55 0.68 4 4.37 7 2 3 7.53 0.67 3 3.39 -4 6 3 25.80 0.94 2 19.93 -3 9 3 9.75 0.86 2 6.91 2 5 4 15.68 0.82 3 4.45 -6 6 5 14.97 0.90 2 10.29 -8 8 5 14.21 0.89 2 10.06 -1 4 6 28.40 0.83 3 4.52 -9 8 6 15.27 0.97 2 18.99 5 9 7 15.39 0.82 4 4.29 18 Inconsistent equivalents 5259 Unique reflections, of which 0 suppressed R(int) = 0.1193 R(sigma) = 0.1388 Friedel opposites merged Maximum memory for data reduction = 4107 / 53519 Default effective X-H distances for T = 20.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 0.98 0.97 0.96 0.93 0.86 0.89 1.10 0.82 0.93 0.86 0.93 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 = 5334 / 528525 wR2 = 0.2612 before cycle 1 for 5259 data and 411 / 411 parameters GooF = S = 1.013; Restrained GooF = 1.013 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1413 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14232 0.00059 -0.016 OSF 401 -1.07363 0.33605 -3.195 tors H2M Mean shift/esd = 0.021 Maximum = -3.195 for tors H2M Max. shift = 1.021 A for H2M Max. dU = 0.001 for C27 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5334 / 528525 wR2 = 0.2615 before cycle 2 for 5259 data and 411 / 411 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1413 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14232 0.00059 -0.007 OSF Mean shift/esd = 0.038 Maximum = 1.576 for tors H2M Max. shift = 0.525 A for H2O Max. dU = 0.001 for C27 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5334 / 528525 wR2 = 0.2610 before cycle 3 for 5259 data and 411 / 411 parameters GooF = S = 1.012; Restrained GooF = 1.012 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1413 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14234 0.00059 0.043 OSF Mean shift/esd = 0.035 Maximum = 2.320 for tors H2M Max. shift = 0.739 A for H2M Max. dU =-0.001 for C27 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5334 / 528525 wR2 = 0.2613 before cycle 4 for 5259 data and 411 / 411 parameters GooF = S = 1.013; Restrained GooF = 1.013 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1413 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14233 0.00059 -0.015 OSF 401 -0.83836 0.34063 -2.461 tors H2M Mean shift/esd = 0.037 Maximum = -2.461 for tors H2M Max. shift = 0.815 A for H2M Max. dU = 0.000 for C28 Largest correlation matrix elements -0.773 U12 C27 / U22 C27 -0.670 y C27 / x C27 0.545 U12 C28 / U13 C28 -0.772 U12 C27 / U11 C27 0.663 z C27 / x C27 -0.530 U23 C27 / U11 C27 0.754 U13 C27 / U11 C27 0.625 U23 C28 / U22 C28 0.517 z C28 / y C28 0.723 U13 C27 / U33 C27 0.611 U23 C28 / U33 C28 -0.506 U23 C27 / U22 C27 -0.707 U13 C27 / U23 C27 -0.562 U12 C27 / U13 C27 -0.503 U23 C27 / U33 C27 0.676 U12 C27 / U23 C27 0.560 U12 C28 / U22 C28 0.501 U12 C28 / U11 C28 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 -0.0967 0.4881 0.4297 147 0.820 0.000 O1 C1 H1 H1A -0.1267 0.4082 0.2573 23 0.970 0.000 C1 O1 C2 H1B -0.0929 0.3553 0.3542 23 0.970 0.000 C1 O1 C2 H2 -0.0150 0.3561 0.2193 13 0.980 0.000 C2 N1 C1 C3 H3A 0.0096 0.4933 0.1299 23 0.970 0.000 C3 N2 C2 H3B -0.0551 0.5442 0.1799 23 0.970 0.000 C3 N2 C2 H7A 0.0784 0.3034 0.6359 137 0.960 0.000 C7 C6 H7A H7B 0.1085 0.1938 