++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXTL XLMP CRYSTAL STRUCTURE REFINEMENT - MULTI-CPU VERSION + + Copyright(c) Bruker AXS Inc. 1993-2018 Version 2018/3 + + marc004a started at 10:39:20 on 13-Jan-2020 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Command line parameters: marc004a -a50000 -b3000 -c624 -g0 -m0 -t4 -a sets the approximate maximum number of atoms including hydrogens. -b sets the maximum number of full-matrix parameters (not used by CGLS). For example -b9000 allows refinement of 1000 anisotropic atoms or 3000 with BLOC 1. For a 32-bit version, -b times the square root of the number of threads should not exceed about 65500. -c sets the reflection buffer size. This depends on the CPU cache size but will rarely need changing. -g sets the number of reflection groups used for calculating R_complete, This must be greater than 1 but not greater than the total number of reflections for refinement. -m sets the current reflection group number. This may not be less than 1 nor greater than the number set by -g. These command line flags override other ways of defining free-R reflections. The -m value is also used as a seed for the WIGL pseudo-random shifts. -t sets the number of threads, otherwise it is set to the apparent number of CPUs. For optimal performance on hyperthreading systems, -t should be set to a little more than half the number of CPUs; e.g. -t4 or -t5 for an Intel i7 processor. Running 4 threads on 4 processors TITL marc004a in C2/c marc004a.res created by SHELXL-2018/3 at 10:37:55 on 13-Jan-2020 CELL 1.54178 19.9030 11.3141 22.0976 90.000 90.020 90.000 ZERR 8.000 0.0008 0.0005 0.0009 0.000 0.002 0.000 LATT 7 SYMM -X, Y, 1/2-Z SFAC C H O UNIT 280 208 40 V = 4976.04 F(000) = 2208.0 Mu = 0.75 mm-1 Cell Wt = 4212.45 Rho = 1.406 TEMP -173.160 SIZE 0.18 0.184 0.195 L.S. 20 BOND $H LIST 4 FMAP 2 ACTA OMIT -1 3 27 OMIT -4 0 4 OMIT 0 0 2 CONF EADP_TOLU C1A C1B EADP_TOLU C2A C2B EADP_TOLU C3A C3B EADP_TOLU C4A C4B EADP_TOLU C5A C5B EADP_TOLU C6A C6B EADP_TOLU C7A C7B PLAN 5 EQIV $1 -x+1/2, y+1/2, -z+1/2 HTAB O2 O4_$1 WGHT 0.054900 3.311600 FVAR 0.04783 0.89613 O1 3 0.333179 0.530693 0.179784 11.00000 0.02266 0.01590 = 0.01710 0.00122 -0.00290 -0.00130 O2 3 0.264809 0.485579 0.261940 11.00000 0.01688 0.02035 = 0.01902 -0.00138 -0.00209 0.00268 O3 3 0.245326 0.367408 0.147060 11.00000 0.02252 0.02139 = 0.01924 -0.00107 -0.00677 -0.00075 O4 3 0.349644 0.103904 0.281952 11.00000 0.02596 0.01601 = 0.03146 0.00270 -0.00682 -0.00253 O5 3 0.617012 0.233921 0.430524 11.00000 0.02175 0.02884 = 0.02588 0.00252 -0.00783 0.00547 C1 1 0.315672 0.442698 0.223764 11.00000 0.01791 0.01566 = 0.01675 0.00093 -0.00067 0.00078 C2 1 0.289672 0.336332 0.189767 11.00000 0.01706 0.02038 = 0.01615 -0.00019 -0.00079 -0.00042 C3 1 0.305129 0.226273 0.207207 11.00000 0.02108 0.01765 = 0.02110 -0.00211 -0.00206 -0.00345 C4 1 0.349202 0.203203 0.258457 11.00000 0.01882 0.01628 = 0.02208 -0.00112 -0.00003 0.00054 C5 1 0.391844 0.302353 0.281224 11.00000 0.01713 0.01702 = 0.01747 -0.00076 -0.00076 0.00003 C6 1 0.375510 0.414885 0.263345 11.00000 0.01619 0.01724 = 0.01573 -0.00008 0.00033 0.00044 C7 1 0.409807 0.515403 0.286108 11.00000 0.01602 0.01614 = 0.01669 -0.00110 0.00188 0.00133 C8 1 0.395905 0.628693 0.258974 11.00000 0.01539 0.01611 = 0.01863 0.00026 0.00151 0.00079 C9 1 0.423174 0.733269 0.283168 11.00000 0.01577 0.01623 = 0.02173 -0.00020 0.00173 0.00097 C10 1 0.411683 0.840227 0.252442 11.00000 0.02070 0.01597 = 0.02739 -0.00024 0.00041 -0.00060 C11 1 0.375072 0.842090 0.199511 11.00000 0.02254 0.01727 = 0.02738 0.00561 0.00040 0.00176 C12 1 0.348230 0.738483 0.174896 11.00000 0.02166 0.02098 = 0.02038 0.00303 -0.00142 0.00090 C13 1 0.358564 0.633361 0.204982 11.00000 0.01720 0.01640 = 0.01967 -0.00067 0.00091 -0.00008 C14 1 0.448851 0.286087 0.320473 11.00000 0.01838 0.01654 = 0.01851 0.00088 0.00003 0.00091 C15 1 0.476259 0.172643 0.332831 11.00000 0.02325 0.01726 = 0.02721 0.00005 -0.00284 0.00089 C16 1 0.531084 0.158254 0.369356 11.00000 0.02377 0.01905 = 0.02937 0.00362 -0.00308 0.00486 C17 1 0.562880 0.257657 0.394651 11.00000 0.01719 0.02635 = 0.01906 0.00230 -0.00197 0.00346 C18 1 0.539744 0.369437 0.381955 11.00000 0.01743 0.02046 = 0.01788 0.00028 -0.00015 0.00043 C19 1 0.481056 0.387129 0.346461 11.00000 0.01617 0.01795 = 0.01603 0.00012 0.00101 0.00092 C20 1 0.456039 0.504313 0.333287 11.00000 0.01518 0.01671 = 0.01710 0.00025 0.00127 -0.00083 C21 1 0.473706 0.612538 0.366337 11.00000 0.01478 0.01801 = 0.01911 -0.00196 0.00095 -0.00082 C22 1 0.498488 0.609934 0.426274 11.00000 0.01955 0.02174 = 0.02035 -0.00107 0.00022 -0.00011 C23 1 0.512474 0.712539 0.457744 11.00000 0.02251 0.02827 = 0.02013 -0.00572 -0.00091 -0.00108 C24 1 0.501737 0.822213 0.430891 11.00000 0.02456 0.02276 = 0.02781 -0.00867 -0.00035 -0.00264 C26 1 0.474329 0.827691 0.373874 11.00000 0.02201 0.01778 = 0.02857 -0.00308 -0.00020 -0.00126 C27 1 0.458613 0.724789 0.340801 11.00000 0.01499 0.01787 = 0.02195 -0.00203 0.00110 -0.00050 C28 1 0.212190 0.271848 0.115960 11.00000 0.02338 0.02658 = 0.02256 -0.00400 -0.00637 -0.00330 C29 1 0.645229 0.331918 0.462945 11.00000 0.02070 0.03714 = 0.02281 -0.00073 -0.00542 0.00232 H1 2 0.229356 0.505417 0.239168 11.00000 0.04663 H2 2 0.283968 0.157831 0.189627 11.00000 0.03032 H3 2 0.428992 0.915535 0.267832 11.00000 0.02575 H4 2 0.367678 0.916930 0.178971 11.00000 0.02345 H5 2 0.321988 0.739929 0.137253 11.00000 0.02852 H6 2 0.454594 0.104540 0.313286 11.00000 0.03110 H7 2 0.549727 0.076659 0.378250 11.00000 0.03309 H8 2 0.564820 0.435755 0.394864 11.00000 0.02195 H9 2 0.503039 0.533853 0.446752 11.00000 0.02394 H10 2 0.528752 0.708664 0.499763 11.00000 0.02629 H11 2 0.511893 0.896066 0.452638 11.00000 0.03356 H12 2 0.463559 0.906160 0.357797 11.00000 0.02851 H13 2 0.182462 0.311610 0.086148 11.00000 0.03356 H14 2 0.187168 0.225330 0.144423 11.00000 0.02973 H15 2 0.245068 0.223331 0.094753 11.00000 0.02511 H16 2 0.611231 0.368637 0.489042 11.00000 0.02407 H17 2 0.664627 0.389480 0.434944 11.00000 0.02374 H18 2 0.681063 0.296669 0.488253 11.00000 0.03134 RESI 1 TOLU PART 1 C1A 1 0.745972 0.601104 0.459650 21.00000 0.02829 0.03607 = 0.02249 -0.00074 -0.00407 -0.00138 AFIX 43 H1A 2 0.750774 0.615548 