++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXTL XLMP CRYSTAL STRUCTURE REFINEMENT - MULTI-CPU VERSION + + Copyright(c) Bruker AXS Inc. 1993-2018 Version 2018/3 + + neal054_d started at 16:35:01 on 18-Oct-2021 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Command line parameters: neal054_d -a50000 -b3000 -c624 -g0 -m0 -t12 -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 12 threads on 12 processors TITL neal054_d.res in P2(1) REM Old TITL neal054 in P2(1) REM SHELXT solution in P2(1) REM R1 0.098, Rweak 0.039, Alpha 0.221, Orientation as input REM Flack x = 0.134 ( 0.017 ) from Parsons' quotients REM Formula found by SHELXT: C18 N4 O6 I CELL 1.54178 6.252 11.7415 13.0366 90 96.74 90 ZERR 2 0.0004 0.0007 0.0007 0 0.002 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H N O I UNIT 34 46 4 8 2 V = 950.38 F(000) = 448.0 Mu = 13.43 mm-1 Cell Wt = 892.55 Rho = 1.559 L.S. 20 PLAN 5 SIZE 0.028 0.099 0.172 TEMP -173.15 CONF BOND $H LIST 6 fmap 2 MORE -1 WGHT 0.0993 0.2501 FVAR 0.57939 REM REM REM I1 5 1.07196 0.20812 -0.02950 11.00000 0.04176 0.03809 0.02668 = -0.00942 0.00154 0.00789 O3 4 0.59811 0.42745 0.56120 11.00000 0.02070 0.01431 0.02327 = -0.00211 0.00588 0.00671 N1 3 0.07755 0.76993 0.48961 11.00000 0.01986 0.01365 0.02591 = -0.00585 0.00580 -0.00092 AFIX 43 H1 2 0.17724 0.82319 0.49376 11.00000 -1.20000 AFIX 0 O1 4 -0.00697 0.58851 0.43809 11.00000 0.01902 0.02163 0.04280 = -0.00757 0.00253 -0.00169 O2 4 0.44227 0.59315 0.60556 11.00000 0.02683 0.01394 0.01959 = -0.00157 0.00375 0.00561 O4 4 0.47990 0.55059 0.16913 11.00000 0.03164 0.03542 0.01580 = -0.00421 0.00287 0.00112 C5 1 0.52188 0.58775 0.27369 11.00000 0.02898 0.01859 0.01371 = 0.00057 0.00518 -0.00835 AFIX 13 H5 2 0.65964 0.63179 0.28382 11.00000 -1.20000 AFIX 0 C4 1 0.33709 0.66248 0.29424 11.00000 0.02192 0.02416 0.02135 = -0.00058 -0.00289 0.00111 AFIX 23 H4a 2 0.19856 0.63120 0.26153 11.00000 -1.20000 H4b 2 0.35527 0.74066 0.26817 11.00000 -1.20000 AFIX 0 C8 1 0.45371 0.56479 0.71648 11.00000 0.03464 0.02670 0.01435 = -0.00685 0.00633 -0.00153 C9 1 0.68293 0.54493 0.76323 11.00000 0.04118 0.03005 0.02599 = -0.00303 -0.00130 -0.00118 AFIX 137 H9a 2 0.73732 0.47471 0.73498 11.00000 -1.50000 H9b 2 0.68776 0.53789 0.83837 11.00000 -1.50000 H9c 2 0.77267 0.60928 0.74672 11.00000 -1.50000 AFIX 0 C11 1 0.35823 0.67004 0.75923 11.00000 0.06490 0.03612 0.03381 = -0.00971 0.01444 0.01221 AFIX 137 H11a 2 0.45215 0.73542 0.75100 11.00000 -1.50000 H11b 2 0.34493 0.65877 0.83269 11.00000 -1.50000 H11c 2 0.21552 0.68436 0.72178 11.00000 -1.50000 AFIX 0 N2 3 0.44910 0.55151 0.44105 11.00000 0.01624 0.01825 0.01594 = -0.00286 0.00620 0.00246 C7 1 0.50458 0.51719 0.53916 11.00000 0.00815 0.01084 0.02446 = -0.00856 0.00384 -0.00468 C16 1 0.83072 0.45691 0.17594 11.00000 0.02618 0.02789 0.02273 = -0.00722 0.00537 -0.00734 AFIX 43 H16 2 0.88363 0.49339 0.23888 11.00000 -1.20000 AFIX 0 C10 1 0.30929 0.46070 0.72988 11.00000 0.03148 0.04035 0.02530 = 0.00414 0.01532 0.00447 AFIX 137 H10a 2 0.17359 0.46863 0.68452 11.00000 -1.50000 H10b 2 0.27920 0.45607 0.80187 11.00000 -1.50000 H10c 2 0.38325 0.39123 0.71179 11.00000 -1.50000 AFIX 0 C2 1 0.11982 0.66949 0.44973 11.00000 0.01256 0.01051 0.02829 = 0.00374 -0.00012 -0.00552 C12 1 0.54802 0.42431 0.03778 11.00000 0.04104 0.03305 0.01680 = 0.00365 -0.00021 -0.00369 AFIX 43 H12 2 0.40688 0.44016 0.00558 11.00000 -1.20000 AFIX 0 C14 1 0.88235 0.33052 0.03814 11.00000 0.02370 0.02912 0.03127 = -0.00163 0.01110 0.00646 C6 1 0.52482 0.49490 0.35317 11.00000 0.02334 0.01541 