0.6395 137 0.960 0.001 C7 C6 H7A H7C 0.0479 0.2205 0.5619 137 0.960 0.001 C7 C6 H7A H8A 0.1205 0.1513 0.4254 137 0.960 0.000 C8 C6 H8A H8B 0.1891 0.1400 0.4912 137 0.960 0.000 C8 C6 H8A H8C 0.1870 0.2096 0.3937 137 0.960 0.001 C8 C6 H8A H9A 0.2339 0.3442 0.5125 137 0.960 0.000 C9 C6 H9A H9B 0.2282 0.2713 0.6066 137 0.960 0.000 C9 C6 H9A H9C 0.1911 0.3762 0.6076 137 0.960 0.000 C9 C6 H9A H1C 0.1025 0.8696 0.4373 137 0.960 0.000 C12 C11 H1C H1D 0.1399 0.9300 0.5261 137 0.960 0.000 C12 C11 H1C H1E 0.0895 0.8418 0.5522 137 0.960 0.000 C12 C11 H1C H1F 0.2686 0.7610 0.4215 137 0.960 0.000 C13 C11 H1F H1G 0.2557 0.8767 0.4354 137 0.960 0.000 C13 C11 H1F H1H 0.2104 0.8150 0.3560 137 0.960 0.000 C13 C11 H1F H1I 0.1858 0.7705 0.6589 137 0.960 0.000 C14 C11 H1I H1J 0.2381 0.8528 0.6234 137 0.960 0.000 C14 C11 H1I H1K 0.2548 0.7383 0.6079 137 0.960 0.000 C14 C11 H1I H6 0.5943 0.5708 0.9950 147 0.820 0.000 O6 C15 H6 H1L 0.5769 0.6505 0.8652 23 0.970 0.000 C15 O6 C16 H1M 0.6088 0.7426 0.9254 23 0.970 0.000 C15 O6 C16 H16 0.4953 0.7818 0.8713 13 0.980 0.000 C16 N4 C15 C17 H1N 0.5350 0.8108 1.0657 23 0.970 0.000 C17 N5 C16 H1O 0.4678 0.8595 1.0155 23 0.970 0.000 C17 N5 C16 H2A 0.2916 0.6048 0.7147 137 0.960 0.000 C21 C20 H2A H2B 0.2983 0.5191 0.6326 137 0.960 0.001 C21 C20 H2A H2C 0.3595 0.5945 0.6528 137 0.960 0.001 C21 C20 H2A H2D 0.3138 0.3895 0.8707 137 0.960 0.000 C22 C20 H2D H2E 0.2771 0.3798 0.7622 137 0.960 0.000 C22 C20 H2D H2F 0.2591 0.4700 0.8344 137 0.960 0.000 C22 C20 H2D H2G 0.4437 0.4626 0.6978 137 0.960 0.000 C23 C20 H2G H2H 0.3896 0.3768 0.6765 137 0.960 0.000 C23 C20 H2G H2I 0.4280 0.3839 0.7839 137 0.960 0.000 C23 C20 H2G H2J 0.2822 0.6032 1.3325 137 0.960 0.000 C26 C25 H2J H2K 0.2456 0.5158 1.3908 137 0.960 0.000 C26 C25 H2J H2L 0.2264 0.5372 1.2750 137 0.960 0.000 C26 C25 H2J H2M 0.3019 0.3248 1.3405 137 0.960 0.071 C27 C25 H2M H2N 0.3068 0.3358 1.2209 137 0.960 0.071 C27 C25 H2M H2O 0.2391 0.3673 1.2755 137 0.960 0.060 C27 C25 H2M H2P 0.3877 0.5367 1.3822 137 0.960 0.002 C28 C25 H2P H2Q 0.4120 0.4328 1.3388 137 0.960 0.002 C28 C25 H2P H2R 0.3612 0.4361 1.4304 137 0.960 0.001 C28 C25 H2P 02SRC141 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq N1 0.03540 0.42691 0.33887 1.00000 0.03979 0.03092 0.03663 0.00227 -0.00286 -0.00204 0.03585 0.00718 0.00022 0.00032 0.00033 0.00000 0.00269 0.00263 0.00256 0.00226 0.00207 0.00206 0.00110 N2 0.03432 0.57331 0.25777 1.00000 0.04628 0.03828 0.02581 0.00243 -0.00347 -0.00338 0.03687 0.00731 0.00023 0.00033 0.00032 0.00000 0.00281 0.00265 0.00240 0.00230 0.00203 0.00218 0.00111 N3 0.09686 0.56284 0.41830 1.00000 0.03824 0.02674 0.03380 0.00100 -0.00009 -0.00470 0.03295 0.00717 0.00021 0.00031 0.00032 0.00000 0.00267 0.00246 0.00254 0.00214 0.00207 0.00198 0.00107 O1 -0.10101 0.50157 0.36832 1.00000 0.06167 0.03461 0.03742 -0.00271 0.00729 0.00459 0.04446 0.00673 0.00021 0.00027 0.00028 0.00000 0.00263 0.00216 0.00212 0.00202 0.00198 0.00185 0.00100 H1 -0.09672 0.48815 0.42969 1.00000 0.06668 0.00000 0.00000 O2 0.02602 0.26206 0.37955 1.00000 0.04449 0.03425 0.04245 0.00024 -0.00355 -0.00579 0.04049 0.00629 0.00019 0.00027 0.00028 0.00000 0.00237 0.00222 