0.417523 21.00000 -1.20000 AFIX 0 C2A 1 0.685227 0.624393 0.487547 21.00000 0.02580 0.04362 = 0.03366 -0.00026 -0.00369 0.00048 AFIX 43 H2A 2 0.648938 0.655273 0.464514 21.00000 -1.20000 AFIX 0 C3A 1 0.676873 0.603115 0.548661 21.00000 0.03385 0.03729 = 0.03592 -0.00256 0.00541 -0.00211 AFIX 43 H3A 2 0.635100 0.619233 0.567740 21.00000 -1.20000 AFIX 0 C4A 1 0.730277 0.557881 0.581869 21.00000 0.05903 0.03159 = 0.02315 0.00232 0.00146 0.00040 AFIX 43 H4A 2 0.725141 0.542617 0.623888 21.00000 -1.20000 AFIX 0 C5A 1 0.791136 0.535022 0.553578 21.00000 0.04428 0.02832 = 0.03078 -0.00064 -0.01239 0.00560 AFIX 43 H5A 2 0.827360 0.503812 0.576577 21.00000 -1.20000 AFIX 0 C6A 1 0.800078 0.556913 0.492281 21.00000 0.02728 0.02320 = 0.02963 -0.00709 -0.00583 -0.00061 C7A 1 0.866660 0.537012 0.461911 21.00000 0.02733 0.04436 = 0.04886 -0.01560 -0.00579 0.00320 AFIX 137 H7A 2 0.859515 0.522045 0.418703 21.00000 -1.50000 H7B 2 0.889013 0.468691 0.480298 21.00000 -1.50000 H7C 2 0.894877 0.607321 0.466924 21.00000 -1.50000 AFIX 66 PART 2 C1B 1 0.732894 0.624265 0.474089 -21.00000 0.02829 0.03607 = 0.02249 -0.00074 -0.00407 -0.00138 AFIX 43 H1B 2 0.692890 0.665526 0.463894 -21.00000 -1.20000 AFIX 65 C2B 1 0.783933 0.612382 0.431602 -21.00000 0.02580 0.04362 = 0.03366 -0.00026 -0.00369 0.00048 AFIX 43 H2B 2 0.778811 0.645521 0.392370 -21.00000 -1.20000 AFIX 65 C3B 1 0.842465 0.552010 0.446519 -21.00000 0.03385 0.03729 = 0.03592 -0.00256 0.00541 -0.00211 AFIX 43 H3B 2 0.877348 0.543889 0.417481 -21.00000 -1.20000 AFIX 65 C4B 1 0.849959 0.503522 0.503922 -21.00000 0.05903 0.03159 = 0.02315 0.00232 0.00146 0.00040 AFIX 43 H4B 2 0.889963 0.462261 0.514116 -21.00000 -1.20000 AFIX 65 C5B 1 0.798921 0.515405 0.546409 -21.00000 0.04428 0.02832 = 0.03078 -0.00064 -0.01239 0.00560 AFIX 43 H5B 2 0.804043 0.482266 0.585641 -21.00000 -1.20000 AFIX 65 C6B 1 0.740388 0.575776 0.531493 -21.00000 0.02728 0.02320 = 0.02963 -0.00709 -0.00583 -0.00061 AFIX 0 C7B 1 0.690217 0.591204 0.574533 -21.00000 0.02733 0.04436 = 0.04886 -0.01560 -0.00579 0.00320 AFIX 137 H7D 2 0.709540 0.583428 0.615136 -21.00000 -1.50000 H7E 2 0.655352 0.531065 0.568815 -21.00000 -1.50000 H7F 2 0.670394 0.669995 0.569988 -21.00000 -1.50000 PART 0 AFIX 0 HKLF 4 Covalent radii and connectivity table for marc004a in C2/c C 0.770 H 0.320 O 0.660 O1 - C13 C1 O2 - C1 O3 - C2 C28 O4 - C4 O5 - C17 C29 C1 - O2 O1 C2 C6 C2 - O3 C3 C1 C3 - C2 C4 C4 - O4 C3 C5 C5 - C6 C14 C4 C6 - C5 C7 C1 C7 - C20 C6 C8 C8 - C13 C9 C7 C9 - C10 C8 C27 C10 - C11 C9 C11 - C10 C12 C12 - C13 C11 C13 - C12 O1 C8 C14 - C15 C19 C5 C15 - C16 C14 C16 - C15 C17 C17 - O5 C18 C16 C18 - C17 C19 C19 - C18 C14 C20 C20 - C7 C19 C21 C21 - C22 C27 C20 C22 - C23 C21 C23 - C22 C24 C24 - C26 C23 C26 - C24 C27 C27 - C26 C21 C9 C28 - O3 C29 - O5 C1A_1^a - C2A_1^a C6A_1^a C2A_1^a - C3A_1^a C1A_1^a C3A_1^a - C2A_1^a C4A_1^a C4A_1^a - C5A_1^a C3A_1^a C5A_1^a - C4A_1^a C6A_1^a C6A_1^a - C5A_1^a C1A_1^a C7A_1^a C7A_1^a - C6A_1^a C1B_1^b - C2B_1^b C6B_1^b C2B_1^b - C1B_1^b C3B_1^b C3B_1^b - C4B_1^b C2B_1^b C4B_1^b - C5B_1^b C3B_1^b C5B_1^b - C4B_1^b C6B_1^b C6B_1^b - C5B_1^b C1B_1^b C7B_1^b C7B_1^b - C6B_1^b Operators for generating equivalent atoms: $1 -x+1/2, y+1/2, -z+1/2 h k l Fo^2 Sigma Why rejected (first 50 of each listed) 6 0 1 0.03 0.01 systematically absent but >3sig(I) 0 0 3 0.03 0.01 systematically absent but >3sig(I) 0 0 3 0.03 0.01 systematically absent but >3sig(I) -4 0 3 0.03 0.01 systematically absent but >3sig(I) -10 0 3 0.03 0.01 systematically absent but >3sig(I) 8 0 5 0.04 0.01 systematically absent but >3sig(I) 8 0 5 0.03 0.01 systematically absent but >3sig(I) 8 0 5 0.04 0.01 systematically absent but >3sig(I) -4 0 5 0.09 0.01 systematically absent but >3sig(I) -8 0 5 0.07 0.01 systematically absent but >3sig(I) -10 0 5 0.03 0.01 systematically absent but >3sig(I) -18 0 5 0.13 0.03 systematically absent but >3sig(I) -8 0 7 0.04 0.01 systematically absent but >3sig(I) -10 0 7 0.13 0.02 systematically absent but >3sig(I) -12 0 9 0.06 0.02 systematically absent but >3sig(I) 10 0 11 0.13 0.03 systematically absent but >3sig(I) -6 0 11 0.03 0.01 systematically absent but >3sig(I) -8 0 11 0.05 0.01 systematically absent but >3sig(I) -10 0 11 0.07 0.01 systematically absent but >3sig(I) 0 0 13 0.03 0.01 systematically absent but >3sig(I) -10 0 15 0.06 0.02 systematically absent but >3sig(I) 911 Systematically absent reflections rejected 36740 Reflections read, of which 915 rejected -24 =< h =< 24, -14 =< k =< 14, -26 =< l =< 27, Max. 2-theta = 150.96 21 Systematic absence violations (I>3sig(I)) before merging 2 Inconsistent equivalents 5111 Unique reflections, of which 0 suppressed R(int) = 0.0320 R(sigma) = 0.0239 Friedel opposites merged Maximum memory for data reduction = 5192 / 60860 Reflection statistics for all twin components combined (TWST 0 set) Number of data for d > 0.796A (CIF: max) and d > 0.833A (CIF: full) (ignoring systematic absences): Unique reflections found (point group) 5111 4495 Unique reflections possible (point group) 5159 4506 Unique reflections found (Laue group) 5111 4495 Unique reflections possible (Laue group) 5159 4506 Default effective X-H and X-D distances for T = -173.2C 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 = 623 Memory required = 98 / 6396 / 681384 wR2 = 0.0994 before cycle 1 for 5111 data and 445 / 445 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 3.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.04783 0.00008 0.046 OSF 2 0.89613 0.00165 0.002 FVAR 2 Mean shift/esd = 0.003 Maximum = 0.046 for OSF Max. shift = 0.000 A for H7F_1^b Max. dU = 0.000 for H12 Least-squares cycle 2 Maximum vector length = 623 Memory required = 98 / 6396 / 681384 wR2 = 0.0994 before cycle 2 for 5111 data and 445 / 445 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 3.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.04783 0.00008 0.000 OSF 2 0.89613 0.00165 0.001 FVAR 2 Mean shift/esd = 0.001 Maximum = 0.005 for U23 O2 Max. shift = 0.000 A for H7F_1^b Max. dU = 0.000 for H7 Least-squares cycle 3 Maximum vector length = 623 Memory required = 98 / 6396 / 681384 wR2 = 0.0994 before cycle 3 for 5111 data and 445 / 445 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 3.