+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 10:05:14 on 18-Jun-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01SRC413 in P2(1)/n CELL 0.71073 11.8293 10.3312 21.6318 90.000 100.203 90.000 ZERR 4.00 0.0002 0.0002 0.0005 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O P UNIT 88 128 12 28 12 V = 2601.84 F(000) = 1144.0 Mu = 0.28 mm-1 Cell Wt = 2173.66 Rho = 1.387 MERG 2 OMIT -3.00 55.00 OMIT -3 0 7 OMIT 4 3 0 OMIT -5 1 5 OMIT 1 0 9 OMIT 2 2 7 OMIT 1 1 10 EXTI 0.00522 FMAP 2 PLAN 10 SIZE 0.07 0.20 0.26 ACTA BOND $H CONF WGHT 0.07760 1.30160 L.S. 4 TEMP 20.00 FVAR 0.35971 C1 1 0.301711 0.945407 0.212625 11.00000 0.09254 0.05580 = 0.06871 0.01968 0.01892 0.00905 AFIX 137 H1A 2 0.296218 0.894580 0.175059 11.00000 -1.50000 H1B 2 0.291033 0.890553 0.246948 11.00000 -1.50000 H1C 2 0.376094 0.985281 0.221879 11.00000 -1.50000 AFIX 0 C2 1 0.367975 0.889876 0.035281 11.00000 0.13824 0.05837 = 0.07804 0.00757 0.03859 0.02812 AFIX 137 H2A 2 0.409697 0.915976 0.075515 11.00000 -1.50000 H2B 2 0.418876 0.845958 0.012300 11.00000 -1.50000 H2C 2 0.306752 0.832665 0.041064 11.00000 -1.50000 AFIX 0 C3 1 -0.004151 1.165364 0.141888 11.00000 0.04654 0.06654 = 0.07905 -0.00105 0.01052 -0.01662 AFIX 23 H3A 2 -0.014661 1.105367 0.174895 11.00000 -1.20000 H3B 2 -0.008050 1.116937 0.103151 11.00000 -1.20000 AFIX 0 C4 1 -0.095451 1.264651 0.134248 11.00000 0.04629 0.10513 = 0.11325 -0.00367 0.02353 -0.00605 AFIX 23 H4A 2 -0.169561 1.223765 0.133280 11.00000 -1.20000 H4B 2 -0.082177 1.324338 0.169403 11.00000 -1.20000 AFIX 0 C5 1 -0.194464 1.406562 0.058541 11.00000 0.06918 0.12153 = 0.14287 -0.04448 -0.01848 0.04525 AFIX 23 H5A 2 -0.203941 1.467577 0.091321 11.00000 -1.20000 H5B 2 -0.261275 1.350498 0.051153 11.00000 -1.20000 AFIX 0 C6 1 -0.185131 1.477133 0.000520 11.00000 0.10701 0.08440 = 0.16647 -0.02659 -0.05292 0.03412 AFIX 23 H6A 2 -0.253392 1.529307 -0.012428 11.00000 -1.20000 H6B 2 -0.119241 1.534538 0.008150 11.00000 -1.20000 AFIX 0 C7 1 -0.136823 1.451654 -0.097859 11.00000 0.06777 0.10331 = 0.19015 0.06981 0.00166 0.01024 AFIX 23 H7A 2 -0.076251 1.513021 -0.082559 11.00000 -1.20000 H7B 2 -0.200522 1.498715 -0.122202 11.00000 -1.20000 AFIX 0 C8 1 -0.094554 1.354596 -0.137409 11.00000 0.08170 0.17890 = 0.10410 0.06004 -0.01103 0.02582 AFIX 23 H8A 2 -0.151355 1.286210 -0.145990 11.00000 -1.20000 H8B 2 -0.088392 1.394651 -0.177233 11.00000 -1.20000 AFIX 0 C9 1 0.008385 1.202367 -0.064847 11.00000 0.06907 0.07968 = 0.09719 0.01207 0.00745 -0.00834 AFIX 23 H9A 2 -0.058018 1.147259 -0.077668 11.00000 -1.20000 H9B 2 -0.000075 1.244886 -0.025947 11.00000 -1.20000 AFIX 0 C10 1 0.111206 1.124684 -0.054797 11.00000 0.07499 0.07557 = 0.06760 -0.00525 -0.00992 -0.01291 AFIX 23 H10A 2 0.126262 1.094907 -0.095086 11.00000 -1.20000 H10B 2 0.098778 1.049052 -0.030286 11.00000 -1.20000 AFIX 0 C11 1 0.546280 1.178778 0.172332 11.00000 0.04153 0.04191 = 0.05137 0.00562 0.01046 -0.00300 C12 1 0.580872 1.201362 0.236505 11.00000 0.06654 0.07034 = 0.05991 -0.00141 -0.00640 0.01297 AFIX 43 H12 2 0.543914 1.264370 0.256316 11.00000 -1.20000 AFIX 0 C13 1 0.669608 1.130801 0.270805 11.00000 0.07780 0.09071 = 0.07473 0.01052 -0.01782 0.00994 AFIX 43 H13 2 0.691582 1.146295 0.313600 11.00000 -1.20000 AFIX 0 C14 1 0.725460 1.038304 0.242365 11.00000 0.05621 0.07513 = 0.11159 0.02483 -0.00525 0.00867 AFIX 43 H14 2 0.785010 0.990902 0.265701 11.00000 -1.20000 AFIX 0 C15 1 0.693082 1.016001 0.179315 11.00000 0.05765 0.05679 = 0.12683 0.00739 0.03028 0.01490 AFIX 43 H15 2 0.730949 0.952975 0.160028 11.00000 -1.20000 AFIX 0 C16 1 0.603830 1.086671 0.143469 11.00000 0.05377 0.05644 = 0.06989 -0.00100 0.01909 0.00179 AFIX 43 H16 2 0.583410 1.071747 0.100543 11.00000 -1.20000 AFIX 0 C17 1 0.462097 1.431050 0.132432 11.00000 0.03914 0.04244 = 0.04481 0.00206 0.00595 0.00208 C18 1 0.439074 1.512587 0.179633 11.00000 0.06099 0.05019 = 0.05545 -0.00500 0.01153 0.00201 AFIX 43 H18 2 0.400183 1.480956 0.210246 11.00000 -1.20000 AFIX 0 C19 1 0.473487 1.640147 0.181423 11.00000 0.08665 0.04426 = 0.07471 -0.00775 0.00275 0.00482 AFIX 43 H19 2 0.457137 1.694560 0.212938 11.00000 -1.20000 AFIX 0 C20 1 0.531823 1.686857 0.136753 11.00000 0.08049 0.03914 = 0.09357 0.00638 -0.00831 -0.00556 AFIX 43 H20 2 0.555548 1.772803 0.138408 11.00000 -1.20000 AFIX 0 C21 1 0.555352 1.608697 0.090017 11.00000 0.07167 0.06061 = 0.08557 0.02257 0.01848 -0.01174 AFIX 43 H21 2 0.594959 1.641361 0.059933 11.00000 -1.20000 AFIX 0 C22 1 0.520192 1.479801 0.087167 11.00000 0.06048 0.05199 = 0.06186 0.00532 0.01998 -0.00205 AFIX 43 H22 2 0.535640 1.426596 0.054996 11.00000 -1.20000 AFIX 0 N1 3 0.211277 1.082704 0.086049 11.00000 0.05985 0.04262 = 0.04400 -0.00532 0.01400 -0.01149 N2 3 0.393782 1.213592 0.059826 11.00000 0.04815 0.05435 = 0.03756 -0.00304 0.01276 -0.00504 N3 3 0.322175 1.248042 0.172245 11.00000 0.04179 0.05196 = 0.03686 -0.00651 0.01201 -0.00711 O1 4 0.214775 1.043682 0.203647 11.00000 0.07068 0.05132 = 0.05173 0.01100 0.02515 -0.00321 O2 4 0.321716 1.000411 0.001343 11.00000 0.09948 0.04593 = 0.05424 -0.00717 0.02652 0.00759 O4 4 -0.094926 1.332107 0.077868 11.00000 0.05320 0.08542 = 0.13273 0.00925 0.00675 0.00936 O5 4 -0.172956 1.389654 -0.046914 11.00000 0.08708 0.07165 = 0.13301 0.00877 0.00864 -0.00002 O6 4 0.013782 1.297142 -0.112060 11.00000 0.06693 0.12943 = 0.09203 0.04663 0.00715 0.01019 O7 4 0.211005 1.194197 -0.022575 11.00000 0.06748 0.05341 = 0.04334 0.00442 -0.00472 -0.00844 O30 4 0.106529 1.228123 0.157826 11.00000 0.03814 0.04860 = 0.06445 -0.01022 0.01252 -0.00595 P1 5 0.219231 1.151571 0.152038 11.00000 0.04546 0.03868 = 0.04039 -0.00058 0.01282 -0.00464 P2 5 0.286845 1.124804 0.035783 11.00000 0.05701 0.03893 = 0.03602 -0.00298 0.01012 -0.00237 P3 5 0.421384 1.263069 0.131079 11.00000 0.03905 0.04160 = 0.03634 -0.00109 0.00973 -0.00161 HKLF 4 Covalent radii and connectivity table for 01SRC413 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 C1 - O1 C2 - O2 C3 - O30 C4 C4 - O4 C3 C5 - O4 C6 C6 - O5 C5 C7 - O5 C8 C8 - O6 C7 C9 - O6 C10 C10 - C9 O7 C11 - C16 C12 P3 C12 - C13 C11 C13 - C14 C12 C14 - C13 C15 C15 - C14 C16 C16 - C11 C15 C17 - C22 C18 P3 C18 - C19 C17 C19 - C20 C18 C20 - C21 C19 C21 - C20 C22 C22 - C17 C21 N1 - P1 P2 N2 - P2 P3 N3 - P1 P3 O1 - C1 P1 O2 - C2 P2 O4 - C4 C5 O5 - C6 C7 O6 - C9 C8 O7 - C10 P2 O30 - C3 P1 P1 - O30 N3 N1 O1 P2 - N2 O2 O7 N1 P3 - N3 N2 C17 C11 19305 Reflections read, of which 491 rejected -14 =< h =< 15, -12 =< k =< 13, -27 =< l =< 28, Max. 2-theta = 54.93 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -2 2 2 984.61 4.05 4 267.93 -10 1 10 19.99 0.84 3 4.28 -7 2 10 39.63 0.89 4 11.42 3 Inconsistent equivalents 5841 Unique reflections, of which 0 suppressed R(int) = 0.0376 R(sigma) = 0.0450 Friedel opposites merged Maximum memory for data reduction = 3772 / 58894 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 = 4685 / 401713 wR2 = 0.1533 before cycle 1 for 5841 data and 319 / 319 parameters GooF = S = 1.004; Restrained GooF = 1.004 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0776 * P )^2 + 1.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36086 0.00088 1.312 OSF 2 0.00590 0.00111 0.610 EXTI Mean shift/esd = 0.279 Maximum = 1.312 for OSF Max. shift = 0.024 A for H2B Max. dU =-0.002 for C6 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4685 / 401713 wR2 = 0.1526 before cycle 2 for 5841 data and 319 / 319 parameters GooF = S = 1.000; Restrained GooF = 1.000 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0776 * P )^2 + 1.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36095 0.00088 0.104 OSF 2 0.00613 0.00114 0.202 EXTI Mean shift/esd = 0.093 Maximum = 0.499 for tors H2A Max. shift = 0.016 A for H2B Max. dU = 0.000 for C5 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4685 / 401713 wR2 = 0.1525 before cycle 3 for 5841 data and 319 / 319 parameters GooF = S = 1.000; Restrained GooF = 1.000 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0776 * P )^2 + 1.