0.00225 0.00189 0.00176 0.00187 0.00096 O3 0.11219 0.35637 0.45115 1.00000 0.03904 0.03133 0.03609 -0.00124 -0.00127 0.00130 0.03553 0.00604 0.00018 0.00026 0.00026 0.00000 0.00224 0.00198 0.00205 0.00177 0.00174 0.00163 0.00091 O4 0.10418 0.71960 0.33759 1.00000 0.04994 0.03396 0.03388 0.00594 -0.00345 -0.00593 0.03935 0.00599 0.00019 0.00028 0.00028 0.00000 0.00244 0.00216 0.00213 0.00194 0.00175 0.00172 0.00096 O5 0.15611 0.68678 0.49171 1.00000 0.04524 0.02749 0.03690 0.00045 -0.00222 -0.00761 0.03661 0.00574 0.00018 0.00025 0.00026 0.00000 0.00225 0.00196 0.00220 0.00178 0.00177 0.00165 0.00092 C1 -0.09054 0.41393 0.30998 1.00000 0.04283 0.03001 0.03559 -0.00302 0.00098 -0.00431 0.03615 0.00908 0.00028 0.00040 0.00041 0.00000 0.00352 0.00308 0.00309 0.00278 0.00251 0.00243 0.00133 H1A -0.12673 0.40818 0.25728 1.00000 0.04338 0.00000 0.00000 H1B -0.09293 0.35527 0.35419 1.00000 0.04338 0.00000 0.00000 C2 -0.02154 0.41702 0.26049 1.00000 0.04380 0.02796 0.03067 -0.00138 0.00033 -0.00059 0.03416 0.00888 0.00027 0.00039 0.00038 0.00000 0.00351 0.00299 0.00295 0.00259 0.00250 0.00236 0.00131 H2 -0.01498 0.35612 0.21933 1.00000 0.04099 0.00000 0.00000 C3 -0.01149 0.51050 0.19435 1.00000 0.05582 0.03794 0.03287 -0.00204 -0.00118 -0.00542 0.04225 0.00923 0.00031 0.00042 0.00041 0.00000 0.00385 0.00327 0.00315 0.00284 0.00268 0.00280 0.00144 H3A 0.00956 0.49333 0.12989 1.00000 0.05070 0.00000 0.00000 H3B -0.05511 0.54418 0.17993 1.00000 0.05070 0.00000 0.00000 C4 0.05854 0.52647 0.34157 1.00000 0.02824 0.03241 0.03032 0.00163 0.00741 -0.00191 0.03020 0.00913 0.00025 0.00039 0.00040 0.00000 0.00299 0.00302 0.00304 0.00270 0.00236 0.00230 0.00123 C5 0.05644 0.34110 0.39255 1.00000 0.03752 0.03314 0.03734 -0.00749 0.00376 0.00249 0.03595 0.00999 0.00029 0.00042 0.00042 0.00000 0.00346 0.00339 0.00330 0.00284 0.00267 0.00269 0.00135 C6 0.14047 0.27362 0.51630 1.00000 0.04139 0.03024 0.03340 0.00753 -0.00285 0.00338 0.03508 0.00917 0.00027 0.00039 0.00040 0.00000 0.00342 0.00300 0.00308 0.00266 0.00253 0.00240 0.00135 C7 0.08919 0.24529 0.59552 1.00000 0.05405 0.04790 0.04472 0.00886 0.00577 0.00161 0.04881 0.01112 0.00031 0.00047 0.00045 0.00000 0.00398 0.00370 0.00349 0.00314 0.00291 0.00294 0.00156 H7A 0.07838 0.30342 0.63589 1.00000 0.07321 0.00000 0.00000 H7B 0.10849 0.19385 0.63949 1.00000 0.07321 0.00000 0.00000 H7C 0.04788 0.22045 0.56189 1.00000 0.07321 0.00000 0.00000 C8 0.16116 0.18564 0.45070 1.00000 0.04901 0.03590 0.05453 -0.00792 -0.00172 0.00662 0.04654 0.01009 0.00031 0.00042 0.00047 0.00000 0.00375 0.00326 0.00382 0.00313 0.00289 0.00274 0.00152 H8A 0.12053 0.15130 0.42542 1.00000 0.06980 0.00000 0.00000 H8B 0.18912 0.14002 0.49117 1.00000 0.06980 0.00000 0.00000 H8C 0.18700 0.20957 0.39374 1.00000 0.06980 0.00000 0.00000 C9 0.20419 0.32061 0.56521 1.00000 0.05559 0.04074 0.03907 -0.00574 -0.00633 0.01048 0.04528 0.00964 0.00030 0.00044 0.00044 0.00000 0.00397 0.00341 0.00338 0.00292 0.00283 0.00283 0.00153 H9A 0.23385 0.34425 0.51248 1.00000 0.06791 0.00000 0.00000 H9B 0.22821 0.27131 0.60663 1.00000 0.06791 0.00000 0.00000 H9C 0.19106 0.37618 0.60764 1.00000 0.06791 0.00000 0.00000 C10 