0.01853 = -0.00343 0.01015 0.00241 AFIX 23 H6a 2 0.42767 0.43167 0.32814 11.00000 -1.20000 H6b 2 0.67222 0.46457 0.37109 11.00000 -1.20000 AFIX 0 C13 1 0.67563 0.34995 -0.00663 11.00000 0.03526 0.03397 0.01464 = -0.00775 0.00643 -0.00328 AFIX 43 H13 2 0.62213 0.31147 -0.06846 11.00000 -1.20000 AFIX 0 C1 1 -0.12443 0.79449 0.52604 11.00000 0.01975 0.01739 0.06122 = 0.00006 0.01360 0.00085 AFIX 137 H1a 2 -0.23964 0.79047 0.46830 11.00000 -1.50000 H1b 2 -0.12012 0.87115 0.55596 11.00000 -1.50000 H1c 2 -0.15197 0.73870 0.57884 11.00000 -1.50000 AFIX 0 C15 1 0.96343 0.38314 0.13046 11.00000 0.02955 0.02634 0.02203 = 0.00010 0.00363 -0.01003 AFIX 43 H15 2 1.10618 0.36862 0.16124 11.00000 -1.20000 AFIX 0 C3 1 0.34695 0.66144 0.41329 11.00000 0.01426 0.01128 0.02656 = -0.00252 0.00026 0.00124 AFIX 13 H3 2 0.44001 0.72512 0.44364 11.00000 -1.20000 AFIX 0 C17 1 0.62558 0.47867 0.13271 11.00000 0.02942 0.02367 0.01567 = -0.00096 0.00533 -0.00238 HKLF 4 Covalent radii and connectivity table for neal054_d.res in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 I 1.330 I1 - C14 O3 - C7 N1 - C2 C1 O1 - C2 O2 - C7 C8 O4 - C17 C5 C5 - O4 C4 C6 C4 - C5 C3 C8 - O2 C11 C9 C10 C9 - C8 C11 - C8 N2 - C7 C6 C3 C7 - O3 O2 N2 C16 - C17 C15 C10 - C8 C2 - O1 N1 C3 C12 - C13 C17 C14 - C13 C15 I1 C6 - N2 C5 C13 - C12 C14 C1 - N1 C15 - C16 C14 C3 - N2 C4 C2 C17 - C16 O4 C12 Floating origin restraints generated 9 Systematically absent reflections rejected 3177 Reflections read, of which 9 rejected -7 =< h =< 6, -13 =< k =< 11, -15 =< l =< 14, Max. 2-theta = 127.28 0 Systematic absence violations (I>3sig(I)) before merging 0 Inconsistent equivalents 2488 Unique reflections, of which 0 suppressed R(int) = 0.0310 R(sigma) = 0.0612 Friedel opposites not merged Maximum memory for data reduction = 2805 / 25732 Reflection statistics for all twin components combined (TWST 0 set) Number of data for d > 0.860A (CIF: max) and d > 0.833A (CIF: full) (ignoring systematic absences): Unique reflections found (point group) 2488 2488 Unique reflections possible (point group) 3120 3427 Unique reflections found (Laue group) 1552 1552 Unique reflections possible (Laue group) 1646 1805 Unique Friedel pairs found 936 936 Unique Friedel pairs possible 1474 1622 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 = 56 / 3452 / 329620 wR2 = 0.137032 before cycle 1 for 2488 data and 221 / 221 parameters GooF = S = 1.088; Restrained GooF = 1.088 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0993 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57939 0.00251 -0.002 OSF Mean shift/esd = 0.002 Maximum = -0.030 for z I1 Max. shift = 0.001 A for H11C Max. dU = 0.000 for C16 Least-squares cycle 2 Maximum vector length = 623 Memory required = 56 / 3452 / 329620 wR2 = 0.137032 before cycle 2 for 2488 data and 221 / 221 parameters GooF = S = 1.088; Restrained GooF = 1.088 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0993 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57939 0.00251 0.002 OSF Mean shift/esd = 0.001 Maximum = -0.011 for z I1 Max. shift = 0.000 A for H1C Max. dU = 0.000 for C16 Least-squares cycle 3 Maximum vector length = 623 Memory required = 56 / 3452 / 329620 wR2 = 0.137032 before cycle 3 for 2488 data and 221 / 221 parameters GooF = S = 1.088; Restrained GooF = 1.088 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0993 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57939 0.00251 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for tors H1A Max. shift = 0.000 A for H1C Max. dU = 0.000 for C16 