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36095 0.00088 -0.002 OSF 2 0.00613 0.00115 -0.001 EXTI Mean shift/esd = 0.008 Maximum = 0.172 for tors H2A Max. shift = 0.005 A for H2B Max. dU = 0.000 for C9 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4685 / 401713 wR2 = 0.1525 before cycle 4 for 5841 data and 319 / 319 parameters GooF = S = 1.000; Restrained GooF = 1.000 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0776 * P )^2 + 1.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36095 0.00088 -0.003 OSF 2 0.00613 0.00115 -0.001 EXTI Mean shift/esd = 0.003 Maximum = 0.061 for tors H2A Max. shift = 0.002 A for H2B Max. dU = 0.000 for C6 Largest correlation matrix elements 0.506 U23 C7 / U22 C7 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.2981 0.8961 0.1749 137 0.960 0.000 C1 O1 H1A H1B 0.2902 0.8893 0.2464 137 0.960 0.000 C1 O1 H1A H1C 0.3763 0.9855 0.2231 137 0.960 0.000 C1 O1 H1A H2A 0.4067 0.9156 0.0764 137 0.960 0.000 C2 O2 H2A H2B 0.4220 0.8485 0.0134 137 0.960 0.000 C2 O2 H2A H2C 0.3073 0.8307 0.0394 137 0.960 0.000 C2 O2 H2A H3A -0.0143 1.1051 0.1748 23 0.970 0.000 C3 O30 C4 H3B -0.0081 1.1172 0.1030 23 0.970 0.000 C3 O30 C4 H4A -0.1695 1.2237 0.1337 23 0.970 0.000 C4 O4 C3 H4B -0.0819 1.3243 0.1696 23 0.970 0.000 C4 O4 C3 H5A -0.2036 1.4676 0.0916 23 0.970 0.000 C5 O4 C6 H5B -0.2615 1.3506 0.0515 23 0.970 0.000 C5 O4 C6 H6A -0.2529 1.5297 -0.0125 23 0.970 0.000 C6 O5 C5 H6B -0.1187 1.5341 0.0080 23 0.970 0.000 C6 O5 C5 H7A -0.0759 1.5125 -0.0827 23 0.970 0.000 C7 O5 C8 H7B -0.2002 1.4988 -0.1224 23 0.970 0.000 C7 O5 C8 H8A -0.1514 1.2851 -0.1454 23 0.970 0.000 C8 O6 C7 H8B -0.0892 1.3931 -0.1774 23 0.970 0.000 C8 O6 C7 H9A -0.0580 1.1472 -0.0775 23 0.970 0.000 C9 O6 C10 H9B 0.0001 1.2446 -0.0257 23 0.970 0.000 C9 O6 C10 H10A 0.1258 1.0950 -0.0952 23 0.970 0.000 C10 C9 O7 H10B 0.0985 1.0490 -0.0303 23 0.970 0.000 C10 C9 O7 H12 0.5436 1.2639 0.2562 43 0.930 0.000 C12 C13 C11 H13 0.6922 1.1469 0.3135 43 0.930 0.000 C13 C14 C12 H14 0.7850 0.9907 0.2657 43 0.930 0.000 C14 C13 C15 H15 0.7308 0.9526 0.1603 43 0.930 0.000 C15 C14 C16 H16 0.5831 1.0717 0.1005 43 0.930 0.000 C16 C11 C15 H18 0.4000 1.4810 0.2101 43 0.930 0.000 C18 C19 C17 H19 0.4577 1.6944 0.2129 43 0.930 0.000 C19 C20 C18 H20 0.5546 1.7731 0.1385 43 0.930 0.000 C20 C21 C19 H21 0.5952 1.6415 0.0600 43 0.930 0.000 C21 C20 C22 H22 0.5356 1.4265 0.0550 43 0.930 0.000 C22 C17 C21 01SRC413 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.30211 0.94553 0.21276 1.00000 0.09292 0.05656 0.06642 0.01899 0.01859 0.00884 0.07142 0.00698 0.00032 0.00031 0.00016 0.00000 0.00238 0.00174 0.00194 0.00150 0.00170 0.00170 0.00087 H1A 0.29813 0.89610 0.17485 1.00000 0.10713 0.00000 0.00000 H1B 0.29022 0.88933 0.24636 1.00000 0.10713 0.00000 0.00000 H1C 0.37632 0.98550 0.22315 1.00000 0.10713 0.00000 0.00000 C2 0.36818 0.88994 0.03540 1.00000 0.13789 0.05798 0.07849 0.00696 0.03829 0.02833 0.08912 0.00858 0.00041 0.00034 0.00018 0.00000 0.00360 0.00192 0.00238 0.00173 0.00236 0.00218 0.00122 H2A 0.40669 0.91560 0.07641 1.00000 0.13368 0.00000 0.00000 H2B 0.42196 0.84846 0.01343 1.00000 0.13368 0.00000 0.00000 H2C 0.30734 0.83074 0.03940 1.00000 0.13368 0.00000 0.00000 C3 -0.00403 1.16534 0.14186 1.00000 0.04640 0.06653 0.07904 -0.00088 0.01050 -0.01678 0.06406 0.00552 0.00024 0.00031 0.00016 0.00000 0.00151 0.00187 0.00212 0.00156 0.00140 0.00141 0.00079 H3A -0.01434 1.10506 0.17480 1.00000 0.07687 0.00000 0.00000 H3B -0.00806 1.11721 0.10303 1.00000 0.07687 0.00000 0.00000 C4 -0.09536 1.26451 0.13452 1.00000 0.04637 0.10352 0.11607 -0.00484 0.02356 -0.00636 0.08753 0.00757 0.00028 0.00043 0.00021 0.00000 0.00176 0.00296 0.00329 0.00250 0.00191 0.00183 0.00117 H4A -0.16945 1.22366 0.13367 1.00000 0.10504 0.00000 0.00000 H4B -0.08185 1.32429 0.16963 1.00000 0.10504 0.00000 0.00000 C5 -0.19457 1.40655 0.05877 1.00000 0.06941 0.12026 0.14818 -0.04722 -0.02144 0.04546 