0.11723 0.66162 0.40811 1.00000 0.03189 0.03045 0.03593 -0.00219 -0.00104 0.00392 0.03279 0.00906 0.00026 0.00040 0.00043 0.00000 0.00315 0.00319 0.00334 0.00291 0.00251 0.00235 0.00129 C11 0.18325 0.79077 0.50393 1.00000 0.05124 0.02808 0.03393 0.00055 -0.00163 -0.00600 0.03780 0.00895 0.00029 0.00039 0.00041 0.00000 0.00368 0.00297 0.00321 0.00267 0.00263 0.00258 0.00138 C12 0.12322 0.86488 0.50499 1.00000 0.06527 0.03345 0.04385 -0.00764 0.00206 0.00078 0.04751 0.01020 0.00032 0.00042 0.00046 0.00000 0.00413 0.00320 0.00346 0.00296 0.00289 0.00293 0.00152 H1C 0.10250 0.86956 0.43727 1.00000 0.07127 0.00000 0.00000 H1D 0.13987 0.92997 0.52613 1.00000 0.07127 0.00000 0.00000 H1E 0.08948 0.84179 0.55224 1.00000 0.07127 0.00000 0.00000 C13 0.23409 0.81288 0.42180 1.00000 0.05586 0.05529 0.05101 0.00236 0.00530 -0.01555 0.05398 0.01058 0.00032 0.00050 0.00046 0.00000 0.00417 0.00403 0.00396 0.00340 0.00310 0.00318 0.00170 H1F 0.26859 0.76101 0.42152 1.00000 0.08097 0.00000 0.00000 H1G 0.25573 0.87673 0.43539 1.00000 0.08097 0.00000 0.00000 H1H 0.21042 0.81502 0.35602 1.00000 0.08097 0.00000 0.00000 C14 0.21867 0.78785 0.60787 1.00000 0.07597 0.04322 0.04326 0.00360 -0.01482 -0.01334 0.05446 0.00981 0.00035 0.00047 0.00045 0.00000 0.00456 0.00363 0.00361 0.00322 0.00319 0.00323 0.00171 H1I 0.18582 0.77055 0.65885 1.00000 0.08168 0.00000 0.00000 H1J 0.23809 0.85280 0.62339 1.00000 0.08168 0.00000 0.00000 H1K 0.25478 0.73834 0.60790 1.00000 0.08168 0.00000 0.00000 N4 0.44898 0.66037 0.93530 1.00000 0.04233 0.02911 0.02772 0.00059 0.00617 -0.00365 0.03296 0.00731 0.00022 0.00031 0.00032 0.00000 0.00278 0.00246 0.00258 0.00213 0.00197 0.00196 0.00108 N5 0.44925 0.72903 1.08905 1.00000 0.04651 0.02825 0.04421 -0.00838 0.00113 -0.00531 0.03966 0.00748 0.00023 0.00032 0.00035 0.00000 0.00293 0.00254 0.00277 0.00236 0.00219 0.00210 0.00117 N6 0.39195 0.57157 1.06762 1.00000 0.04403 0.03323 0.02891 0.00674 0.00297 -0.00035 0.03535 0.00755 0.00023 0.00033 0.00032 0.00000 0.00277 0.00259 0.00256 0.00219 0.00200 0.00215 0.00109 O6 0.58613 0.62842 1.01397 1.00000 0.06568 0.03700 0.04015 0.00088 -0.00171 0.00665 0.04767 0.00673 0.00022 0.00028 0.00027 0.00000 0.00282 0.00230 0.00227 0.00199 0.00195 0.00206 0.00106 H6 0.59430 0.57083 0.99502 1.00000 0.07150 0.00000 0.00000 O7 0.45845 0.63094 0.76540 1.00000 0.05232 0.03922 0.03166 0.00607 0.00957 -0.00103 0.04091 0.00638 0.00019 0.00027 0.00027 0.00000 0.00248 0.00232 0.00215 0.00185 0.00183 0.00178 0.00097 O8 0.37808 0.54825 0.85539 1.00000 0.04076 0.02988 0.03157 0.00030 0.00381 -0.00589 0.03402 0.00582 0.00018 0.00025 0.00026 0.00000 0.00223 0.00192 0.00195 0.00171 0.00161 0.00167 0.00088 O9 0.38580 0.63598 1.23362 1.00000 0.11476 0.07431 0.04283 -0.01196 0.02941 -0.05175 0.07679 0.00809 0.00027 0.00038 0.00033 0.00000 0.00427 0.00340 0.00260 0.00273 0.00259 0.00304 0.00162 O10 0.33831 0.49011 1.18987 1.00000 0.08701 0.04351 0.03404 -0.00295 0.02496 -0.02237 0.05442 0.00679 0.00022 0.00029 0.00028 0.00000 0.00324 0.00248 0.00224 0.00206 0.00206 0.00229 0.00118 C15 0.57381 0.69039 0.92733 1.00000 0.04381 0.04545 0.03476 0.00842 -0.00186 -0.00515 0.04140 0.01004 