+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007jmw0007 started at 10:13:30 on 28-Feb-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007jmw0007 in P-1 CELL 0.71073 7.8170 9.2412 10.0613 85.450 67.970 79.532 ZERR 2.00 0.0003 0.0002 0.0003 0.002 0.002 0.002 LATT 1 SFAC C H B O S UNIT 24 34 2 8 2 V = 662.48 F(000) = 284.0 Mu = 0.25 mm-1 Cell Wt = 536.25 Rho = 1.344 MERG 2 OMIT -3.00 55.00 FMAP 2 PLAN 5 ACTA SIZE 0.16 0.08 0.02 BOND $H L.S. 6 TEMP -153.00 WGHT 0.0178 0.9666 EXTI 0.009410 FVAR 1.48588 C1 1 0.351922 0.842815 0.223065 11.00000 0.01717 0.01520 = 0.01988 -0.00160 -0.00719 -0.00255 C2 1 0.473386 0.794550 0.292228 11.00000 0.01383 0.01660 = 0.01526 -0.00125 -0.00402 -0.00225 C3 1 0.671159 0.815763 0.413378 11.00000 0.02520 0.01986 = 0.02939 -0.00222 -0.01714 -0.00061 AFIX 23 H3A 2 0.673389 0.868205 0.494630 11.00000 -1.20000 H3B 2 0.786389 0.826030 0.329554 11.00000 -1.20000 AFIX 0 C4 1 0.667112 0.654990 0.452124 11.00000 0.02761 0.02276 = 0.02532 -0.00193 -0.01706 0.00033 AFIX 23 H4A 2 0.774520 0.614118 0.480804 11.00000 -1.20000 H4B 2 0.550749 0.644732 0.534860 11.00000 -1.20000 AFIX 0 C5 1 0.552721 0.642996 0.271781 11.00000 0.01591 0.01607 = 0.01920 0.00115 -0.00726 -0.00178 C6 1 0.494293 0.576017 0.184198 11.00000 0.02505 0.01495 = 0.02817 -0.00326 -0.01442 0.00172 AFIX 43 H6 2 0.534006 0.475673 0.157124 11.00000 -1.20000 AFIX 0 C7 1 0.006446 1.156972 0.168527 11.00000 0.02136 0.01475 = 0.01984 0.00075 -0.01142 -0.00060 C8 1 0.069525 1.224433 0.277148 11.00000 0.01575 0.01391 = 0.02014 -0.00025 -0.00859 -0.00035 C9 1 -0.204085 1.175343 0.208768 11.00000 0.02204 0.02022 = 0.03637 -0.00198 -0.01739 -0.00036 AFIX 137 H9A 2 -0.231152 1.129322 0.135975 11.00000 -1.50000 H9B 2 -0.256681 1.280355 0.214109 11.00000 -1.50000 H9C 2 -0.260152 1.128194 0.302163 11.00000 -1.50000 AFIX 0 C10 1 0.100755 1.207400 0.013541 11.00000 0.03101 0.02560 = 0.02060 0.00197 -0.01157 -0.00505 AFIX 137 H10A 2 0.236233 1.194768 -0.010732 11.00000 -1.50000 H10B 2 0.052214 1.311405 0.003025 11.00000 -1.50000 H10C 2 0.074243 1.148339 -0.050973 11.00000 -1.50000 AFIX 0 C11 1 -0.070937 1.224577 0.429893 11.00000 0.02519 0.02279 = 0.02016 -0.00234 -0.00992 -0.00209 AFIX 137 H11A 2 -0.106300 1.126696 0.454848 11.00000 -1.50000 H11B 2 -0.182432 1.297320 0.438061 11.00000 -1.50000 H11C 2 -0.014818 1.249808 0.495444 11.00000 -1.50000 AFIX 0 C12 1 0.124769 1.375438 0.234119 11.00000 0.02352 0.01699 = 0.02497 0.00102 -0.00974 -0.00465 AFIX 137 H12A 2 0.158796 1.411264 0.308463 11.00000 -1.50000 H12B 2 0.019208 1.443817 0.223119 11.00000 -1.50000 H12C 2 0.231968 1.368725 0.142996 11.00000 -1.50000 AFIX 0 B1 3 0.223720 0.990446 0.223922 11.00000 0.01496 0.01839 = 0.01449 0.00166 -0.00403 -0.00350 O1 4 0.509153 0.881425 0.379839 