0.11758 0.00861 0.00036 0.00052 0.00027 0.00000 0.00244 0.00369 0.00449 0.00357 0.00270 0.00257 0.00187 H5A -0.20363 1.46764 0.09159 1.00000 0.14110 0.00000 0.00000 H5B -0.26148 1.35063 0.05150 1.00000 0.14110 0.00000 0.00000 C6 -0.18493 1.47713 0.00040 1.00000 0.10544 0.08440 0.16334 -0.02374 -0.04991 0.03309 0.12671 0.00904 0.00044 0.00049 0.00030 0.00000 0.00350 0.00296 0.00514 0.00340 0.00352 0.00264 0.00212 H6A -0.25292 1.52975 -0.01254 1.00000 0.15206 0.00000 0.00000 H6B -0.11873 1.53409 0.00796 1.00000 0.15206 0.00000 0.00000 C7 -0.13673 1.45146 -0.09797 1.00000 0.06764 0.10398 0.18968 0.06924 0.00048 0.00999 0.12316 0.01097 0.00039 0.00051 0.00031 0.00000 0.00249 0.00346 0.00561 0.00388 0.00302 0.00245 0.00203 H7A -0.07587 1.51248 -0.08266 1.00000 0.14779 0.00000 0.00000 H7B -0.20016 1.49881 -0.12238 1.00000 0.14779 0.00000 0.00000 C8 -0.09487 1.35379 -0.13736 1.00000 0.08014 0.18233 0.10443 0.06208 -0.00737 0.02594 0.12519 0.01133 0.00040 0.00065 0.00024 0.00000 0.00287 0.00570 0.00352 0.00374 0.00255 0.00336 0.00205 H8A -0.15144 1.28507 -0.14544 1.00000 0.15023 0.00000 0.00000 H8B -0.08921 1.39309 -0.17743 1.00000 0.15023 0.00000 0.00000 C9 0.00841 1.20225 -0.06467 1.00000 0.06847 0.08083 0.09401 0.01108 0.00836 -0.00976 0.08184 0.00741 0.00032 0.00039 0.00019 0.00000 0.00213 0.00231 0.00265 0.00205 0.00187 0.00185 0.00101 H9A -0.05804 1.14722 -0.07748 1.00000 0.09820 0.00000 0.00000 H9B 0.00012 1.24456 -0.02569 1.00000 0.09820 0.00000 0.00000 C10 0.11088 1.12466 -0.05482 1.00000 0.07506 0.07601 0.06615 -0.00490 -0.01115 -0.01186 0.07529 0.00572 0.00030 0.00035 0.00017 0.00000 0.00214 0.00214 0.00202 0.00167 0.00165 0.00181 0.00093 H10A 0.12581 1.09501 -0.09515 1.00000 0.09035 0.00000 0.00000 H10B 0.09852 1.04896 -0.03033 1.00000 0.09035 0.00000 0.00000 C11 0.54642 1.17870 0.17236 1.00000 0.04170 0.04177 0.05155 0.00535 0.01073 -0.00293 0.04471 0.00471 0.00021 0.00024 0.00012 0.00000 0.00125 0.00126 0.00144 0.00106 0.00107 0.00105 0.00055 C12 0.58087 1.20112 0.23638 1.00000 0.06787 0.07039 0.05990 -0.00148 -0.00812 0.01358 0.06842 0.00593 0.00028 0.00034 0.00015 0.00000 0.00191 0.00195 0.00184 0.00152 0.00148 0.00162 0.00084 H12 0.54363 1.26387 0.25620 1.00000 0.08210 0.00000 0.00000 C13 0.66992 1.13095 0.27077 1.00000 0.07903 0.09113 0.07600 0.01047 -0.01861 0.01049 0.08600 0.00723 0.00034 0.00039 0.00019 0.00000 0.00232 0.00262 0.00235 0.00201 0.00189 0.00212 0.00111 H13 0.69220 1.14691 0.31350 1.00000 0.10319 0.00000 0.00000 C14 0.72553 1.03815 0.24234 1.00000 0.05544 0.07517 0.11446 0.02507 -0.00358 0.00906 0.08396 0.00790 0.00030 0.00039 0.00022 0.00000 0.00186 0.00230 0.00323 0.00224 0.00197 0.00173 0.00110 H14 0.78503 0.99065 0.26566 1.00000 0.10075 0.00000 0.00000 C15 0.69302 1.01583 0.17951 1.00000 0.05808 0.05756 0.12305 0.00746 0.02860 0.01509 0.07803 0.00776 0.00029 0.00033 0.00021 0.00000 0.00182 0.00185 0.00330 0.00196 0.00202 0.00156 0.00102 H15 0.73077 0.95264 0.16026 1.00000 0.09364 0.00000 0.00000 C16 0.60356 1.08667 0.14346 1.00000 0.05328 0.05620 0.07267 -0.00102 0.02028 0.00167 0.05960 0.00582 0.00024 0.00029 0.00015 0.00000 0.00157 0.00164 0.00194 0.00141 0.00140 0.00134 0.00072 H16 0.58306 1.07168 0.10054 1.00000 0.07152 0.00000 0.00000 C17 0.46217 1.43108 0.13249 1.00000 0.03962 0.04268 0.04422 0.00195 0.00605 0.00203 0.04234 0.00449 0.00020 0.00024 0.00011 0.00000 0.00118 0.00127 0.00130 0.00101 0.00099 0.00103 0.00053 C18 0.43904 1.51252 0.17955 1.00000 0.06096 0.04972 0.05625 -0.00508 0.01122 0.00182 0.05554 0.00516 0.00025 0.00027 0.00014 0.00000 0.00167 0.00149 0.00160 0.00121 0.00129 0.00128 0.00067 H18 0.39997 1.48105 0.21012 1.00000 0.06665 0.00000 0.00000 C19 0.47374 1.64015 0.18127 1.00000 0.08669 0.04390 0.07676 -0.00790 0.00245 0.00540 0.07058 0.00602 0.00031 0.00029 0.00017 0.00000 0.00229 0.00155 0.00219 0.00144 0.00180 0.00154 0.00088 H19 0.45769 1.69444 0.21291 1.00000 0.08470 0.00000 0.00000 C20 0.53139 1.68702 0.13685 1.00000 0.08029 