0.00029 0.00045 0.00043 0.00000 0.00366 0.00346 0.00330 0.00301 0.00257 0.00276 0.00145 H1L 0.57687 0.65045 0.86519 1.00000 0.04967 0.00000 0.00000 H1M 0.60877 0.74259 0.92544 1.00000 0.04967 0.00000 0.00000 C16 0.50326 0.73821 0.93123 1.00000 0.04319 0.03234 0.03421 0.00253 0.00341 -0.00737 0.03654 0.00899 0.00027 0.00040 0.00042 0.00000 0.00353 0.00308 0.00314 0.00267 0.00244 0.00251 0.00136 H16 0.49526 0.78185 0.87132 1.00000 0.04384 0.00000 0.00000 C17 0.49163 0.79655 1.02968 1.00000 0.05126 0.03295 0.04146 -0.00129 0.00528 -0.00923 0.04182 0.00962 0.00030 0.00042 0.00042 0.00000 0.00376 0.00314 0.00344 0.00293 0.00274 0.00265 0.00145 H1N 0.53504 0.81081 1.06567 1.00000 0.05018 0.00000 0.00000 H1O 0.46778 0.85948 1.01546 1.00000 0.05018 0.00000 0.00000 C18 0.42689 0.64956 1.03594 1.00000 0.03746 0.03183 0.03209 0.00170 -0.00098 0.00300 0.03383 0.00917 0.00027 0.00040 0.00041 0.00000 0.00326 0.00313 0.00317 0.00276 0.00245 0.00258 0.00131 C19 0.42969 0.61154 0.84464 1.00000 0.04118 0.03426 0.03031 0.00022 -0.00182 0.00334 0.03530 0.00934 0.00028 0.00041 0.00041 0.00000 0.00346 0.00320 0.00326 0.00285 0.00263 0.00267 0.00132 C20 0.35241 0.48869 0.76573 1.00000 0.05336 0.03720 0.02689 -0.00885 -0.00372 -0.00504 0.03924 0.00883 0.00029 0.00042 0.00039 0.00000 0.00369 0.00325 0.00305 0.00280 0.00254 0.00274 0.00140 C21 0.32274 0.55806 0.68403 1.00000 0.05891 0.05144 0.03367 0.00180 -0.00018 -0.00492 0.04803 0.01025 0.00032 0.00046 0.00043 0.00000 0.00402 0.00375 0.00322 0.00304 0.00278 0.00303 0.00154 H2A 0.29158 0.60475 0.71470 1.00000 0.07205 0.00000 0.00000 H2B 0.29829 0.51911 0.63261 1.00000 0.07205 0.00000 0.00000 H2C 0.35947 0.59446 0.65278 1.00000 0.07205 0.00000 0.00000 C22 0.29534 0.42619 0.81258 1.00000 0.06012 0.03934 0.03742 -0.00707 -0.00877 -0.00858 0.04581 0.00926 0.00031 0.00044 0.00043 0.00000 0.00399 0.00339 0.00326 0.00289 0.00281 0.00287 0.00152 H2D 0.31377 0.38945 0.87067 1.00000 0.06872 0.00000 0.00000 H2E 0.27714 0.37976 0.76216 1.00000 0.06872 0.00000 0.00000 H2F 0.25915 0.46996 0.83442 1.00000 0.06872 0.00000 0.00000 C23 0.40844 0.42205 0.72758 1.00000 0.07077 0.04019 0.04660 -0.01047 0.01048 -0.00064 0.05236 0.01106 0.00034 0.00045 0.00047 0.00000 0.00444 0.00357 0.00364 0.00318 0.00312 0.00311 0.00164 H2G 0.44369 0.46262 0.69782 1.00000 0.07853 0.00000 0.00000 H2H 0.38957 0.37685 0.67651 1.00000 0.07853 0.00000 0.00000 H2I 0.42800 0.38392 0.78391 1.00000 0.07853 0.00000 0.00000 C24 0.37370 0.57200 1.16876 1.00000 0.04119 0.03189 0.03836 -0.00242 0.00579 -0.00055 0.03706 0.01033 0.00028 0.00043 0.00045 0.00000 0.00342 0.00330 0.00355 0.00304 0.00265 0.00259 0.00136 C25 0.31581 0.46824 1.29535 1.00000 0.08956 0.03864 0.04011 -0.00374 0.02382 -0.01476 0.05569 0.01135 0.00038 0.00046 0.00047 0.00000 0.00529 0.00357 0.00359 0.00319 0.00354 0.00335 0.00180 C26 0.26316 0.53674 1.32593 1.00000 0.07699 0.19855 0.07972 0.06902 0.04802 0.07268 0.11756 0.02148 0.00043 0.00086 0.00065 0.00000 0.00583 0.01096 0.00558 0.00682 0.00473 0.00675 0.00420 H2J 0.28223 0.60323 1.33254 1.00000 0.17635 0.00000 0.00000 H2K 0.24557 0.51576 1.39078 1.00000 0.17635 0.00000 0.00000 H2L 0.22636 0.53716 