11.00000 0.02353 0.01557 = 0.02598 -0.00472 -0.01511 0.00198 O2 4 0.675814 0.572789 0.332731 11.00000 0.02510 0.01507 = 0.02736 -0.00210 -0.01618 0.00292 O3 4 0.080516 1.000659 0.174698 11.00000 0.02072 0.01339 = 0.02572 -0.00140 -0.01309 0.00073 O4 4 0.236403 1.119658 0.274796 11.00000 0.01772 0.01628 = 0.02328 -0.00175 -0.01146 0.00123 S1 5 0.339638 0.697485 0.129746 11.00000 0.02585 0.01720 = 0.02684 -0.00343 -0.01645 0.00017 HKLF 4 Covalent radii and connectivity table for 2007jmw0007 in P-1 C 0.770 H 0.320 B 0.820 O 0.660 S 1.030 C1 - C2 B1 S1 C2 - C1 O1 C5 C3 - O1 C4 C4 - O2 C3 C5 - C6 O2 C2 C6 - C5 S1 C7 - O3 C9 C10 C8 C8 - O4 C11 C12 C7 C9 - C7 C10 - C7 C11 - C8 C12 - C8 B1 - O4 O3 C1 O1 - C2 C3 O2 - C5 C4 O3 - B1 C7 O4 - B1 C8 S1 - C6 C1 10247 Reflections read, of which 12 rejected -10 =< h =< 10, -11 =< k =< 12, -12 =< l =< 13, Max. 2-theta = 54.99 0 Systematic absence violations 0 Inconsistent equivalents 3010 Unique reflections, of which 0 suppressed R(int) = 0.0567 R(sigma) = 0.0528 Friedel opposites merged Maximum memory for data reduction = 1861 / 30574 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 = 2347 / 210245 wR2 = 0.1162 before cycle 1 for 3010 data and 168 / 168 parameters GooF = S = 1.060; Restrained GooF = 1.060 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0178 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.49318 0.00406 1.798 OSF 2 0.01414 0.00446 1.061 EXTI Mean shift/esd = 0.227 Maximum = 1.798 for OSF Max. shift = 0.008 A for H9C Max. dU = 0.000 for B1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2347 / 210245 wR2 = 0.1158 before cycle 2 for 3010 data and 168 / 168 parameters GooF = S = 1.056; Restrained GooF = 1.056 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0178 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.49517 0.00408 0.488 OSF 2 0.01584 0.00460 0.368 EXTI Mean shift/esd = 0.082 Maximum = 0.488 for OSF Max. shift = 0.003 A for H9C Max. dU = 0.000 for B1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2347 / 210245 wR2 = 0.1158 before cycle 3 for 3010 data and 168 / 168 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0178 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.49525 0.00410 0.020 OSF 2 0.01584 0.00465 0.001 EXTI Mean shift/esd = 0.004 Maximum = 0.020 for U33 C7 Max. shift = 0.000 A for H12C Max. dU = 0.000 for C7 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2347 / 210245 wR2 = 0.1158 before cycle 4 for 3010 data and 168 / 168 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0178 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.49526 0.00410 0.002 OSF 2 0.01585 0.00465 0.001 EXTI Mean shift/esd = 0.001 Maximum = -0.003 for U13 O4 Max. shift = 0.000 A for H9B Max. dU = 0.000 for C3 