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.04783 0.00008 0.001 OSF 2 0.89613 0.00165 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H2 Max. dU = 0.000 for H13 Least-squares cycle 4 Maximum vector length = 623 Memory required = 98 / 6396 / 681384 wR2 = 0.0994 before cycle 4 for 5111 data and 445 / 445 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 3.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.04783 0.00008 0.000 OSF 2 0.89613 0.00165 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.001 for x C14 Max. shift = 0.000 A for H7D_1^b Max. dU = 0.000 for H16 Least-squares cycle 5 Maximum vector length = 623 Memory required = 98 / 6396 / 681384 wR2 = 0.0994 before cycle 5 for 5111 data and 445 / 445 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 3.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.04783 0.00008 0.000 OSF 2 0.89613 0.00165 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x C24 Max. shift = 0.000 A for H7D_1^b Max. dU = 0.000 for H1 Least-squares cycle 6 Maximum vector length = 623 Memory required = 98 / 6396 / 681384 wR2 = 0.0994 before cycle 6 for 5111 data and 445 / 445 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 3.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.04783 0.00008 0.000 OSF 2 0.89613 0.00165 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x C29 Max. shift = 0.000 A for H7E_1^b Max. dU = 0.000 for H2 Least-squares cycle 7 Maximum vector length = 623 Memory required = 98 / 6396 / 681384 wR2 = 0.0994 before cycle 7 for 5111 data and 445 / 445 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 3.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.04783 0.00008 0.000 OSF 2 0.89613 0.00165 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x C29 Max. shift = 0.000 A for H7F_1^b Max. dU = 0.000 for H2 Least-squares cycle 8 Maximum vector length = 623 Memory required = 98 / 6396 / 681384 wR2 = 0.0994 before cycle 8 for 5111 data and 445 / 445 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 3.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.04783 0.00008 0.000 OSF 2 0.89613 0.00165 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for y C8 Max. shift = 0.000 A for H7F_1^b Max. dU = 0.000 for H6 Least-squares cycle 9 Maximum vector length = 623 Memory required = 98 / 6396 / 681384 wR2 = 0.0994 before cycle 9 for 5111 data and 445 / 445 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 3.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.04783 0.00008 0.000 OSF 2 0.89613 0.00165 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x C24 Max. shift = 0.000 A for H7E_1^b Max. dU = 0.000 for H3 Least-squares cycle 10 Maximum vector length = 623 Memory required = 98 / 6396 / 681384 wR2 = 0.0994 before cycle 10 for 5111 data and 445 / 445 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 3.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.04783 0.00008 0.000 OSF 2 0.89613 0.00165 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x C24 Max. shift = 0.000 A for H7E_1^b Max. dU = 0.000 for H3 Least-squares cycle 11 Maximum vector length = 623 Memory required = 98 / 6396 / 681384 wR2 = 0.0994 before cycle 11 for 5111 data and 445 / 445 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 3.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.04783 0.00008 0.000 OSF 2 0.89613 0.00165 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x C29 Max. shift = 0.000 A for H7E_1^b Max. dU = 0.000 for H11 Least-squares cycle 12 Maximum vector length = 623 Memory required = 98 / 6396 / 681384 wR2 = 0.0994 before cycle 12 for 5111 data and 445 / 445 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 3.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.04783 0.00008 0.000 OSF 2 0.89613 0.00165 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x C24 Max. shift = 0.000 A for H7E_1^b Max. dU = 0.000 for H3 Least-squares cycle 13 Maximum vector length = 623 Memory required = 98 / 6396 / 681384 wR2 = 0.0994 before cycle 13 for 5111 data and 445 / 445 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 3.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.04783 0.00008 0.000 OSF 2 0.89613 0.00165 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x C29 Max. shift = 0.000 A for H7 Max. dU = 0.000 for H1 Least-squares cycle 14 Maximum vector length = 623 Memory required = 98 / 6396 / 681384 wR2 = 0.0994 before cycle 14 for 5111 data and 445 / 445 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 3.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.04783 0.00008 0.000 OSF 2 0.89613 0.00165 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x O2 Max. shift = 0.000 A for H7E_1^b Max. dU = 0.000 for H16 Least-squares cycle 15 Maximum vector length = 623 Memory required = 98 / 6396 / 681384 wR2 = 0.0994 before cycle 15 for 5111 data and 445 / 445 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 3.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.04783 0.00008 0.000 OSF 2 0.89613 0.00165 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x O2 Max. shift = 0.000 A for H7D_1^b Max. dU = 0.000 for H9 Least-squares cycle 16 Maximum vector length = 623 Memory required = 98 / 6396 / 681384 wR2 = 0.0994 before cycle 16 for 5111 data and 445 / 445 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 3.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.04783 0.00008 0.001 OSF 2 0.89613 0.00165 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H7E_1^b Max. dU = 0.000 for H1 Least-squares cycle 17 Maximum vector length = 623 Memory required = 98 / 6396 / 681384 wR2 = 0.0994 before cycle 17 for 5111 data and 445 / 445 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 3.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.04783 0.00008 0.000 OSF 2 0.89613 0.00165 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x O2 Max. shift = 0.000 A for H11 Max. dU = 0.000 for H9 Least-squares cycle 18 Maximum vector length = 623 Memory required = 98 / 6396 / 681384 wR2 = 0.0994 before cycle 18 for 5111 data and 445 / 445 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 3.