1.27498 1.00000 0.17635 0.00000 0.00000 C27 0.28851 0.36498 1.28188 1.00000 0.69854 0.18606 0.12163 -0.09188 0.24510 -0.29658 0.33106 0.02893 0.00134 0.00111 0.00101 0.00000 0.04210 0.01405 0.00962 0.01033 0.01799 0.02186 0.01708 H2M 0.30191 0.32480 1.34045 1.00000 0.49659 0.00000 0.00000 H2N 0.30683 0.33576 1.22090 1.00000 0.49659 0.00000 0.00000 H2O 0.23907 0.36731 1.27555 1.00000 0.49659 0.00000 0.00000 C28 0.37413 0.46846 1.36783 1.00000 0.09902 0.34782 0.08706 0.13788 0.05085 0.11279 0.17707 0.02787 0.00051 0.00121 0.00072 0.00000 0.00749 0.01933 0.00650 0.00977 0.00576 0.01000 0.00730 H2P 0.38775 0.53666 1.38221 1.00000 0.26560 0.00000 0.00000 H2Q 0.41201 0.43276 1.33879 1.00000 0.26560 0.00000 0.00000 H2R 0.36121 0.43611 1.43042 1.00000 0.26560 0.00000 0.00000 Final Structure Factor Calculation for 02SRC141 in P2(1)/c Total number of l.s. parameters = 411 Maximum vector length = 511 Memory required = 4923 / 22995 wR2 = 0.2612 before cycle 5 for 5259 data and 0 / 411 parameters GooF = S = 1.013; Restrained GooF = 1.013 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1413 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0849 for 2675 Fo > 4sig(Fo) and 0.1774 for all 5259 data wR2 = 0.2612, GooF = S = 1.013, Restrained GooF = 1.013 for all data Occupancy sum of asymmetric unit = 44.00 for non-hydrogen and 48.00 for hydrogen atoms Principal mean square atomic displacements U 0.0433 0.0342 0.0301 N1 0.0488 0.0371 0.0248 N2 0.0403 0.0336 0.0250 N3 0.0634 0.0388 0.0312 O1 0.0500 0.0401 0.0314 O2 0.0407 0.0349 0.0309 O3 0.0541 0.0360 0.0279 O4 0.0491 0.0361 0.0246 O5 0.0442 0.0366 0.0277 C1 0.0439 0.0312 0.0274 C2 0.0575 0.0377 0.0315 C3 0.0358 0.0330 0.0218 C4 0.0431 0.0386 0.0262 C5 0.0431 0.0393 0.0229 C6 0.0587 0.0508 0.0369 C7 0.0603 0.0480 0.0313 C8 0.0648 0.0372 0.0339 C9 0.0386 0.0326 0.0271 C10 0.0532 0.0336 0.0266 C11 0.0653 0.0479 0.0294 C12 0.0712 0.0525 0.0383 C13 0.0876 0.0398 0.0360 C14 0.0446 0.0293 0.0251 N4 0.0495 0.0458 0.0237 N5 0.0442 0.0380 0.0238 N6 0.0676 0.0404 0.0351 O6 0.0551 0.0419 0.0257 O7 0.0438 0.0315 0.0268 O8 0.1567 0.0431 0.0305 O9 0.1032 0.0375 0.0226 O10 0.0538 0.0402 0.0301 C15 0.0470 0.0357 0.0270 C16 0.0562 0.0402 0.0291 C17 0.0390 0.0336 0.0289 C18 0.0431 0.0333 0.0295 C19 0.0551 0.0420 0.0206 C20 0.0616 0.0491 0.0335 C21 0.0655 0.0455 0.0264 C22 0.0739 0.0515 0.0317 C23 0.0448 0.0354 0.0309 C24 0.1010 0.0358 0.0303 C25 0.2666 0.0552 0.0309 C26 may be split into 0.2682 0.5510 1.3328 and 0.2582 0.5225 1.3190 0.9065 0.0618 0.0249 C27 may be split into 0.3094 0.3514 1.2921 and 0.2676 0.3786 1.2717 0.4477 0.0559 0.0276 C28 may be split into 0.3797 0.4890 1.3766 and 0.3686 0.4480 1.3590 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.005 0.010 0.015 0.020 0.027 0.035 0.046 0.061 0.089 1.000 Number in group 593. 535. 496. 485. 569. 500. 533. 500. 529. 519. GooF 0.907 0.903 1.003 0.953 1.087 1.151 1.103 1.161 0.997 0.818 K 4.957 2.401 1.480 1.231 1.028 1.044 1.049 1.049 1.023 0.996 Resolution(A) 0.84 0.88 0.92 0.97 1.02 1.09 1.18 1.30 1.48 1.85 inf Number in group 534. 530. 515. 540. 525. 515. 528. 518. 531. 