0.03947 0.09227 0.00681 -0.00720 -0.00548 0.07341 0.00612 0.00031 0.00030 0.00018 0.00000 0.00223 0.00150 0.00252 0.00159 0.00190 0.00151 0.00095 H20 0.55460 1.77315 0.13846 1.00000 0.08810 0.00000 0.00000 C21 0.55543 1.60883 0.09003 1.00000 0.07249 0.06083 0.08558 0.02330 0.01705 -0.01163 0.07259 0.00668 0.00030 0.00032 0.00017 0.00000 0.00206 0.00187 0.00237 0.00175 0.00173 0.00162 0.00091 H21 0.59523 1.64154 0.06004 1.00000 0.08711 0.00000 0.00000 C22 0.52022 1.47972 0.08718 1.00000 0.05995 0.05186 0.06311 0.00521 0.01985 -0.00239 0.05721 0.00559 0.00025 0.00028 0.00014 0.00000 0.00165 0.00154 0.00173 0.00129 0.00136 0.00132 0.00069 H22 0.53564 1.42649 0.05501 1.00000 0.06866 0.00000 0.00000 N1 0.21124 1.08268 0.08603 1.00000 0.06009 0.04232 0.04496 -0.00563 0.01408 -0.01184 0.04854 0.00386 0.00020 0.00020 0.00010 0.00000 0.00130 0.00111 0.00115 0.00089 0.00096 0.00100 0.00051 N2 0.39368 1.21371 0.05984 1.00000 0.04838 0.05400 0.03803 -0.00303 0.01290 -0.00493 0.04617 0.00386 0.00018 0.00021 0.00009 0.00000 0.00115 0.00120 0.00106 0.00091 0.00088 0.00099 0.00049 N3 0.32212 1.24800 0.17228 1.00000 0.04230 0.05168 0.03704 -0.00641 0.01186 -0.00703 0.04309 0.00358 0.00017 0.00020 0.00009 0.00000 0.00105 0.00119 0.00104 0.00087 0.00083 0.00093 0.00047 O1 0.21493 1.04370 0.20364 1.00000 0.07089 0.05119 0.05191 0.01099 0.02521 -0.00292 0.05625 0.00372 0.00017 0.00018 0.00008 0.00000 0.00122 0.00104 0.00105 0.00086 0.00091 0.00095 0.00048 O2 0.32182 1.00054 0.00146 1.00000 0.09946 0.04608 0.05374 -0.00722 0.02561 0.00749 0.06496 0.00401 0.00020 0.00018 0.00009 0.00000 0.00160 0.00105 0.00113 0.00086 0.00106 0.00107 0.00056 O4 -0.09479 1.33198 0.07766 1.00000 0.05296 0.08553 0.13218 0.00933 0.00605 0.00852 0.09148 0.00506 0.00020 0.00026 0.00015 0.00000 0.00128 0.00172 0.00241 0.00164 0.00138 0.00124 0.00081 O5 -0.17336 1.38961 -0.04690 1.00000 0.08609 0.07150 0.13226 0.00825 0.00778 -0.00003 0.09803 0.00561 0.00024 0.00027 0.00016 0.00000 0.00182 0.00161 0.00249 0.00173 0.00168 0.00141 0.00085 O6 0.01355 1.29756 -0.11189 1.00000 0.06728 0.13019 0.09272 0.04768 0.00650 0.01123 0.09767 0.00581 0.00021 0.00032 0.00013 0.00000 0.00153 0.00227 0.00187 0.00173 0.00131 0.00152 0.00089 O7 0.21093 1.19435 -0.02255 1.00000 0.06691 0.05329 0.04425 0.00436 -0.00420 -0.00854 0.05653 0.00329 0.00017 0.00019 0.00008 0.00000 0.00121 0.00107 0.00101 0.00082 0.00086 0.00093 0.00049 O30 0.10657 1.22816 0.15776 1.00000 0.03863 0.04871 0.06392 -0.01018 0.01236 -0.00577 0.05002 0.00314 0.00014 0.00017 0.00009 0.00000 0.00090 0.00098 0.00114 0.00083 0.00079 0.00076 0.00044 P1 0.21922 1.15158 0.15205 1.00000 0.04549 0.03885 0.04039 -0.00060 0.01289 -0.00469 0.04093 0.00115 0.00005 0.00006 0.00003 0.00000 0.00035 0.00033 0.00034 0.00024 0.00026 0.00026 0.00018 P2 0.28683 1.12480 0.03577 1.00000 0.05687 0.03905 0.03596 -0.00296 0.01005 -0.00240 0.04374 0.00119 0.00006 0.00006 0.00003 0.00000 0.00040 0.00034 0.00033 0.00024 0.00027 0.00028 0.00019 P3 0.42139 1.26306 0.13107 1.00000 0.03910 0.04161 0.03638 -0.00108 0.00974 -0.00160 0.03865 0.00111 0.00005 0.00006 0.00003 0.00000 0.00032 0.00034 0.00032 0.00024 0.00024 0.00025 0.00018 Final Structure Factor Calculation for 01SRC413 in P2(1)/n Total number of l.s. parameters = 319 Maximum vector length = 511 Memory required = 4366 / 24017 wR2 = 0.1525 before cycle 5 for 5841 data and 0 / 319 parameters GooF = S = 1.000; Restrained GooF = 1.000 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0776 * P )^2 + 1.