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.04783 0.00008 0.000 OSF 2 0.89613 0.00165 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z C20 Max. shift = 0.000 A for H7E_1^b Max. dU = 0.000 for H3 Least-squares cycle 19 Maximum vector length = 623 Memory required = 98 / 6396 / 681384 wR2 = 0.0994 before cycle 19 for 5111 data and 445 / 445 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 3.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.04783 0.00008 0.000 OSF 2 0.89613 0.00165 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x C29 Max. shift = 0.000 A for H7E_1^b Max. dU = 0.000 for H4 Least-squares cycle 20 Maximum vector length = 623 Memory required = 98 / 6396 / 681384 wR2 = 0.0994 before cycle 20 for 5111 data and 445 / 445 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 3.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.04783 0.00008 0.000 OSF 2 0.89613 0.00165 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x C29 Max. shift = 0.000 A for H7E_1^b Max. dU = 0.000 for H18 Largest correlation matrix elements -0.742 y C1B_1^b / rotZ C1B_1^b 0.541 z C1B_1^b / rotY C1B_1^b Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.7508 0.6155 0.4175 43 0.950 0.000 C1A_1^a C2A_1^a C6A_1^a H2A 0.6489 0.6553 0.4645 43 0.950 0.000 C2A_1^a C3A_1^a C1A_1^a H3A 0.6351 0.6192 0.5677 43 0.950 0.000 C3A_1^a C2A_1^a C4A_1^a H4A 0.7251 0.5426 0.6239 43 0.950 0.000 C4A_1^a C5A_1^a C3A_1^a H5A 0.8274 0.5038 0.5766 43 0.950 0.000 C5A_1^a C4A_1^a C6A_1^a H7A 0.8595 0.5220 0.4187 137 0.980 0.000 C7A_1^a C6A_1^a H7A_1^a H7B 0.8890 0.4687 0.4803 137 0.980 0.000 C7A_1^a C6A_1^a H7A_1^a H7C 0.8949 0.6073 0.4669 137 0.980 0.000 C7A_1^a C6A_1^a H7A_1^a H1B 0.6929 0.6655 0.4639 43 0.950 0.000 C1B_1^b C2B_1^b C6B_1^b H2B 0.7788 0.6455 0.3924 43 0.950 0.000 C2B_1^b C1B_1^b C3B_1^b H3B 0.8773 0.5439 0.4175 43 0.950 0.000 C3B_1^b C4B_1^b C2B_1^b H4B 0.8900 0.4623 0.5141 43 0.950 0.000 C4B_1^b C5B_1^b C3B_1^b H5B 0.8040 0.4823 0.5856 43 0.950 0.000 C5B_1^b C4B_1^b C6B_1^b H7D 0.7095 0.5834 0.6151 137 0.980 0.000 C7B_1^b C6B_1^b H7D_1^b H7E 0.6554 0.5311 0.5688 137 0.980 0.000 C7B_1^b C6B_1^b H7D_1^b H7F 0.6704 0.6700 0.5700 137 0.980 0.000 C7B_1^b C6B_1^b H7D_1^b marc004a in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq O1 0.33318 0.53069 0.17978 1.00000 0.02266 0.01590 0.01710 0.00122 -0.00290 -0.00130 0.01855 0.00124 0.00004 0.00006 0.00003 0.00000 0.00038 0.00036 0.00035 0.00027 0.00028 0.00028 0.00017 O2 0.26481 0.48558 0.26194 1.00000 0.01688 0.02035 0.01902 -0.00138 -0.00209 0.00268 0.01875 0.00128 0.00004 0.00007 0.00003 0.00000 0.00036 0.00037 0.00037 0.00028 0.00028 0.00028 0.00017 O3 0.24533 0.36741 0.14706 1.00000 0.02252 0.02139 0.01924 -0.00107 -0.00677 -0.00075 0.02105 0.00127 0.00004 0.00007 0.00003 0.00000 0.00038 0.00038 0.00037 0.00029 0.00029 0.00030 0.00017 O4 0.34964 0.10390 0.28195 1.00000 0.02596 0.01601 0.03146 0.00270 -0.00682 -0.00253 0.02448 0.00134 0.00004 0.00007 0.00004 0.00000 0.00041 0.00037 0.00043 0.00030 0.00032 0.00030 0.00018 O5 0.61701 0.23392 0.43052 1.00000 0.02175 0.02884 0.02588 0.00252 -0.00783 0.00547 0.02549 0.00142 0.00004 0.00007 0.00004 0.00000 0.00040 0.00043 0.00041 0.00032 0.00031 0.00032 0.00019 C1 0.31567 0.44270 0.22376 1.00000 0.01791 0.01566 0.01675 0.00093 -0.00067 0.00078 0.01677 0.00177 0.00005 0.00009 0.00005 0.00000 0.00048 0.00047 0.00047 0.00037 0.00037 0.00038 0.00021 C2 0.28967 0.33633 0.18977 1.00000 0.01706 0.02038 0.01615 -0.00019 -0.00079 -0.00042 0.01786 0.00179 0.00005 0.00009 0.00005 0.00000 0.00048 0.00051 0.00047 0.00038 0.00037 0.00039 0.00021 C3 0.30513 0.22627 0.20721 1.00000 0.02108 0.01765 0.02110 -0.00211 -0.00206 -0.00345 0.01995 0.00183 0.00005 0.00009 0.00005 0.00000 0.00051 0.00050 0.00051 0.00039 0.00040 0.00040 0.00022 C4 0.34920 0.20320 0.25846 1.00000 0.01882 0.01628 0.02208 -0.00112 -0.00003 0.00054 0.01906 0.00182 0.00005 0.00009 0.00005 0.00000 0.00049 0.00048 0.00051 0.00039 0.00039 0.00039 0.00022 C5 0.39184 0.30235 0.28122 1.00000 0.01713 0.01702 0.01747 -0.00076 -0.00076 0.00003 0.01721 0.00175 0.00005 0.00009 0.00005 0.00000 0.00048 0.00048 0.00047 0.00037 0.00037 0.00039 0.00021 C6 0.37551 0.41489 0.26334 1.00000 0.01619 0.01724 0.01573 -0.00008 0.00033 0.00044 0.01639 0.00176 0.00005 0.00009 0.00005 0.00000 0.00047 0.00049 0.00046 0.00037 0.00036 0.00038 0.00021 C7 0.40981 0.51540 0.28611 1.00000 0.01602 0.01614 0.01669 -0.00110 0.00188 0.00133 0.01628 0.00178 0.00005 0.00009 0.00005 0.00000 0.00047 0.00049 0.00047 0.00037 0.00037 0.00037 0.00021 C8 0.39591 0.62869 0.25897 1.00000 0.01539 0.01611 0.01863 0.00026 0.00151 0.00079 0.01671 0.00179 0.00005 0.00009 0.00005 0.00000 0.00047 0.00049 0.00049 0.00037 0.00037 0.00037 0.00021 C9 0.42317 0.73327 0.28317 1.00000 0.01577 0.01623 0.02173 -0.00020 0.00173 0.00097 0.01791 0.00184 0.00005 0.00009 0.00005 0.00000 0.00047 0.00049 0.00051 0.00038 0.00038 0.00037 0.00021 C10 0.41168 0.84023 0.25244 1.00000 0.02070 0.01597 0.02739 -0.00024 0.00041 -0.00060 0.02135 0.00193 0.00006 0.00010 0.00005 0.00000 0.00051 0.00050 0.00055 0.00041 0.00042 0.00040 0.00023 C11 0.37507 0.84209 0.19951 1.00000 0.02254 0.01727 0.02738 0.00561 0.00040 0.00176 0.02239 0.00202 0.00006 0.00010 0.00005 0.00000 0.00054 0.00051 0.00056 0.00042 0.00042 0.00041 0.00023 C12 0.34823 0.73848 0.17490 1.00000 0.02166 0.02098 0.02038 0.00303 -0.00142 0.00090 0.02101 0.00196 0.00006 0.00010 0.00005 0.00000 0.00052 0.00053 0.00052 0.00041 0.00041 0.00042 0.00023 C13 0.35856 0.63336 0.20498 1.00000 0.01720 0.01640 0.01967 -0.00067 0.00091 -0.00008 0.01776 0.00181 0.00005 0.00009 0.00005 0.00000 0.00048 0.00049 0.00049 0.00038 0.00037 0.00038 0.00021 C14 0.44885 0.28609 0.32047 1.00000 0.01838 0.01654 0.01851 0.00088 0.00003 0.00091 0.01781 0.00181 0.00005 0.00009 0.00005 0.00000 0.00048 0.00049 0.00049 0.00037 0.00038 0.00038 0.00021 C15 0.47626 0.17264 0.33283 1.00000 0.02325 0.01726 0.02721 0.00005 -0.00284 0.00089 0.02257 0.00200 0.00006 0.00010 0.00005 0.00000 0.00054 0.00052 0.00055 0.00042 0.00043 0.00042 0.00023 C16 0.53108 0.15825 0.36936 1.00000 0.02377 0.01905 0.02937 0.00362 -0.00308 0.00486 0.02406 0.00206 0.00006 0.00010 0.00005 0.00000 0.00055 0.00053 0.00058 0.00043 0.00044 0.00043 0.00024 C17 0.56288 0.25766 0.39465 1.00000 0.01719 0.02635 0.01906 0.00230 -0.00197 0.00346 0.02087 0.00194 0.00005 0.00010 0.00005 0.00000 0.00049 0.00056 0.00050 