523. GooF 0.832 0.864 0.892 0.905 0.972 0.981 1.059 1.023 1.068 1.413 K 1.288 1.168 1.130 1.063 1.042 1.025 1.020 1.019 1.046 0.986 R1 0.552 0.427 0.347 0.234 0.181 0.155 0.128 0.112 0.092 0.071 Recommended weighting scheme: WGHT 0.1107 1.3985 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) 2 1 2 544.34 109.04 9.86 0.029 4.95 1 4 3 452.40 0.19 8.54 0.001 2.61 -6 7 4 98.73 753.16 7.45 0.076 1.47 -6 9 4 0.00 453.53 7.23 0.059 1.25 5 2 0 234.38 27.99 6.81 0.015 3.35 2 6 5 333.93 78.08 6.44 0.024 1.66 2 3 2 164.55 0.37 5.71 0.002 3.40 -3 6 3 658.01 141.86 5.09 0.033 1.89 9 2 3 132.60 20.61 4.90 0.013 1.83 -2 2 5 166.25 9.89 4.74 0.009 2.36 -4 1 3 169.17 12.92 4.63 0.010 3.18 6 7 10 48.87 306.98 4.58 0.048 1.01 0 6 3 381.84 18.74 4.57 0.012 1.97 -2 1 4 164.62 19.48 4.37 0.012 3.03 8 2 0 796.52 407.25 4.12 0.056 2.27 1 7 6 497.12 184.64 4.10 0.038 1.42 2 2 0 806.61 471.69 4.02 0.060 5.48 4 0 2 786.84 321.11 3.86 0.050 3.83 -3 2 3 229.78 90.15 3.79 0.026 3.20 8 3 4 104.73 22.25 3.66 0.013 1.76 -5 1 4 505.03 34.97 3.57 0.016 2.48 7 4 2 208.31 105.41 3.56 0.028 2.01 -5 2 1 206.06 0.32 3.50 0.002 3.26 2 7 6 118.59 4.24 3.44 0.006 1.41 -10 6 1 250.08 75.49 3.42 0.024 1.45 9 2 0 685.60 243.32 3.42 0.043 2.05 -4 2 1 870.61 532.04 3.39 0.064 3.77 -8 9 3 243.85 87.48 3.36 0.026 1.21 10 8 1 168.25 68.43 3.28 0.023 1.25 -2 2 1 606.75 1022.03 3.22 0.088 5.08 12 8 1 130.53 284.05 3.14 0.047 1.15 -4 7 5 610.99 338.01 3.13 0.051 1.47 -8 3 2 556.61 358.88 3.07 0.052 2.03 4 6 1 193.98 107.06 3.06 0.029 1.99 -11 2 7 99.67 22.81 3.06 0.013 1.27 -4 7 3 284.33 124.85 3.06 0.031 1.64 5 2 9 12.40 90.77 3.05 0.026 1.32 19 6 0 885.88 514.11 3.04 0.063 0.93 -9 6 2 19.85 90.34 3.01 0.026 1.51 -4 6 7 419.68 246.24 2.98 0.043 1.37 4 9 8 214.78 18.11 2.95 0.012 1.06 8 9 1 129.20 244.95 2.95 0.043 1.25 -14 8 2 201.72 81.11 2.94 0.025 1.05 -4 10 1 201.33 115.76 2.93 0.030 1.28 -12 1 1 299.23 185.73 2.92 0.038 1.60 13 4 5 299.72 151.92 2.89 0.034 1.19 8 2 7 0.00 71.88 2.88 0.023 1.42 -1 5 6 545.03 340.02 2.87 0.051 1.68 -7 4 10 147.60 8.29 2.87 0.008 1.12 11 5 7 611.48 378.02 2.86 0.054 1.14 Bond lengths and angles N1 - Distance Angles C5 1.3915 (0.0069) C4 1.3958 (0.0066) 132.32 (0.45) C2 1.4872 (0.0066) 118.25 (0.42) 109.43 (0.41) N1 - C5 C4 N2 - Distance Angles C4 1.3293 (0.0063) C3 1.4571 (0.0066) 113.09 (0.42) N2 - C4 N3 - Distance Angles C4 1.3190 (0.0064) C10 1.3770 (0.0068) 115.64 (0.43) N3 - C4 O1 - Distance Angles C1 1.4069 (0.0061) O1 - O2 - Distance Angles C5 1.2131 (0.0063) O2 - O3 - Distance Angles C5 1.3205 (0.0064) C6 1.4831 (0.0061) 119.97 (0.40) O3 - C5 O4 - Distance Angles C10 1.2187 (0.0060) O4 - O5 - Distance Angles C10 1.3477 (0.0062) C11 1.4842 (0.0062) 120.36 (0.39) O5 - C10 C1 - Distance Angles O1 1.4069 (0.0061) C2 1.5010 (0.0076) 110.63 (0.43) C1 - O1 C2 - Distance Angles N1 1.4872 (0.0066) C1 1.5010 (0.0076) 111.17 (0.42) C3 1.5257 (0.0076) 102.17 (0.40) 113.17 (0.46) C2 - N1 C1 C3 - Distance Angles N2 1.4571 (0.0066) C2 1.5257 (0.0076) 103.39 (0.39) C3 - N2 C4 - Distance Angles N3 1.3190 (0.0064) N2 1.3293 (0.0063) 128.89 (0.46) N1 1.3958 (0.0066) 122.65 (0.46) 108.45 (0.44) C4 - N3 N2 C5 - Distance Angles O2 1.2131 (0.0063) O3 1.3205 (0.0064) 