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0518 for 4160 Fo > 4sig(Fo) and 0.0793 for all 5841 data wR2 = 0.1525, GooF = S = 1.000, Restrained GooF = 1.000 for all data Occupancy sum of asymmetric unit = 35.00 for non-hydrogen and 32.00 for hydrogen atoms Principal mean square atomic displacements U 0.0964 0.0760 0.0419 C1 0.1494 0.0692 0.0487 C2 0.0796 0.0759 0.0367 C3 0.1180 0.1022 0.0424 C4 0.2213 0.0887 0.0427 C5 0.2410 0.0836 0.0555 C6 may be split into -0.1907 1.4721 0.0081 and -0.1792 1.4822 -0.0073 0.2342 0.0819 0.0534 C7 may be split into -0.1347 1.4602 -0.0899 and -0.1388 1.4427 -0.1061 0.2167 0.1112 0.0477 C8 0.1055 0.0772 0.0628 C9 0.1015 0.0780 0.0464 C10 0.0539 0.0444 0.0358 C11 0.0946 0.0658 0.0449 C12 0.1169 0.0952 0.0459 C13 0.1325 0.0743 0.0451 C14 0.1249 0.0678 0.0414 C15 0.0749 0.0567 0.0472 C16 0.0456 0.0432 0.0382 C17 0.0613 0.0590 0.0463 C18 0.0991 0.0709 0.0417 C19 0.1156 0.0664 0.0383 C20 0.1013 0.0767 0.0398 C21 0.0696 0.0567 0.0453 C22 0.0670 0.0427 0.0360 N1 0.0577 0.0461 0.0347 N2 0.0575 0.0389 0.0329 N3 0.0766 0.0589 0.0332 O1 0.1014 0.0565 0.0369 O2 0.1372 0.0867 0.0505 O4 0.1386 0.0851 0.0704 O5 0.1628 0.0761 0.0540 O6 0.0806 0.0494 0.0396 O7 0.0693 0.0449 0.0359 O30 0.0496 0.0389 0.0343 P1 0.0572 0.0401 0.0339 P2 0.0430 0.0393 0.0337 P3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.016 0.024 0.034 0.044 0.056 0.072 0.100 0.157 1.000 Number in group 590. 605. 561. 630. 555. 604. 546. 593. 575. 582. GooF 0.896 0.909 0.997 1.081 1.026 1.070 1.019 1.011 1.018 0.954 K -0.020 0.855 0.878 0.920 0.956 0.971 0.991 1.007 1.030 1.016 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 604. 587. 579. 572. 582. 581. 584. 580. 587. 585. GooF 0.874 0.879 0.932 0.928 0.943 0.949 1.034 0.941 1.030 1.389 K 1.017 1.027 0.992 1.011 1.015 1.020 1.035 1.057 1.039 0.992 R1 0.239 0.190 0.153 0.126 0.107 0.084 0.064 0.046 0.046 0.041 Recommended weighting scheme: WGHT 0.0743 1.2341 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 8 109.55 202.29 4.61 0.077 2.22 0 1 10 454.70 298.32 4.46 0.094 2.09 0 3 8 124.84 67.99 4.43 0.045 2.11 -11 6 13 70.87 200.65 4.42 0.077 0.85 3 1 1 283.00 446.56 4.37 0.115 3.49 -1 3 7 692.88 471.69 4.36 0.118 2.30 -3 3 5 68.65 30.83 4.34 0.030 2.33 2 0 2 245.96 152.34 4.34 0.067 4.76 1 1 8 80.81 154.53 4.26 0.068 2.43 -3 0 25 126.18 354.24 4.24 0.102 0.86 2 1 6 142.42 82.48 4.23 0.049 2.72 5 2 3 81.88 41.42 3.96 0.035 1.95 3 4 0 21.08 0.06 3.92 0.001 2.15 -5 0 7 205.26 315.40 3.88 0.097 2.03 5 1 3 34.08 74.81 3.86 0.047 2.06 -2 3 8 440.49 638.14 3.80 0.137 2.08 0 2 11 575.87 409.11 3.78 0.110 1.81 -8 3 1 0.00 22.99 3.64 0.026 1.35 -4 1 6 171.58 260.82 3.63 0.088 2.41 1 3 8 160.64 247.06 3.62 0.086 2.02 5 1 0 36.06 9.73 3.57 0.017 2.27 -2 2 9 181.51 119.93 3.56 0.060 2.13 -1 3 12 690.86 503.82 3.52 0.122 1.60 4 5 13 30.04 72.00 3.49 0.046 1.12 7 8 7 10.11 36.24 3.49 0.033 0.94 -2 5 3 257.26 370.57 3.46 0.105 1.91 -10 9 6 -23.72 31.75 3.41 0.031 0.82 -7 1 2 49.72 89.90 3.40 0.052 1.67 -12 0 16 649.24 447.70 3.34 0.115 0.86 -8 3 15 1.32 18.00 3.27 0.023 1.07 -2 6 5 81.38 48.43 3.25 0.038 1.57 -2 4 4 61.60 33.20 3.23 0.031 2.22 -1 5 8 20.49 46.42 3.19 0.037 1.64 -9 0 17 15.81 43.91 3.16 0.036 0.99 -9 5 9 0.00 18.95 3.15 0.024 1.06 7 10 4 1.98 30.41 3.15 0.030 0.85 -1 2 13 111.76 171.45 3.14 0.071 1.58 -9 2 23 28.03 4.04 3.12 0.011 0.81 6 3 0 31.67 64.62 3.11 0.044 1.69 0 2 3 170.17 117.84 3.11 0.059 4.18 0 3 6 119.22 177.12 3.07 0.072 2.47 -3 1 1 971.23 1272.97 3.04 0.194 3.68 0 5 1 7.91 26.22 3.01 0.028 2.06 -11 0 13 23.80 57.86 3.00 0.041 0.97 -2 0 8 125.85 83.11 3.00 0.050 2.60 -10 3 10 36.02 68.66 2.99 0.045 1.05 -4 10 1 33.75 64.64 2.98 0.044 0.98 4 3 13 3.16 24.01 2.98 0.027 1.24 -4 5 1 134.94 193.40 2.93 0.076 1.69 -1 4 2 415.18 315.88 2.92 0.097 2.47 Bond lengths and angles C1 - Distance Angles O1 1.4349 (0.0037) H1A 0.9600 109.47 H1B 0.9600 109.47 109.47 H1C 0.9600 109.47 109.47 109.47 C1 - O1 H1A H1B C2 - Distance Angles O2 1.4152 (0.0039) H2A 0.9600 109.47 H2B 0.9600 109.47 109.47 H2C 0.9600 109.47 109.47 109.47 C2 - O2 H2A H2B C3 - Distance Angles O30 1.4464 (0.0031) C4 1.4770 (0.0048) 109.14 (0.26) H3A 0.9700 109.85 109.85 H3B 0.9700 109.85 109.85 108.28 C3 - O30 C4 H3A C4 - Distance Angles O4 1.4148 (0.0048) C3 1.4770 (0.0048) 108.62 (0.30) H4A 0.9700 109.97 109.97 H4B 0.9700 109.97 109.97 108.35 C4 - O4 C3 H4A C5 - Distance Angles O4 1.4082 (0.0044) C6 1.4798 (0.0077) 109.26 (0.42) H5A 0.9700 109.83 109.83 H5B 0.9700 109.82 109.82 108.26 C5 - O4 C6 H5A C6 - Distance Angles O5 1.3902 (0.0057) C5 1.4798 (0.0077) 109.87 (0.41) H6A 0.9700 109.69 109.69 H6B 0.9700 109.69 109.69 108.18 C6 - O5 C5 H6A C7 - Distance Angles O5 1.4093 (0.0058) C8 1.4626 (0.0075) 109.07 (0.40) H7A 0.9700 109.87 109.87 H7B 0.9700 109.87 109.87 108.29 C7 - O5 C8 H7A C8 - Distance Angles O6 1.4268 (0.0049) C7 1.4626 (0.0075) 115.46 (0.43) H8A 0.9700 108.41 108.41 H8B 0.9700 108.41 108.41 107.46 C8 - O6 C7 H8A C9 - Distance Angles O6 1.4279 (0.0044) C10 1.4373 (0.0051) 110.43 (0.32) H9A 0.9700 109.57 109.57 H9B 0.9700 109.57 109.57 108.11 C9 - O6 C10 H9A C10 - Distance Angles C9 1.4373 (0.0051) O7 1.4538 (0.0036) 112.85 (0.30) H10A 0.9700 109.02 109.02 H10B 0.9700 109.02 109.02 107.80 C10 - C9 O7 H10A C11 - Distance Angles C16 1.3789 (0.0038) C12 1.3919 (0.0040) 119.02 (0.26) P3 1.8102 (0.0025) 122.11 (0.22) 118.71 (0.21) C11 - C16 C12 C12 - Distance Angles C13 1.3824 (0.0045) C11 1.3919 (0.0040) 120.60 (0.33) H12 0.9300 119.70 119.70 C12 - C13 C11 C13 - Distance Angles C14 1.3687 (0.0057) C12 1.3824 (0.0045) 120.44 (0.36) H13 0.9300 119.78 119.78 C13 - C14 C12 C14 - Distance Angles C13 1.3687 (0.0057) C15 1.3649 (0.0056) 119.51 (0.32) H14 0.9300 120.24 120.24 C14 - C13 C15 C15 - Distance Angles C14 1.3649 (0.0056) C16 1.4040 (0.0045) 121.11 (0.32) H15 0.9300 119.44 119.44 C15 - C14 C16 C16 - Distance Angles C11 1.3789 (0.0038) C15 1.4040 (0.0045) 119.30 (0.31) H16 0.9300 120.35 120.35 C16 - C11 C15 C17 - Distance Angles C22 1.3869 (0.0036) C18 1.3849 (0.0036) 119.11 (0.25) P3 1.8004 (0.0025) 120.13 (0.20) 120.73 (0.20) C17 - C22 C18 C18 - Distance Angles C19 1.3795 (0.0042) C17 1.3849 (0.0036) 120.26 (0.29) H18 0.9300 119.87 119.87 C18 - C19 C17 C19 - Distance Angles C20 1.3620 (0.0052) C18 1.3795 (0.0042) 120.30 (0.32) H19 0.9300 119.85 119.85 C19 - C20 C18 C20 - Distance Angles C21 1.3644 (0.0051) C19 1.3620 (0.0052) 120.63 (0.29) H20 0.9300 119.69 119.69 C20 - C21 C19 C21 - Distance Angles C20 1.3644 (0.0051) C22 1.3954 (0.0043) 119.93 (0.31) H21 0.9300 120.03 120.03 C21 - C20 C22 C22 - Distance Angles C17 1.3869 (0.0036) C21 1.3954 (0.0043) 119.76 (0.29) H22 0.9300 120.12 120.12 C22 - C17 C21 N1 - Distance Angles P1 1.5835 (0.0021) P2 1.5859 (0.0021) 122.96 (0.13) N1 - P1 N2 - Distance Angles P2 1.5746 (0.0022) P3 1.6009 (0.0021) 121.30 (0.13) N2 - P2 N3 - Distance Angles P1 1.5736 (0.0020) P3 1.6027 (0.0019) 120.91 (0.12) N3 - P1 O1 - Distance Angles C1 1.4349 (0.0037) P1 1.5845 (0.0018) 118.82 (0.17) O1 - C1 O2 - Distance Angles C2 1.4152 (0.0039) P2 1.5745 (0.0019) 121.58 (0.20) O2 - C2 O4 - Distance Angles C4 1.4148 (0.0048) C5 1.4082 (0.0044) 112.89 (0.37) O4 - C4 O5 - Distance Angles C6 1.3902 (0.0057) C7 1.4093 (0.0058) 111.47 (0.43) O5 - C6 O6 - Distance Angles C9 1.4279 (0.0044) C8 1.4268 (0.0049) 114.06 (0.31) O6 - C9 O7 - Distance Angles C10 1.4538 (0.0036) P2 1.5852 (0.0019) 117.11 (0.19) O7 - C10 O30 - Distance Angles C3 1.4464 (0.0031) P1 1.5733 (0.0018) 119.92 (0.18) O30 - C3 P1 - Distance Angles O30 1.5733 (0.0018) N3 1.5736 (0.0020) 106.50 (0.10) N1 1.5835 (0.0021) 112.39 (0.11) 117.06 (0.11) O1 1.5845 (0.0018) 99.50 (0.10) 111.66 (0.11) 108.35 (0.11) P1 - O30 N3 N1 P2 - Distance Angles N2 1.5746 (0.0022) O2 1.5745 (0.0019) 111.65 (0.12) O7 1.5852 (0.0019) 107.88 (0.11) 98.83 (0.11) N1 1.5859 (0.0021) 116.77 (0.11) 109.07 (0.11) 111.18 (0.12) P2 - N2 O2 O7 P3 - Distance Angles N3 1.6027 (0.0019) N2 1.6009 (0.0021) 117.33 (0.11) C17 1.8004 (0.0025) 107.74 (0.11) 109.39 (0.12) C11 1.8102 (0.0026) 107.10 (0.11) 109.37 (0.12) 105.23 (0.11) P3 - N3 N2 C17 Selected torsion angles 72.95 ( 0.36) O30 - C3 - C4 - O4 60.20 ( 0.50) O4 - C5 - C6 - O5 -73.13 ( 0.53) O5 - C7 - C8 - O6 71.94 ( 0.41) O6 - C9 - C10 - O7 -0.94 ( 0.48) C16 - C11 - C12 - C13 174.62 ( 0.29) P3 - C11 - C12 - C13 -0.08 ( 0.58) C11 - C12 - C13 - C14 0.49 ( 0.60) C12 - C13 - C14 - C15 0.12 ( 0.56) C13 - C14 - C15 - C16 1.52 ( 0.42) C12 - C11 - C16 - C15 -173.88 ( 0.23) P3 - C11 - C16 - C15 -1.14 ( 0.48) C14 - C15 - C16 - C11 -0.19 ( 0.42) C22 - C17 - C18 - C19 178.04 ( 0.23) P3 - C17 - C18 - C19 -0.25 ( 0.48) C17 - C18 - C19 - C20 0.15 ( 0.53) C18 - C19 - C20 - C21 0.38 ( 0.53) C19 - C20 - C21 - C22 0.71 ( 0.42) C18 - C17 - C22 - C21 -177.53 ( 0.24) P3 - C17 - C22 - C21 -0.81 ( 0.49) C20 - C21 - C22 - C17 165.75 ( 0.32) C3 - C4 - O4 - C5 178.00 ( 0.36) C6 - C5 - O4 - C4 -165.86 ( 0.36) C5 - C6 - O5 - C7 164.03 ( 0.37) C8 - C7 - O5 - C6 163.13 ( 0.41) C10 - C9 - O6 - C8 77.52 ( 0.58) C7 - C8 - O6 - C9 130.97 ( 0.28) C9 - C10 - O7 - P2 -164.87 ( 0.24) C4 - C3 - O30 - P1 179.63 ( 0.20) C3 - O30 - P1 - N3 50.19 ( 0.23) C3 - O30 - P1 - N1 -64.27 ( 0.22) C3 - O30 - P1 - O1 -133.20 ( 0.14) P3 - N3 - P1 - O30 -6.52 ( 0.20) P3 - N3 - P1 - N1 119.16 ( 0.15) P3 - N3 - P1 - O1 112.50 ( 0.17) P2 - N1 - P1 - O30 -11.24 ( 0.22) P2 - N1 - P1 - N3 -138.55 ( 0.16) P2 - N1 - P1 - O1 177.29 ( 0.22) C1 - O1 - P1 - O30 -70.60 ( 0.24) C1 - O1 - P1 - N3 59.75 ( 0.24) C1 - O1 - P1 - N1 -128.62 ( 0.15) P3 - N2 - P2 - O2 123.82 ( 0.16) P3 - N2 - P2 - O7 -2.19 ( 0.22) P3 - N2 - P2 - N1 82.13 ( 0.30) C2 - O2 - P2 - N2 -164.54 ( 0.28) C2 - O2 - P2 - O7 -48.40 ( 0.31) C2 - O2 - P2 - N1 176.20 ( 0.22) C10 - O7 - P2 - N2 59.94 ( 0.24) C10 - O7 - P2 - O2 -54.56 ( 0.25) C10 - O7 - P2 - N1 15.54 ( 0.23) P1 - N1 - P2 - N2 143.24 ( 0.17) P1 - N1 - P2 - O2 -108.81 ( 0.17) P1 - N1 - P2 - O7 18.81 ( 0.20) P1 - N3 - P3 - N2 142.71 ( 0.15) P1 - N3 - P3 - C17 -104.52 ( 0.16) P1 - N3 - P3 - C11 -14.26 ( 0.21) P2 - N2 - P3 - N3 -137.33 ( 0.15) P2 - N2 - P3 - C17 107.91 ( 0.16) P2 - N2 - P3 - C11 -160.96 ( 0.21) C22 - C17 - P3 - N3 20.83 ( 0.24) C18 - C17 - P3 - N3 -32.37 ( 0.25) C22 - C17 - P3 - N2 149.41 ( 0.21) C18 - C17 - P3 - N2 85.03 ( 0.23) C22 - C17 - P3 - C11 -93.19 ( 0.23) C18 - C17 - P3 - C11 127.71 ( 0.22) C16 - C11 - P3 - N3 -47.71 ( 0.25) C12 - C11 - P3 - N3 -0.41 ( 0.25) C16 - C11 - P3 - N2 -175.82 ( 0.23) C12 - C11 - P3 - N2 -117.82 ( 0.23) C16 - C11 - P3 - C17 66.76 ( 0.25) C12 - C11 - P3 - C17 FMAP and GRID set by program FMAP 2 3 27 GRID -1.042 -2 -2 1.042 2 2 R1 = 0.0790 for 5841 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.46 at 0.9579 0.8123 0.1060 [ 1.05 A from C9 ] Deepest hole -0.31 at 0.3392 0.1370 0.0216 [ 0.75 A from P2 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 4207 / 26178 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0421 1.1877 -0.1060 1.00000 0.05 0.46 1.05 C9 1.18 O6 1.37 H10A 1.41 C10 Q2 1 -0.1028 1.3868 0.1211 1.00000 0.05 0.39 1.11 O4 1.22 H4B 1.30 C4 1.50 H5A Q3 1 0.0702 1.1779 -0.0247 1.00000 0.05 0.39 1.03 C10 1.06 C9 1.08 H9B 1.38 H10B Q4 1 0.2830 0.8703 0.0083 1.00000 0.05 0.29 0.80 H2C 1.09 C2 1.44 O2 1.64 H2B Q5 1 0.3785 0.9927 0.0353 1.00000 0.05 0.25 0.90 O2 1.07 C2 1.20 H2A 1.67 H2B Q6 1 0.1947 1.1082 0.0818 1.00000 0.05 0.24 0.33 N1 1.56 P1 1.61 P2 2.43 O30 Q7 1 0.3996 1.2192 0.0460 1.00000 0.05 0.24 0.32 N2 1.64 P2 1.87 P3 2.46 O7 Q8 1 0.2560 1.1077 -0.0259 1.00000 0.05 0.22 1.05 O7 1.33 P2 1.42 O2 1.73 C10 Q9 1 0.6244 1.1596 0.1123 1.00000 0.05 0.20 1.04 H16 1.07 C16 1.73 C11 2.14 C15 Q10 1 0.3455 1.2775 0.2464 1.00000 0.05 0.19 1.61 N3 2.01 H1B 2.32 H12 2.37 H18 Shortest distances between peaks (including symmetry equivalents) 4 5 1.73 1 3 1.73 5 8 2.14 3 8 2.32 5 7 2.36 7 8 2.39 6 8 2.56 4 8 2.57 3 6 2.61 5 6 2.82 7 9 2.86 6 7 2.91 1 8 2.92 Time profile in seconds ----------------------- 0.11: 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. 0.39: 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 2.38: Structure factors and derivatives 3.86: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.20: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.27: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.11: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 10:05:22 Total elapsed time: 7.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++