0.00041 0.00038 0.00042 0.00022 C18 0.53974 0.36944 0.38195 1.00000 0.01743 0.02046 0.01788 0.00028 -0.00015 0.00043 0.01859 0.00186 0.00005 0.00010 0.00005 0.00000 0.00049 0.00052 0.00048 0.00039 0.00038 0.00040 0.00022 C19 0.48106 0.38713 0.34646 1.00000 0.01617 0.01795 0.01603 0.00012 0.00101 0.00092 0.01671 0.00177 0.00005 0.00009 0.00004 0.00000 0.00048 0.00050 0.00046 0.00036 0.00037 0.00038 0.00021 C20 0.45604 0.50431 0.33329 1.00000 0.01518 0.01671 0.01710 0.00025 0.00127 -0.00083 0.01633 0.00177 0.00005 0.00009 0.00005 0.00000 0.00046 0.00049 0.00047 0.00037 0.00037 0.00037 0.00021 C21 0.47371 0.61254 0.36634 1.00000 0.01478 0.01801 0.01911 -0.00196 0.00095 -0.00082 0.01730 0.00176 0.00005 0.00009 0.00005 0.00000 0.00046 0.00050 0.00049 0.00038 0.00037 0.00037 0.00021 C22 0.49849 0.60993 0.42627 1.00000 0.01955 0.02174 0.02035 -0.00107 0.00022 -0.00011 0.02055 0.00189 0.00005 0.00010 0.00005 0.00000 0.00050 0.00054 0.00051 0.00041 0.00039 0.00040 0.00022 C23 0.51247 0.71254 0.45774 1.00000 0.02251 0.02827 0.02013 -0.00572 -0.00091 -0.00108 0.02364 0.00193 0.00006 0.00011 0.00005 0.00000 0.00054 0.00058 0.00054 0.00043 0.00041 0.00044 0.00024 C24 0.50174 0.82221 0.43089 1.00000 0.02456 0.02276 0.02781 -0.00867 -0.00035 -0.00264 0.02504 0.00194 0.00006 0.00010 0.00005 0.00000 0.00056 0.00055 0.00058 0.00045 0.00044 0.00044 0.00024 C26 0.47433 0.82769 0.37387 1.00000 0.02201 0.01778 0.02857 -0.00308 -0.00020 -0.00126 0.02279 0.00193 0.00006 0.00010 0.00005 0.00000 0.00053 0.00052 0.00058 0.00043 0.00042 0.00041 0.00023 C27 0.45861 0.72479 0.34080 1.00000 0.01499 0.01787 0.02195 -0.00203 0.00110 -0.00050 0.01827 0.00181 0.00005 0.00009 0.00005 0.00000 0.00047 0.00051 0.00052 0.00039 0.00038 0.00037 0.00022 C28 0.21219 0.27185 0.11596 1.00000 0.02338 0.02658 0.02256 -0.00400 -0.00637 -0.00330 0.02417 0.00188 0.00006 0.00011 0.00005 0.00000 0.00055 0.00058 0.00055 0.00045 0.00044 0.00046 0.00024 C29 0.64523 0.33192 0.46295 1.00000 0.02070 0.03714 0.02281 -0.00073 -0.00542 0.00232 0.02688 0.00209 0.00006 0.00012 0.00005 0.00000 0.00055 0.00067 0.00055 0.00049 0.00044 0.00049 0.00025 H1 0.22936 0.50542 0.23917 1.00000 0.04663 0.03072 0.00093 0.00157 0.00079 0.00000 0.00472 H2 0.28397 0.15783 0.18963 1.00000 0.03032 0.02700 0.00077 0.00138 0.00067 0.00000 0.00368 H3 0.42899 0.91554 0.26783 1.00000 0.02575 0.02508 0.00072 0.00129 0.00063 0.00000 0.00344 H4 0.36768 0.91693 0.17897 1.00000 0.02345 0.02366 0.00070 0.00126 0.00062 0.00000 0.00333 H5 0.32199 0.73993 0.13725 1.00000 0.02852 0.02587 0.00074 0.00129 0.00068 0.00000 0.00360 H6 0.45459 0.10454 0.31329 1.00000 0.03110 0.02689 0.00078 0.00135 0.00068 0.00000 0.00373 H7 0.54973 0.07666 0.37825 1.00000 0.03309 0.02605 0.00077 0.00141 0.00067 0.00000 0.00384 H8 0.56482 0.43576 0.39486 1.00000 0.02195 0.02484 0.00071 0.00126 0.00061 0.00000 0.00321 H9 0.50304 0.53385 0.44675 1.00000 0.02394 0.02388 0.00070 0.00128 0.00062 0.00000 0.00334 H10 0.52875 0.70866 0.49976 1.00000 0.02629 0.02489 0.00071 0.00124 0.00067 0.00000 0.00350 H11 0.51189 0.89607 0.45264 1.00000 0.03356 0.02748 0.00078 0.00138 0.00069 0.00000 0.00392 H12 0.46356 0.90616 0.35780 1.00000 0.02851 0.02485 0.00074 0.00133 0.00065 0.00000 0.00360 H13 0.18246 0.31161 0.08615 1.00000 0.03356 0.02662 0.00078 0.00140 0.00071 0.00000 0.00383 H14 0.18717 0.22533 0.14442 1.00000 0.02973 0.02491 0.00074 0.00131 0.00068 0.00000 0.00371 H15 0.24507 0.22333 0.09475 1.00000 0.02511 0.02390 0.00073 0.00126 0.00064 0.00000 0.00343 H16 0.61123 0.36864 0.48904 1.00000 0.02407 0.02377 0.00072 0.00123 0.00063 0.00000 0.00336 H17 0.66463 0.38948 0.43494 1.00000 0.02374 0.02372 0.00071 0.00124 0.00064 0.00000 0.00338 H18 0.68106 0.29667 0.48825 1.00000 0.03134 0.02583 0.00077 0.00133 0.00069 0.00000 0.00374 C1A_1^a 0.74597 0.60110 0.45965 0.89613 0.02829 0.03607 0.02249 -0.00074 -0.00407 -0.00138 0.02895 0.00250 0.00008 0.00014 0.00006 0.00165 0.00073 0.00080 0.00069 0.00055 0.00056 0.00057 0.00032 H1A_1^a 0.75077 0.61555 0.41752 0.89613 0.03474 0.00165 0.00000 C2A_1^a 0.68523 0.62439 0.48755 0.89613 0.02580 0.04362 0.03366 -0.00026 -0.00369 0.00048 0.03436 0.00259 0.00007 0.00014 0.00007 0.00165 0.00071 0.00085 0.00075 0.00062 0.00056 0.00060 0.00034 H2A_1^a 0.64894 0.65527 0.46451 0.89613 0.04123 0.00165 0.00000 C3A_1^a 0.67687 0.60312 0.54866 0.89613 0.03385 0.03729 0.03592 -0.00256 0.00541 -0.00211 0.03569 0.00310 0.00009 0.00015 0.00008 0.00165 0.00085 0.00083 0.00084 0.00066 0.00066 0.00065 0.00036 H3A_1^a 0.63510 0.61923 0.56774 0.89613 0.04283 0.00165 0.00000 C4A_1^a 0.73028 0.55788 0.58187 0.89613 0.05903 0.03159 0.02315 0.00232 0.00146 0.00040 0.03792 0.00288 0.00010 0.00014 0.00007 0.00165 0.00111 0.00075 0.00068 0.00055 0.00065 0.00073 0.00037 H4A_1^a 0.72514 0.54262 0.62389 0.89613 0.04551 0.00165 0.00000 C5A_1^a 0.79114 0.53502 0.55358 0.89613 0.04428 0.02832 0.03078 -0.00064 -0.01239 0.00560 0.03446 0.00300 0.00009 0.00014 0.00007 0.00165 0.00083 0.00078 0.00071 0.00056 0.00059 0.00061 0.00035 H5A_1^a 0.82736 0.50381 0.57658 0.89613 0.04136 0.00165 0.00000 C6A_1^a 0.80008 0.55691 0.49228 0.89613 0.02728 0.02320 0.02963 -0.00709 -0.00583 -0.00061 0.02671 0.00217 0.00007 0.00012 0.00006 0.00165 0.00066 0.00063 0.00067 0.00050 0.00051 0.00051 0.00029 C7A_1^a 0.86666 0.53701 0.46191 0.89613 0.02733 0.04436 0.04886 -0.01560 -0.00579 0.00320 0.04019 0.00279 0.00008 0.00016 0.00008 0.00165 0.00076 0.00090 0.00097 0.00074 0.00065 0.00066 0.00039 H7A_1^a 0.85952 0.52205 0.41870 0.89613 0.06028 0.00165 0.00000 H7B_1^a 0.88901 0.46869 0.48030 0.89613 0.06028 0.00165 0.00000 H7C_1^a 0.89488 0.60732 0.46692 0.89613 0.06028 0.00165 0.00000 C1B_1^b 0.73289 0.62427 0.47409 0.10387 0.02829 0.03607 0.02249 -0.00074 -0.00407 -0.00138 0.02895 0.01653 0.00040 0.00086 0.00039 0.00165 0.00073 0.00080 0.00069 0.00055 0.00056 0.00057 0.00032 H1B_1^b 0.69289 0.66553 0.46389 0.10387 0.03474 0.00165 0.00000 C2B_1^b 0.78393 0.61238 0.43160 0.10387 0.02580 0.04362 0.03366 -0.00026 -0.00369 0.00048 0.03436 0.01759 0.00049 0.00089 0.00031 0.00165 0.00071 0.00085 0.00075 0.00062 0.00056 0.00060 0.00034 H2B_1^b 0.77881 0.64552 0.39237 0.10387 0.04123 0.00165 0.00000 C3B_1^b 0.84247 0.55201 0.44652 0.10387 0.03385 0.03729 0.03592 -0.00256 0.00541 -0.00211 