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2347 / 210245 wR2 = 0.1158 before cycle 5 for 3010 data and 168 / 168 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0178 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.49526 0.00410 0.000 OSF 2 0.01584 0.00465 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y S1 Max. shift = 0.000 A for H12B Max. dU = 0.000 for C8 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2347 / 210245 wR2 = 0.1158 before cycle 6 for 3010 data and 168 / 168 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0178 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.49526 0.00410 0.000 OSF 2 0.01584 0.00465 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y S1 Max. shift = 0.000 A for H10A Max. dU = 0.000 for C4 Largest correlation matrix elements 0.650 EXTI / OSF -0.573 U13 O2 / U33 O2 -0.548 U13 O3 / U33 O3 -0.616 U13 S1 / U11 S1 -0.573 U13 C3 / U11 C3 -0.545 U13 C7 / U33 C7 -0.601 U13 S1 / U33 S1 -0.572 U13 O2 / U11 O2 -0.542 U13 O4 / U11 O4 -0.584 U13 C9 / U33 C9 -0.569 U13 O1 / U33 O1 -0.542 U13 C7 / U11 C7 -0.582 U13 C9 / U11 C9 -0.561 U13 C6 / U11 C6 -0.540 U13 O4 / U33 O4 -0.581 U13 C4 / U33 C4 -0.555 U13 O1 / U11 O1 -0.532 U13 C10 / U11 C10 -0.580 U13 C4 / U11 C4 -0.553 U13 C6 / U33 C6 -0.531 U13 C8 / U11 C8 -0.574 U13 C3 / U33 C3 -0.548 U13 O3 / U11 O3 -0.526 z C3 / x C3 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3A 0.6731 0.8681 0.4949 23 0.990 0.000 C3 O1 C4 H3B 0.7864 0.8261 0.3298 23 0.990 0.000 C3 O1 C4 H4A 0.7745 0.6143 0.4808 23 0.990 0.000 C4 O2 C3 H4B 0.5508 0.6449 0.5348 23 0.990 0.000 C4 O2 C3 H6 0.5341 0.4757 0.1573 43 0.950 0.000 C6 C5 S1 H9A -0.2311 1.1302 0.1354 137 0.980 0.000 C9 C7 H9A H9B -0.2569 1.2802 0.2153 137 0.980 0.000 C9 C7 H9A H9C -0.2597 1.1271 0.3016 137 0.980 0.000 C9 C7 H9A H10A 0.2364 1.1945 -0.0105 137 0.980 0.000 C10 C7 H10A H10B 0.0527 1.3115 0.0032 137 0.980 0.000 C10 C7 H10A H10C 0.0741 1.1486 -0.0508 137 0.980 0.000 C10 C7 H10A H11A -0.1063 1.1268 0.4548 137 0.980 0.000 C11 C8 H11A H11B -0.1824 1.2974 0.4382 137 0.980 0.000 C11 C8 H11A H11C -0.0146 1.2498 0.4953 137 0.980 0.000 C11 C8 H11A H12A 0.1592 1.4110 0.3082 137 0.980 0.000 C12 C8 H12A H12B 0.0191 1.4439 0.2233 137 0.980 0.000 C12 C8 H12A H12C 0.2317 1.3686 0.1428 137 0.980 0.000 C12 C8 H12A 2007jmw0007 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.35188 0.84280 0.22317 1.00000 0.01735 0.01587 0.01937 -0.00126 -0.00671 -0.00309 0.01744 0.00290 0.00030 0.00022 0.00023 0.00000 0.00103 0.00096 0.00109 0.00077 0.00087 0.00079 0.00043 C2 0.47338 0.79449 0.29228 1.00000 0.01398 0.01715 0.01526 -0.00127 -0.00380 -0.00274 0.01584 0.00287 0.00028 0.00022 0.00022 0.00000 0.00097 0.00096 0.00103 0.00075 0.00081 0.00076 0.00042 C3 0.67111 0.81571 0.41352 