126.86 (0.51) N1 1.3915 (0.0069) 120.25 (0.49) 112.81 (0.47) C5 - O2 O3 C6 - Distance Angles O3 1.4831 (0.0061) C7 1.4994 (0.0078) 109.71 (0.43) C8 1.5075 (0.0077) 110.50 (0.42) 112.74 (0.47) C9 1.5083 (0.0077) 102.70 (0.41) 111.37 (0.46) 109.37 (0.45) C6 - O3 C7 C8 C7 - Distance Angles C6 1.4994 (0.0078) C7 - C8 - Distance Angles C6 1.5075 (0.0077) C8 - C9 - Distance Angles C6 1.5083 (0.0077) C9 - C10 - Distance Angles O4 1.2187 (0.0060) O5 1.3477 (0.0062) 123.41 (0.46) N3 1.3770 (0.0068) 128.31 (0.48) 108.28 (0.45) C10 - O4 O5 C11 - Distance Angles O5 1.4842 (0.0062) C14 1.4998 (0.0078) 102.97 (0.42) C13 1.5025 (0.0080) 110.06 (0.45) 110.70 (0.51) C12 1.5239 (0.0081) 109.47 (0.43) 109.81 (0.50) 113.34 (0.49) C11 - O5 C14 C13 C12 - Distance Angles C11 1.5239 (0.0081) C12 - C13 - Distance Angles C11 1.5025 (0.0080) C13 - C14 - Distance Angles C11 1.4998 (0.0078) C14 - N4 - Distance Angles C19 1.3879 (0.0066) C18 1.3963 (0.0068) 131.80 (0.45) C16 1.4765 (0.0066) 118.15 (0.43) 110.05 (0.42) N4 - C19 C18 N5 - Distance Angles C18 1.3273 (0.0065) C17 1.4526 (0.0069) 113.26 (0.44) N5 - C18 N6 - Distance Angles C18 1.3099 (0.0067) C24 1.3720 (0.0070) 116.60 (0.46) N6 - C18 O6 - Distance Angles C15 1.4104 (0.0063) O6 - O7 - Distance Angles C19 1.2131 (0.0061) O7 - O8 - Distance Angles C19 1.3168 (0.0064) C20 1.4834 (0.0060) 119.71 (0.40) O8 - C19 O9 - Distance Angles C24 1.2155 (0.0065) O9 - O10 - Distance Angles C24 1.3185 (0.0065) C25 1.4801 (0.0070) 121.56 (0.45) O10 - C24 C15 - Distance Angles O6 1.4104 (0.0063) C16 1.5097 (0.0078) 110.59 (0.45) C15 - O6 C16 - Distance Angles N4 1.4765 (0.0065) C15 1.5097 (0.0079) 110.71 (0.43) C17 1.5190 (0.0078) 101.78 (0.41) 113.49 (0.46) C16 - N4 C15 C17 - Distance Angles N5 1.4526 (0.0069) C16 1.5190 (0.0078) 103.48 (0.41) C17 - N5 C18 - Distance Angles N6 1.3099 (0.0066) N5 1.3273 (0.0065) 128.95 (0.49) N4 1.3963 (0.0068) 123.43 (0.48) 107.60 (0.46) C18 - N6 N5 C19 - Distance Angles O7 1.2131 (0.0061) O8 1.3168 (0.0064) 126.45 (0.49) N4 1.3879 (0.0066) 120.24 (0.50) 113.28 (0.46) C19 - O7 O8 C20 - Distance Angles O8 1.4834 (0.0060) C23 1.4961 (0.0081) 110.22 (0.45) C21 1.5081 (0.0077) 109.97 (0.43) 113.16 (0.46) C22 1.5234 (0.0078) 101.95 (0.38) 110.63 (0.47) 110.35 (0.48) C20 - O8 C23 C21 C21 - Distance Angles C20 1.5081 (0.0077) C21 - C22 - Distance Angles C20 1.5234 (0.0078) C22 - C23 - Distance Angles C20 1.4961 (0.0081) C23 - C24 - Distance Angles O9 1.2155 (0.0065) O10 1.3185 (0.0065) 121.53 (0.50) N6 1.3720 (0.0070) 128.23 (0.51) 110.24 (0.49) C24 - O9 O10 C25 - Distance Angles C26 1.4315 (0.0101) C28 1.4516 (0.0124) 111.49 (0.77) C27 1.4781 (0.0120) 111.51 (1.17) 110.39 (1.31) O10 1.4801 (0.0070) 111.33 (0.57) 110.96 (0.57) 100.71 (0.55) C25 - C26 C28 C27 C26 - Distance Angles C25 1.4315 (0.0101) C26 - C27 - Distance Angles C25 1.4781 (0.0120) C27 - C28 - Distance Angles C25 1.4516 (0.0123) C28 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.82 2.09 2.904(5) 171.4 O1-H1...N3_$1 0.82 2.60 3.025(5) 113.4 O1-H1...O3_$1 0.82 2.08 2.895(6) 173.5 O6-H6...N6_$2 0.82 2.55 2.967(5) 112.7 O6-H6...O8_$2 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)