0.03569 0.01718 0.00041 0.00087 0.00037 0.00165 0.00085 0.00083 0.00084 0.00066 0.00066 0.00065 0.00036 H3B_1^b 0.87735 0.54389 0.41748 0.10387 0.04283 0.00165 0.00000 C4B_1^b 0.84996 0.50352 0.50392 0.10387 0.05903 0.03159 0.02315 0.00232 0.00146 0.00040 0.03792 0.01873 0.00041 0.00090 0.00041 0.00165 0.00111 0.00075 0.00068 0.00055 0.00065 0.00073 0.00037 H4B_1^b 0.88996 0.46226 0.51412 0.10387 0.04551 0.00165 0.00000 C5B_1^b 0.79892 0.51541 0.54641 0.10387 0.04428 0.02832 0.03078 -0.00064 -0.01239 0.00560 0.03446 0.01910 0.00050 0.00093 0.00033 0.00165 0.00083 0.00078 0.00071 0.00056 0.00059 0.00061 0.00035 H5B_1^b 0.80404 0.48227 0.58564 0.10387 0.04136 0.00165 0.00000 C6B_1^b 0.74039 0.57578 0.53149 0.10387 0.02728 0.02320 0.02963 -0.00709 -0.00583 -0.00061 0.02671 0.01650 0.00041 0.00087 0.00035 0.00165 0.00066 0.00063 0.00067 0.00050 0.00051 0.00051 0.00029 C7B_1^b 0.69022 0.59120 0.57453 0.10387 0.02733 0.04436 0.04886 -0.01560 -0.00579 0.00320 0.04019 0.02853 0.00089 0.00166 0.00088 0.00165 0.00076 0.00090 0.00097 0.00074 0.00065 0.00066 0.00039 H7D_1^b 0.70954 0.58343 0.61514 0.10387 0.06028 0.00165 0.00000 H7E_1^b 0.65535 0.53106 0.56882 0.10387 0.06028 0.00165 0.00000 H7F_1^b 0.67039 0.67000 0.56999 0.10387 0.06028 0.00165 0.00000 Final Structure Factor Calculation for marc004a in C2/c Total number of l.s. parameters = 445 Maximum vector length = 623 Memory required = 98 / 5951 / 26789 wR2 = 0.0994 before cycle 21 for 5111 data and 0 / 445 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0549 * P )^2 + 3.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 wR2 = 0.0994, GooF = S = 1.040, Restrained GooF = 1.040 for all data R1 = 0.0356 for 4759 Fo > 4sig(Fo) and 0.0378 for all 5111 data Occupancy sum of asymmetric unit = 40.00 for non-hydrogen and 26.00 for H and D atoms Principal mean square atomic displacements U 0.0242 0.0163 0.0151 O1 0.0231 0.0182 0.0150 O2 0.0279 0.0216 0.0137 O3 0.0367 0.0214 0.0153 O4 0.0328 0.0302 0.0135 O5 0.0183 0.0172 0.0148 C1 0.0204 0.0175 0.0157 C2 0.0235 0.0220 0.0143 C3 0.0223 0.0189 0.0160 C4 0.0184 0.0170 0.0162 C5 0.0174 0.0162 0.0155 C6 0.0183 0.0172 0.0134 C7 0.0193 0.0163 0.0145 C8 0.0222 0.0169 0.0147 C9 0.0274 0.0208 0.0159 C10 0.0300 0.0226 0.0145 C11 0.0238 0.0222 0.0170 C12 0.0201 0.0169 0.0163 C13 0.0191 0.0184 0.0159 C14 0.0287 0.0219 0.0171 C15 0.0310 0.0267 0.0145 C16 0.0278 0.0203 0.0145 C17 0.0205 0.0179 0.0173 C18 0.0185 0.0167 0.0150 C19 0.0178 0.0170 0.0143 C20 0.0209 0.0165 0.0145 C21 0.0223 0.0198 0.0195 C22 0.0313 0.0228 0.0169 C23 0.0345 0.0250 0.0156 C24 0.0294 0.0223 0.0167 C26 0.0230 0.0170 0.0148 C27 0.0295 0.0286 0.0144 C28 0.0376 0.0269 0.0161 C29 0.0363 0.0303 0.0203 C1A_1^a 0.0437 0.0351 0.0243 C2A_1^a 0.0425 0.0352 0.0294 C3A_1^a 0.0591 0.0322 0.0225 C4A_1^a 0.0527 0.0283 0.0224 C5A_1^a 0.0366 0.0264 0.0171 C6A_1^a 0.0635 0.0312 0.0258 C7A_1^a 0.0363 0.0303 0.0203 C1B_1^b 0.0437 0.0351 0.0243 C2B_1^b 0.0425 0.0352 0.0294 C3B_1^b 0.0591 0.0322 0.0225 C4B_1^b 0.0527 0.0283 0.0224 C5B_1^b 0.0366 0.0264 0.0171 C6B_1^b 0.0635 0.0312 0.0258 C7B_1^b 0 atoms may be split and 0 atoms NPD Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.014 0.022 0.030 0.039 0.050 0.063 0.083 0.119 1.000 Number in group 543. 508. 533. 516. 488. 499. 493. 518. 506. 507. GooF 0.983 0.990 1.041 1.109 1.068 1.126 1.120 1.041 0.968 0.944 K 1.482 1.044 0.977 0.984 0.983 0.995 1.000 1.005 1.010 1.000 Resolution(A) 0.80 0.83 0.86 0.90 0.95 1.01 1.08 1.19 1.37 1.72 inf Number in group 528. 507. 513. 507. 514. 504. 502. 511. 512. 513. GooF 1.236 1.024 0.870 0.806 0.975 1.059 1.011 0.864 1.168 1.270 K 1.049 1.043 1.023 1.019 0.988 0.972 0.995 1.012 1.033 0.992 R1 0.068 0.054 0.046 0.039 0.036 0.035 0.030 0.027 0.038 0.034 Recommended weighting scheme: WGHT 0.0519 3.4447 Most Disagreeable Reflections (* if suppressed or used for Rfree). Error/esd is calculated as sqrt(wD^2/) where w is given by the weight formula, D = Fo^2-Fc^2 and <> refers to the average over all reflections. h k l Fo^2 Fc^2 Error/esd Fc/Fc(max) Resolution(A) 7 9 11 146.92 299.81 4.78 0.034 1.00 -23 3 9 218.53 425.68 4.61 0.040 0.80 18 0 0 3236.88 2368.79 4.51 0.095 1.11 6 4 4 150.33 67.38 4.38 0.016 2.01 2 8 11 263.45 148.13 4.15 0.024 1.15 19 3 17 2242.07 1601.73 4.13 0.078 0.80 10 8 5 520.38 775.92 3.94 0.054 1.12 1 5 8 516.45 347.06 3.91 0.036 1.74 8 10 7 662.93 941.27 3.91 0.060 0.98 0 4 6 220.86 365.74 3.85 0.037 2.24 2 8 9 340.52 521.12 3.84 0.045 1.22 17 3 19 810.06 1188.02 3.82 0.067 0.81 4 12 8 39.71 6.22 3.82 0.005 0.88 -12 4 23 485.13 741.70 3.77 0.053 0.80 5 9 8 27.78 2.31 3.77 0.003 1.10 8 8 8 212.42 349.69 3.74 0.036 1.12 1 7 4 93.62 39.02 3.70 0.012 1.55 12 4 21 299.51 187.31 3.68 0.027 0.85 3 1 10 716.07 511.34 3.68 0.044 2.06 6 4 1 66.58 22.41 3.67 0.009 2.14 0 14 4 625.60 432.41 3.67 0.041 0.80 18 2 18 946.17 692.67 3.58 0.051 0.81 -3 1 6 152.30 79.06 3.58 0.017 3.10 7 13 3 832.96 611.66 3.55 0.048 0.83 -4 0 2 112112.44 141413.50 3.54 0.734 4.54 4 10 9 646.12 887.37 3.53 0.058 1.01 6 8 11 35.52 6.86 3.50 0.005 1.09 1 7 0 93.15 176.50 3.49 0.026 1.61 4 10 11 0.30 31.78 3.43 0.011 0.97 3 5 6 3683.15 2979.23 3.38 0.106 1.85 6 10 18 591.51 426.83 3.33 0.040 0.81 9 9 8 1959.78 2477.07 3.33 0.097 1.02 5 5 4 7272.02 5978.13 3.32 0.151 1.85 -5 1 3 211594.12 262815.59 3.29 1.000 3.35 2 14 1 220.34 129.09 3.25 0.022 0.80 -2 0 18 1057.66 785.22 3.25 0.055 1.22 -3 1 7 218.93 134.98 3.25 0.023 2.76 9 1 17 77.54 33.75 3.19 0.011 1.11 6 2 11 607.67 810.86 3.14 0.056 1.64 3 13 4 337.73 231.09 3.11 0.030 0.85 10 10 16 1869.67 1408.49 3.11 0.073 0.80 8 4 24 1442.88 1146.16 3.09 0.066 0.83 7 3 8 247.43 362.95 3.08 0.037 1.75 14 2 13 322.04 457.86 3.08 0.042 1.07 7 13 6 264.04 174.45 3.06 0.026 0.81 8 2 9 13.91 0.02 3.03 0.000 1.67 9 9 18 996.33 775.40 3.02 0.054 0.82 11 9 7 970.62 1242.67 3.01 0.069 0.98 7 9 6 89.54 158.57 3.01 0.025 1.10 6 2 8 248.40 161.41 3.00 0.025 1.99 Bond lengths and angles O1 - Distance Angles C13 1.3836 (0.0012) C1 1.4343 (0.0012) 113.50 (0.08) O1 C13 O2 - Distance Angles C1 1.4044 (0.0012) H1 0.8951 (0.0183) 108.49 (1.14) O2 C1 O3 - Distance Angles C2 1.3389 (0.0013) C28 1.4408 (0.0013) 116.15 (0.08) O3 C2 O4 - Distance Angles C4 1.2377 (0.0013) O4 O5 - Distance Angles C17 1.3641 (0.0013) C29 