1.00000 0.02438 0.02067 0.02953 -0.00251 -0.01697 -0.00042 0.02310 0.00310 0.00033 0.00023 0.00026 0.00000 0.00118 0.00106 0.00128 0.00088 0.00102 0.00088 0.00049 H3A 0.67312 0.86812 0.49488 1.00000 0.02772 0.00000 0.00000 H3B 0.78641 0.82607 0.32980 1.00000 0.02772 0.00000 0.00000 C4 0.66711 0.65518 0.45207 1.00000 0.02732 0.02349 0.02513 -0.00239 -0.01655 0.00053 0.02379 0.00314 0.00034 0.00024 0.00026 0.00000 0.00122 0.00111 0.00123 0.00088 0.00103 0.00091 0.00050 H4A 0.77450 0.61433 0.48077 1.00000 0.02854 0.00000 0.00000 H4B 0.55076 0.64491 0.53480 1.00000 0.02854 0.00000 0.00000 C5 0.55263 0.64311 0.27167 1.00000 0.01625 0.01667 0.01902 0.00128 -0.00730 -0.00174 0.01729 0.00298 0.00029 0.00022 0.00023 0.00000 0.00102 0.00096 0.00109 0.00076 0.00086 0.00078 0.00043 C6 0.49437 0.57602 0.18430 1.00000 0.02459 0.01515 0.02886 -0.00323 -0.01444 0.00201 0.02204 0.00310 0.00032 0.00023 0.00025 0.00000 0.00118 0.00098 0.00126 0.00084 0.00101 0.00084 0.00048 H6 0.53411 0.47565 0.15732 1.00000 0.02645 0.00000 0.00000 C7 0.00647 1.15708 0.16839 1.00000 0.02159 0.01454 0.02088 0.00044 -0.01169 -0.00046 0.01824 0.00294 0.00031 0.00022 0.00023 0.00000 0.00109 0.00095 0.00113 0.00078 0.00092 0.00080 0.00044 C8 0.06932 1.22449 0.27715 1.00000 0.01580 0.01438 0.02048 -0.00045 -0.00842 -0.00011 0.01668 0.00292 0.00029 0.00021 0.00023 0.00000 0.00101 0.00092 0.00110 0.00075 0.00086 0.00076 0.00043 C9 -0.20397 1.17527 0.20877 1.00000 0.02259 0.02024 0.03641 -0.00169 -0.01775 -0.00027 0.02474 0.00321 0.00032 0.00024 0.00027 0.00000 0.00118 0.00106 0.00140 0.00092 0.00108 0.00087 0.00051 H9A -0.23105 1.13021 0.13544 1.00000 0.03711 0.00000 0.00000 H9B -0.25689 1.28024 0.21525 1.00000 0.03711 0.00000 0.00000 H9C -0.25970 1.12708 0.30164 1.00000 0.03711 0.00000 0.00000 C10 0.10086 1.20740 0.01372 1.00000 0.03122 0.02570 0.02126 0.00178 -0.01198 -0.00496 0.02545 0.00338 0.00035 0.00025 0.00025 0.00000 0.00130 0.00114 0.00120 0.00089 0.00103 0.00096 0.00050 H10A 0.23635 1.19445 -0.01050 1.00000 0.03818 0.00000 0.00000 H10B 0.05267 1.31149 0.00324 1.00000 0.03818 0.00000 0.00000 H10C 0.07415 1.14855 -0.05084 1.00000 0.03818 0.00000 0.00000 C11 -0.07087 1.22461 0.42988 1.00000 0.02516 0.02306 0.02019 -0.00228 -0.00986 -0.00211 0.02249 0.00317 0.00033 0.00024 0.00024 0.00000 0.00118 0.00108 0.00115 0.00084 0.00096 0.00088 0.00047 H11A -0.10629 1.12675 0.45484 1.00000 0.03374 0.00000 0.00000 H11B -0.18236 1.29741 0.43817 1.00000 0.03374 0.00000 0.00000 H11C -0.01457 1.24976 0.49535 1.00000 0.03374 0.00000 0.00000 C12 0.12474 1.37536 0.23405 1.00000 0.02397 0.01737 0.02496 0.00088 -0.01013 -0.00447 0.02169 0.00312 0.00032 0.00023 0.00025 0.00000 0.00116 0.00100 0.00121 0.00082 0.00097 0.00084 0.00047 H12A 0.15922 1.41104 0.30822 