1.4345 (0.0015) 116.56 (0.09) O5 C17 C1 - Distance Angles O2 1.4044 (0.0012) O1 1.4343 (0.0012) 110.03 (0.08) C2 1.5100 (0.0014) 109.10 (0.08) 107.42 (0.08) C6 1.5105 (0.0014) 107.01 (0.08) 110.20 (0.08) 113.08 (0.08) C1 O2 O1 C2 C2 - Distance Angles O3 1.3389 (0.0013) C3 1.3393 (0.0015) 126.75 (0.10) C1 1.5100 (0.0014) 111.54 (0.09) 121.28 (0.09) C2 O3 C3 C3 - Distance Angles C2 1.3393 (0.0015) C4 1.4558 (0.0015) 121.93 (0.10) H2 0.9632 (0.0156) 122.08 (0.90) 115.65 (0.90) C3 C2 C4 C4 - Distance Angles O4 1.2377 (0.0013) C3 1.4558 (0.0015) 119.56 (0.10) C5 1.4938 (0.0014) 122.44 (0.10) 118.00 (0.09) C4 O4 C3 C5 - Distance Angles C6 1.3721 (0.0014) C14 1.4397 (0.0014) 118.60 (0.09) C4 1.4938 (0.0014) 117.73 (0.09) 123.67 (0.09) C5 C6 C14 C6 - Distance Angles C5 1.3721 (0.0014) C7 1.4185 (0.0014) 121.86 (0.09) C1 1.5105 (0.0014) 123.14 (0.09) 114.68 (0.09) C6 C5 C7 C7 - Distance Angles C20 1.3959 (0.0014) C6 1.4185 (0.0014) 120.65 (0.09) C8 1.4418 (0.0014) 121.12 (0.09) 118.23 (0.09) C7 C20 C6 C8 - Distance Angles C13 1.4064 (0.0015) C9 1.4072 (0.0014) 119.63 (0.09) C7 1.4418 (0.0014) 119.17 (0.09) 121.03 (0.09) C8 C13 C9 C9 - Distance Angles C10 1.4063 (0.0015) C8 1.4072 (0.0014) 118.52 (0.10) C27 1.4588 (0.0015) 123.82 (0.10) 117.56 (0.09) C9 C10 C8 C10 - Distance Angles C11 1.3780 (0.0016) C9 1.4063 (0.0015) 120.59 (0.10) H3 0.9799 (0.0146) 117.84 (0.83) 121.57 (0.83) C10 C11 C9 C11 - Distance Angles C10 1.3780 (0.0016) C12 1.3983 (0.0016) 121.28 (0.10) H4 0.9719 (0.0142) 119.32 (0.82) 119.40 (0.81) C11 C10 C12 C12 - Distance Angles C13 1.3780 (0.0015) C11 1.3983 (0.0016) 118.62 (0.10) H5 0.9822 (0.0150) 120.15 (0.87) 121.23 (0.86) C12 C13 C11 C13 - Distance Angles C12 1.3780 (0.0015) O1 1.3836 (0.0012) 118.43 (0.09) C8 1.4064 (0.0015) 121.36 (0.10) 120.18 (0.09) C13 C12 O1 C14 - Distance Angles C15 1.4211 (0.0015) C19 1.4308 (0.0014) 118.21 (0.09) C5 1.4397 (0.0014) 122.25 (0.10) 119.50 (0.09) C14 C15 C19 C15 - Distance Angles C16 1.3668 (0.0016) C14 1.4211 (0.0015) 121.83 (0.10) H6 0.9829 (0.0154) 121.07 (0.88) 117.08 (0.88) C15 C16 C14 C16 - Distance Angles C15 1.3668 (0.0016) C17 1.4062 (0.0016) 119.90 (0.10) H7 1.0142 (0.0158) 120.99 (0.86) 119.11 (0.86) C16 C15 C17 C17 - Distance Angles O5 1.3641 (0.0013) C18 1.3748 (0.0015) 124.34 (0.10) C16 1.4062 (0.0016) 115.39 (0.10) 120.26 (0.10) C17 O5 C18 C18 - Distance Angles C17 1.3748 (0.0015) C19 1.4209 (0.0014) 121.16 (0.10) H8 0.9452 (0.0144) 119.46 (0.85) 119.25 (0.85) C18 C17 C19 C19 - Distance Angles C18 1.4209 (0.0014) C14 1.4308 (0.0014) 118.49 (0.09) C20 1.4458 (0.0014) 121.55 (0.09) 119.85 (0.09) C19 C18 C14 C20 - Distance Angles C7 1.3959 (0.0014) C19 1.4458 (0.0014) 117.37 (0.09) C21 1.4684 (0.0014) 117.01 (0.09) 125.60 (0.09) C20 C7 C19 C21 - Distance Angles C22 1.4135 (0.0015) C27 1.4218 (0.0014) 117.65 (0.09) C20 1.4684 (0.0014) 122.15 (0.09) 119.80 (0.09) C21 C22 C27 C22 - Distance Angles C23 1.3815 (0.0015) C21 1.4135 (0.0015) 121.62 (0.10) H9 0.9767 (0.0145) 119.26 (0.82) 119.00 (0.81) C22 C23 C21 C23 - Distance Angles C22 1.3815 (0.0015) C24 1.3919 (0.0017) 120.24 (0.10) H10 0.9843 (0.0145) 120.24 (0.83) 119.49 (0.83) C23 C22 C24 C24 - Distance Angles C26 1.3742 (0.0017) C23 1.3919 (0.0017) 119.47 (0.10) H11 0.9848 (0.0158) 119.37 (0.89) 121.12 (0.88) C24 C26 C23 C26 - Distance Angles C24 1.3742 (0.0017) C27 1.4097 (0.0015) 121.74 (0.11) H12 0.9800 (0.0150) 117.39 (0.85) 120.78 (0.84) C26 C24 C27 C27 - Distance Angles C26 1.4097 (0.0015) C21 1.4218 (0.0014) 119.02 (0.10) C9 1.4588 (0.0015) 120.36 (0.10) 120.48 (0.09) C27 C26 C21 C28 - Distance Angles O3 1.4408 (0.0013) H13 0.9931 (0.0158) 104.42 (0.91) H14 0.9596 (0.0155) 109.66 (0.87) 111.97 (1.23) H15 0.9744 (0.0148) 110.17 (0.83) 109.65 (1.21) 110.80 (1.20) C28 O3 H13 H14 C29 - Distance Angles O5 1.4345 (0.0015) H16 0.9815 (0.0145) 110.53 (0.82) H17 0.9779 (0.0146) 110.69 (0.81) 111.24 (1.16) H18 0.9900 (0.0154) 104.63 (0.87) 109.59 (1.18) 109.95 (1.20) C29 O5 H16 H17 C1A_1^a - Distance Angles C2A_1^a 1.3826 (0.0021) C6A_1^a 1.3889 (0.0019) 121.00 (0.14) H1A_1^a 0.9500 119.50 119.50 C1A_1^a C2A_1^a C6A_1^a C2A_1^a - Distance Angles C3A_1^a 1.3819 (0.0023) C1A_1^a 1.3826 (0.0021) 120.53 (0.14) H2A_1^a 0.9500 119.73 119.73 C2A_1^a C3A_1^a C1A_1^a C3A_1^a - Distance Angles C2A_1^a 1.3819 (0.0023) C4A_1^a 1.3891 (0.0026) 119.22 (0.15) H3A_1^a 0.9500 120.39 120.39 C3A_1^a C2A_1^a C4A_1^a C4A_1^a - Distance Angles C5A_1^a 1.3876 (0.0026) C3A_1^a 1.3891 (0.0025) 119.90 (0.14) H4A_1^a 0.9500 120.05 120.05 C4A_1^a C5A_1^a C3A_1^a C5A_1^a - Distance Angles C4A_1^a 1.3876 (0.0026) C6A_1^a 1.3885 (0.0021) 121.23 (0.15) H5A_1^a 0.9500 119.39 119.39 C5A_1^a C4A_1^a C6A_1^a C6A_1^a - Distance Angles C5A_1^a 1.3885 (0.0021) C1A_1^a 1.3889 (0.0019) 118.10 (0.14) C7A_1^a 1.5026 (0.0021) 121.49 (0.14) 120.39 (0.13) C6A_1^a C5A_1^a C1A_1^a C7A_1^a - Distance Angles C6A_1^a 1.5026 (0.0021) H7A_1^a 0.9800 109.47 H7B_1^a 0.9800 109.47 109.47 H7C_1^a 0.9800 109.47 109.47 109.47 C7A_1^a C6A_1^a H7A_1^a H7B_1^a C1B_1^b - Distance Angles C2B_1^b 1.3900 C6B_1^b 1.3900 120.00 H1B_1^b 0.9500 120.00 120.00 C1B_1^b C2B_1^b C6B_1^b C2B_1^b - Distance Angles C1B_1^b 1.3900 C3B_1^b 1.3900 120.00 H2B_1^b 0.9500 120.00 120.00 C2B_1^b C1B_1^b C3B_1^b C3B_1^b - Distance Angles C4B_1^b 1.3900 C2B_1^b 1.3900 120.00 H3B_1^b 0.9500 120.00 120.00 C3B_1^b C4B_1^b C2B_1^b C4B_1^b - Distance Angles C5B_1^b 1.3900 C3B_1^b 1.3900 120.00 H4B_1^b 0.9500 120.00 120.00 C4B_1^b C5B_1^b C3B_1^b C5B_1^b - Distance Angles C4B_1^b 1.3900 C6B_1^b 1.3900 120.00 H5B_1^b 0.9500 120.00 120.00 C5B_1^b C4B_1^b C6B_1^b C6B_1^b - Distance Angles C5B_1^b 1.3900 C1B_1^b 1.3900 120.00 C7B_1^b 1.3902 (0.0191) 120.11 (1.06) 119.86 (1.07) C6B_1^b C5B_1^b C1B_1^b C7B_1^b - Distance Angles C6B_1^b 1.3902 (0.0191) H7D_1^b 0.9800 109.47 H7E_1^b 0.9800 109.47 109.47 H7F_1^b 0.9800 109.47 109.47 109.47 C7B_1^b C6B_1^b H7D_1^b H7E_1^b Selected torsion angles 61.95 ( 0.10) C13 - O1 - C1 - O2 -179.41 ( 0.08) C13 - O1 - C1 - C2 -55.82 ( 0.11) C13 - O1 - C1 - C6 -1.52 ( 0.15) C28 - O3 - C2 - C3 -173.93 ( 0.09) C28 - O3 - C2 - C1 72.62 ( 0.10) O2 - C1 - C2 - O3 -46.63 ( 0.11) O1 - C1 - C2 - O3 -168.43 ( 0.08) C6 - C1 - C2 - O3 -100.27 ( 0.11) O2 - C1 - C2 - C3 140.48 ( 0.10) O1 - C1 - C2 - C3 18.68 ( 0.14) C6 - C1 - C2 - C3 -173.62 ( 0.10) O3 - C2 - C3 - C4 -1.88 ( 0.16) C1 - C2 - C3 - C4 162.84 ( 0.11) C2 - C3 - C4 - O4 -16.34 ( 0.15) C2 - C3 - C4 - C5 -163.20 ( 0.10) O4 - C4 - C5 - C6 15.96 ( 0.14) C3 - C4 - C5 - C6 17.01 ( 0.16) O4 - C4 - C5 - C14 -163.84 ( 0.10) C3 - C4 - C5 - C14 -4.99 ( 0.15) C14 - C5 - C6 - C7 175.21 ( 0.09) C4 - C5 - C6 - C7 -178.18 ( 0.09) C14 - C5 - C6 - C1 2.02 ( 0.15) C4 - C5 - C6 - C1 101.41 ( 0.11) O2 - C1 - C6 - C5 -138.97 ( 0.10) O1 - C1 - C6 - C5 -18.74 ( 0.14) C2 - C1 - C6 - C5 -72.23 ( 0.11) O2 - C1 - C6 - C7 47.39 ( 0.11) O1 - C1 - C6 - C7 167.62 ( 0.08) C2 - C1 - C6 - C7 -7.97 ( 0.15) C5 - C6 - C7 - C20 165.76 ( 0.09) C1 - C6 - C7 - C20 171.64 ( 0.09) C5 - C6 - C7 - C8 -14.63 ( 0.13) C1 - C6 - C7 - C8 168.70 ( 0.09) C20 - C7 - C8 - C13 -10.92 ( 0.14) C6 - C7 - C8 - C13 -6.61 ( 0.15) C20 - C7 - C8 - C9 173.78 ( 0.09) C6 - C7 - C8 - C9 0.42 ( 0.15) C13 - C8 - C9 - C10 175.71 ( 0.09) C7 - C8 - C9 - C10 176.99 ( 0.09) C13 - C8 - C9 - C27 -7.72 ( 0.15) C7 - C8 - C9 - C27 -0.63 ( 0.16) C8 - C9 - C10 - C11 -176.97 ( 0.10) C27 - C9 - C10 - C11 0.15 ( 0.17) C9 - C10 - C11 - C12 0.55 ( 0.17) C10 - C11 - C12 - C13 -178.61 ( 0.09) C11 - C12 - C13 - O1 -0.76 ( 0.16) C11 - C12 - C13 - C8 -150.21 ( 0.10) C1 - O1 - C13 - C12 31.92 ( 0.13) C1 - O1 - C13 - C8 0.28 ( 0.16) C9 - C8 - C13 - C12 -175.09 ( 0.09) C7 - C8 - C13 - C12 178.09 ( 0.09) C9 - C8 - C13 - O1 2.71 ( 0.15) C7 - C8 - C13 - O1 -168.99 ( 0.10) C6 - C5 - C14 - C15 10.80 ( 0.16) C4 - C5 - C14 - C15 8.63 ( 0.15) C6 - C5 - C14 - C19 -171.57 ( 0.09) C4 - C5 - C14 - C19 1.24 ( 0.16) C19 - C14 - C15 - C16 178.89 ( 0.11) C5 - C14 - C15 - C16 -1.55 ( 0.18) C14 - C15 - C16 - C17 8.61 ( 0.15) C29 - O5 - C17 - C18 -172.42 ( 0.10) C29 - O5 - C17 - C16 179.86 ( 0.10) C15 - C16 - C17 - O5 -1.12 ( 0.17) C15 - C16 - C17 - C18 -176.99 ( 0.10) O5 - C17 - C18 - C19 4.08 ( 0.16) C16 - C17 - C18 - C19 -4.29 ( 0.15) C17 - C18 - C19 - C14 179.49 ( 0.10) C17 - C18 - C19 - C20 1.63 ( 0.15) C15 - C14 - C19 - C18 -176.09 ( 0.09) C5 - C14 - C19 - C18 177.91 ( 0.09) C15 - C14 - C19 - C20 0.19 ( 0.15) C5 - C14 - C19 - C20 16.52 ( 0.14) C6 - C7 - C20 - C19 -163.09 ( 0.09) C8 - C7 - C20 - C19 -161.90 ( 0.09) C6 - C7 - C20 - C21 18.49 ( 0.14) C8 - C7 - C20 - C21 163.57 ( 0.10) C18 - C19 - C20 - C7 -12.59 ( 0.14) C14 - C19 - C20 - C7 -18.16 ( 0.15) C18 - C19 - C20 - C21 165.68 ( 0.10) C14 - C19 - C20 - C21 156.12 ( 0.10) C7 - C20 - C21 - C22 -22.16 ( 0.16) C19 - C20 - C21 - C22 -16.44 ( 0.14) C7 - C20 - C21 - C27 165.29 ( 0.10) C19 - C20 - C21 - C27 -4.74 ( 0.16) C27 - C21 - C22 - C23 -177.44 ( 0.10) C20 - C21 - C22 - C23 0.58 ( 0.17) C21 - C22 - C23 - C24 2.88 ( 0.17) C22 - C23 - C24 - C26 -2.03 ( 0.18) C23 - C24 - C26 - C27 -2.22 ( 0.17) C24 - C26 - C27 - C21 173.56 ( 0.10) C24 - C26 - C27 - C9 5.46 ( 0.15) C22 - C21 - C27 - C26 178.35 ( 0.09) C20 - C21 - C27 - C26 -170.31 ( 0.10) C22 - C21 - C27 - C9 2.58 ( 0.15) C20 - C21 - C27 - C9 10.13 ( 0.16) C10 - C9 - C27 - C26 -166.25 ( 0.10) C8 - C9 - C27 - C26 -174.16 ( 0.10) C10 - C9 - C27 - C21 9.46 ( 0.15) C8 - C9 - C27 - C21 -0.57 ( 0.24) C6A_1^a - C1A_1^a - C2A_1^a - C3A_1^a -0.04 ( 0.24) C1A_1^a - C2A_1^a - C3A_1^a - C4A_1^a 0.21 ( 0.24) C2A_1^a - C3A_1^a - C4A_1^a - C5A_1^a 0.23 ( 0.25) C3A_1^a - C4A_1^a - C5A_1^a - C6A_1^a -0.82 ( 0.23) C4A_1^a - C5A_1^a - C6A_1^a - C1A_1^a 177.48 ( 0.15) C4A_1^a - C5A_1^a - C6A_1^a - C7A_1^a 0.98 ( 0.22) C2A_1^a - C1A_1^a - C6A_1^a - C5A_1^a -177.33 ( 0.14) C2A_1^a - C1A_1^a - C6A_1^a - C7A_1^a 0.00 C6B_1^b - C1B_1^b - C2B_1^b - C3B_1^b 0.00 C1B_1^b - C2B_1^b - C3B_1^b - C4B_1^b 0.00 C2B_1^b - C3B_1^b - C4B_1^b - C5B_1^b 0.00 C3B_1^b - C4B_1^b - C5B_1^b - C6B_1^b 0.00 C4B_1^b - C5B_1^b - C6B_1^b - C1B_1^b -177.84 ( 1.12) C4B_1^b - C5B_1^b - C6B_1^b - C7B_1^b 0.00 C2B_1^b - C1B_1^b - C6B_1^b - C5B_1^b 177.85 ( 1.11) C2B_1^b - C1B_1^b - C6B_1^b - C7B_1^b Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.895(18) 1.983(19) 2.8143(11) 153.9(16) O2-H1...O4_$1 FMAP and GRID set by program FMAP 2 1 24 GRID -1.190 -2 -1 1.190 2 1 R1 = 0.0377 for 5111 unique reflections after merging for Fourier Residue reliability criteria (side-chain) Residue Mean(DD) Min(DD) Max(Peak) Mean(U) Max(U) Mean(Anis) Min(Anis) Max(SIMU) Max(BUMP) Sum(occ) N(ats) TolU_1 -0.02 -0.18 0.20 0.034 0.040 0.498 0.381 0.000 0.000 7.000 14 Electron density synthesis with coefficients Fo-Fc Highest peak 0.29 at 0.1521 0.9232 0.2559 [ 0.70 A from C6 ] Deepest hole -0.23 at 0.1683 -0.0039 0.2622 [ 0.75 A from C1 ] Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including eq.) Q1 1 0.3479 0.4232 0.2440 1.00000 0.05 0.29 0.70 C6 0.81 C1 1.82 C5 1.84 O2 Q2 1 0.4673 0.3368 0.3295 1.00000 0.05 0.28 0.71 C14 0.73 C19 1.87 C15 1.88 C5 Q3 1 0.4648 0.5597 0.3500 1.00000 0.05 0.25 0.72 C21 0.75 C20 1.86 C7 1.88 C27 Q4 1 0.3719 0.2556 0.2670 1.00000 0.05 0.24 0.73 C5 0.77 C4 1.80 O4 1.81 C6 Q5 1 0.4708 0.4450 0.3372 1.00000 0.05 0.24 0.72 C19 0.74 C20 1.84 C7 1.89 C14 Shortest distances between peaks (including symmetry equivalents) 2 5 1.24 3 5 1.33 1 4 2.02 2 4 2.52 2 3 2.56 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 and DANG restraints 0.00: Analyse SAME, SADI and NCSY restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU and RIGU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Analyse electron density 0.00: Analyse other restraints etc. 1.25: Read intensity data, sort/merge etc. 0.08: Set up constraints 0.15: OSF, H-atoms from difference map 1.49: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.57: Structure factors and derivatives 0.70: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.21: Solve l.s. equations 0.00: Generate HTAB table 0.21: Other dependent quantities, CIF, tables 0.34: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.01: Peaksearch 0.00: Analyse peaklist ** WARNING: These times are only approximate for multiple threads. To get better estimates run with -t1 ** Please cite: G.M. Sheldrick (2015) "Crystal structure refinement with SHELXL", Acta Cryst., C71, 3-8 (Open Access) if SHELXL proves useful. +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + marc004a finished at 10:39:25 Total elapsed time: 5.19 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++