1.00000 0.03254 0.00000 0.00000 H12B 0.01912 1.44389 0.22333 1.00000 0.03254 0.00000 0.00000 H12C 0.23169 1.36861 0.14277 1.00000 0.03254 0.00000 0.00000 B1 0.22367 0.99042 0.22384 1.00000 0.01576 0.01904 0.01453 0.00209 -0.00402 -0.00426 0.01685 0.00340 0.00033 0.00025 0.00025 0.00000 0.00114 0.00109 0.00116 0.00085 0.00093 0.00089 0.00047 O1 0.50914 0.88132 0.37982 1.00000 0.02319 0.01592 0.02610 -0.00484 -0.01500 0.00187 0.02041 0.00206 0.00022 0.00016 0.00017 0.00000 0.00081 0.00070 0.00086 0.00058 0.00069 0.00059 0.00035 O2 0.67585 0.57279 0.33276 1.00000 0.02494 0.01559 0.02777 -0.00238 -0.01629 0.00308 0.02156 0.00212 0.00022 0.00016 0.00017 0.00000 0.00084 0.00071 0.00089 0.00059 0.00072 0.00060 0.00036 O3 0.08059 1.00060 0.17472 1.00000 0.02126 0.01344 0.02583 -0.00146 -0.01314 0.00074 0.01927 0.00204 0.00021 0.00015 0.00017 0.00000 0.00080 0.00069 0.00085 0.00057 0.00068 0.00057 0.00034 O4 0.23630 1.11965 0.27477 1.00000 0.01767 0.01668 0.02344 -0.00176 -0.01138 0.00112 0.01858 0.00204 0.00021 0.00015 0.00016 0.00000 0.00076 0.00071 0.00083 0.00058 0.00065 0.00057 0.00034 S1 0.33962 0.69748 0.12975 1.00000 0.02622 0.01760 0.02714 -0.00347 -0.01659 0.00018 0.02198 0.00075 0.00008 0.00006 0.00006 0.00000 0.00032 0.00027 0.00033 0.00020 0.00025 0.00021 0.00018 Final Structure Factor Calculation for 2007jmw0007 in P-1 Total number of l.s. parameters = 168 Maximum vector length = 511 Memory required = 2179 / 24017 wR2 = 0.1158 before cycle 7 for 3010 data and 0 / 168 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0178 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0509 for 2537 Fo > 4sig(Fo) and 0.0651 for all 3010 data wR2 = 0.1158, GooF = S = 1.055, Restrained GooF = 1.055 for all data Occupancy sum of asymmetric unit = 18.00 for non-hydrogen and 17.00 for hydrogen atoms Principal mean square atomic displacements U 0.0198 0.0174 0.0152 C1 0.0181 0.0161 0.0133 C2 0.0338 0.0202 0.0153 C3 0.0340 0.0222 0.0152 C4 0.0199 0.0175 0.0145 C5 0.0324 0.0203 0.0135 C6 0.0245 0.0174 0.0128 C7 0.0207 0.0169 0.0124 C8 0.0378 0.0211 0.0152 C9 0.0312 0.0261 0.0190 C10 0.0268 0.0225 0.0182 C11 0.0255 0.0226 0.0170 C12 0.0201 0.0176 0.0128 B1 0.0320 0.0152 0.0140 O1 0.0335 0.0190 0.0122 O2 0.0281 0.0175 0.0123 O3 0.0255 0.0179 0.0123 O4 0.0334 0.0167 0.0158 S1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.021 0.038 0.057 0.080 0.101 0.127 0.158 0.199 0.278 1.000 Number in group 306. 308. 300. 306. 294. 291. 306. 295. 301. 303. GooF 1.135 1.103 1.090 0.997 1.088 1.078 1.060 0.932 1.023 1.026 K 2.806 1.171 1.069 1.014 1.007 0.989 1.011 1.009 1.000 1.010 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.65 inf Number in group 302. 304. 298. 304. 307. 292. 301. 300. 303. 299. GooF 1.061 1.134 1.012 1.092 0.947 1.067 0.982 1.027 1.052 1.157 K 1.067 1.062 1.046 1.010 1.020 0.997 0.983 0.993 1.016 1.008 R1 0.119 0.130 0.106 0.097 0.075 0.065 0.049 0.041 0.042 0.031 Recommended weighting scheme: WGHT 0.0065 0.9762 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) 0 1 1 173.19 354.05 6.40 0.274 6.55 -6 -2 2 209.14 351.11 5.51 0.273 1.07 7 1 1 27.86 69.49 3.99 0.121 1.07 2 -7 9 36.40 87.63 3.95 0.136 0.82 -6 0 3 34.58 75.51 3.80 0.127 1.00 1 -1 12 200.72 114.01 3.73 0.155 0.80 -7 -2 3 42.89 77.09 3.46 0.128 0.89 0 6 4 20.57 42.52 3.42 0.095 1.28 7 1 10 20.65 45.85 3.40 0.099 0.87 -4 8 4 0.78 12.51 3.39 0.051 0.79 1 2 11 -0.11 18.13 3.17 0.062 0.87 7 2 0 36.19 70.54 3.09 0.122 1.03 7 8 0 34.77 7.54 3.05 0.040 0.83 0 0 4 65.92 41.59 3.05 0.094 2.33 3 -2 12 23.76 3.42 3.03 0.027 0.81 0 -5 8 106.57 149.47 3.01 0.178 0.98 -2 -3 9 23.00 55.86 3.01 0.109 0.88 4 0 1 493.23 593.35 2.97 0.355 1.89 1 2 2 -0.61 7.46 2.97 0.040 3.52 -7 -2 1 119.02 168.22 2.95 0.189 0.99 6 4 1 -0.66 9.91 2.91 0.046 1.18 3 -1 3 926.99 808.93 2.90 0.414 2.19 -1 1 10 3.40 23.46 2.87 0.071 0.88 3 0 6 7.43 0.03 2.86 0.002 1.60 -3 9 2 38.98 8.07 2.84 0.041 0.84 -8 -2 3 28.77 3.82 2.83 0.028 0.79 6 1 10 116.23 157.90 2.83 0.183 0.92 2 -2 12 65.00 34.22 2.81 0.085 0.80 7 2 10 98.38 65.61 2.79 0.118 0.87 5 -2 12 -4.10 7.01 2.75 0.039 0.79 7 3 12 20.34 0.25 2.74 0.007 0.77 7 -6 2 27.43 11.74 2.72 0.050 0.82 7 4 8 62.03 38.76 2.72 0.091 0.95 -6 -4 2 127.62 86.62 2.71 0.136 1.02 -1 0 3 1286.02 1116.84 2.70 0.487 2.53 5 -5 10 46.26 23.91 2.68 0.071 0.81 7 3 1 117.27 169.21 2.67 0.189 1.06 -6 -3 6 138.80 81.81 2.67 0.132 0.81 5 9 1 30.41 14.36 2.67 0.055 0.91 -1 -4 9 30.42 57.53 2.66 0.110 0.90 1 -2 9 38.58 17.10 2.63 0.060 1.05 3 -6 10 47.00 22.31 2.60 0.069 0.81 -5 -5 3 10.60 0.04 2.60 0.003 1.03 -3 7 0 165.37 212.39 2.57 0.212 1.07 2 -3 1 1446.37 1294.45 2.55 0.524 2.19 -4 9 1 -1.31 6.35 2.55 0.037 0.81 2 0 11 232.15 318.20 2.53 0.260 0.90 5 -1 2 990.90 874.64 2.52 0.431 1.47 -1 -6 9 107.62 69.65 2.50 0.122 0.82 3 -6 3 212.23 257.31 2.50 0.234 1.18 Bond lengths and angles C1 - Distance Angles C2 1.3700 (0.0028) B1 1.5379 (0.0030) 132.50 (0.19) S1 1.7351 (0.0020) 108.89 (0.15) 118.44 (0.15) C1 - C2 B1 C2 - Distance Angles C1 1.3700 (0.0028) O1 1.3697 (0.0024) 123.48 (0.18) C5 1.4207 (0.0028) 114.10 (0.18) 122.33 (0.18) C2 - C1 O1 C3 - Distance Angles O1 1.4478 (0.0024) C4 1.5062 (0.0030) 110.82 (0.18) H3A 0.9900 109.48 109.48 H3B 0.9900 109.48 109.48 108.06 C3 - O1 C4 H3A C4 - Distance Angles O2 1.4456 (0.0026) C3 1.5062 (0.0030) 111.26 (0.18) H4A 0.9900 109.38 109.38 H4B 0.9900 109.38 109.38 108.00 C4 - O2 C3 H4A C5 - Distance Angles C6 1.3617 (0.0029) O2 1.3715 (0.0024) 123.78 (0.19) C2 1.4207 (0.0028) 112.89 (0.18) 123.33 (0.18) C5 - C6 O2 C6 - Distance Angles C5 1.3617 (0.0030) S1 1.7121 (0.0021) 110.65 (0.16) H6 0.9500 124.67 124.67 C6 - C5 S1 C7 - Distance Angles O3 1.4627 (0.0023) C9 1.5194 (0.0031) 108.82 (0.17) C10 1.5267 (0.0032) 106.35 (0.17) 110.63 (0.18) C8 1.5651 (0.0028) 102.18 (0.15) 114.76 (0.18) 113.33 (0.18) C7 - O3 C9 C10 C8 - Distance Angles O4 1.4710 (0.0024) C11 1.5162 (0.0031) 106.44 (0.16) C12 1.5173 (0.0028) 108.44 (0.17) 110.86 (0.18) C7 1.5651 (0.0028) 103.03 (0.15) 113.06 (0.18) 114.32 (0.17) C8 - O4 C11 C12 C9 - Distance Angles C7 1.5194 (0.0031) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - C7 H9A H9B C10 - Distance Angles C7 1.5267 (0.0032) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - C7 H10A H10B C11 - Distance Angles C8 1.5162 (0.0031) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - C8 H11A H11B C12 - Distance Angles C8 1.5173 (0.0028) H12A 0.9800 109.47 H12B 0.9800 109.47 109.47 H12C 0.9800 109.47 109.47 109.47 C12 - C8 H12A H12B B1 - Distance Angles O4 1.3698 (0.0027) O3 1.3686 (0.0027) 114.21 (0.18) C1 1.5379 (0.0030) 124.87 (0.19) 120.90 (0.19) B1 - O4 O3 O1 - Distance Angles C2 1.3697 (0.0024) C3 1.4478 (0.0024) 112.31 (0.15) O1 - C2 O2 - Distance Angles C5 1.3715 (0.0024) C4 1.4456 (0.0026) 111.03 (0.16) O2 - C5 O3 - Distance Angles B1 1.3686 (0.0027) C7 1.4627 (0.0023) 107.10 (0.15) O3 - B1 O4 - Distance Angles B1 1.3698 (0.0027) C8 1.4710 (0.0024) 106.32 (0.16) O4 - B1 S1 - Distance Angles C6 1.7121 (0.0021) C1 1.7351 (0.0020) 93.45 (0.10) S1 - C6 FMAP and GRID set by program FMAP 2 1 22 GRID -2.632 -2 -2 2.632 2 2 R1 = 0.0645 for 3010 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.33 at 0.2859 0.9113 0.2349 [ 0.73 A from C1 ] Deepest hole -0.29 at 0.4000 0.5235 0.7397 [ 1.32 A from H6 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2233 / 19268 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2859 0.9113 0.2349 1.00000 0.05 0.33 0.73 C1 0.83 B1 1.90 C2 1.94 O4 Q2 1 0.5181 0.7199 0.2786 1.00000 0.05 0.32 0.71 C5 0.71 C2 1.77 C6 1.79 C1 Q3 1 0.0413 1.2002 0.2133 1.00000 0.05 0.30 0.77 C7 0.81 C8 1.86 O3 1.87 O4 Q4 1 0.4749 0.5943 0.2852 1.00000 0.05 0.29 0.79 C5 0.99 C6 1.63 H6 1.78 O2 Q5 1 0.0494 1.0807 0.1685 1.00000 0.05 0.29 0.72 C7 0.74 O3 1.72 B1 1.84 C10 Shortest distances between peaks (including symmetry equivalents) 3 5 1.21 2 4 1.26 1 2 2.43 1 5 2.45 Time profile in seconds ----------------------- 0.05: 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. 0.38: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.52: Structure factors and derivatives 0.89: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.13: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007jmw0007 finished at 10:13:32 Total CPU time: 2.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++