Least-squares cycle 4 Maximum vector length = 623 Memory required = 56 / 3452 / 329620 wR2 = 0.137032 before cycle 4 for 2488 data and 221 / 221 parameters GooF = S = 1.088; Restrained GooF = 1.088 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0993 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57939 0.00251 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H1A Max. shift = 0.000 A for H1B Max. dU = 0.000 for C7 Least-squares cycle 5 Maximum vector length = 623 Memory required = 56 / 3452 / 329620 wR2 = 0.137032 before cycle 5 for 2488 data and 221 / 221 parameters GooF = S = 1.088; Restrained GooF = 1.088 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0993 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57939 0.00251 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H1A Max. shift = 0.000 A for H1B Max. dU = 0.000 for C13 Least-squares cycle 6 Maximum vector length = 623 Memory required = 56 / 3452 / 329620 wR2 = 0.137032 before cycle 6 for 2488 data and 221 / 221 parameters GooF = S = 1.088; Restrained GooF = 1.088 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0993 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57939 0.00251 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H1A Max. shift = 0.000 A for H1B Max. dU = 0.000 for C10 Least-squares cycle 7 Maximum vector length = 623 Memory required = 56 / 3452 / 329620 wR2 = 0.137032 before cycle 7 for 2488 data and 221 / 221 parameters GooF = S = 1.088; Restrained GooF = 1.088 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0993 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57939 0.00251 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H1A Max. shift = 0.000 A for H1B Max. dU = 0.000 for C10 Least-squares cycle 8 Maximum vector length = 623 Memory required = 56 / 3452 / 329620 wR2 = 0.137032 before cycle 8 for 2488 data and 221 / 221 parameters GooF = S = 1.088; Restrained GooF = 1.088 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0993 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57939 0.00251 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H1A Max. shift = 0.000 A for H1B Max. dU = 0.000 for C10 Least-squares cycle 9 Maximum vector length = 623 Memory required = 56 / 3452 / 329620 wR2 = 0.137032 before cycle 9 for 2488 data and 221 / 221 parameters GooF = S = 1.088; Restrained GooF = 1.088 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0993 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57939 0.00251 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H1A Max. shift = 0.000 A for H1B Max. dU = 0.000 for C10 Least-squares cycle 10 Maximum vector length = 623 Memory required = 56 / 3452 / 329620 wR2 = 0.137032 before cycle 10 for 2488 data and 221 / 221 parameters GooF = S = 1.088; Restrained GooF = 1.088 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0993 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57939 0.00251 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H1A Max. shift = 0.000 A for H1B Max. dU = 0.000 for C10 Least-squares cycle 11 Maximum vector length = 623 Memory required = 56 / 3452 / 329620 wR2 = 0.137032 before cycle 11 for 2488 data and 221 / 221 parameters GooF = S = 1.088; Restrained GooF = 1.088 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0993 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57939 0.00251 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H1A Max. shift = 0.000 A for H1B Max. dU = 0.000 for C10 Least-squares cycle 12 Maximum vector length = 623 Memory required = 56 / 3452 / 329620 wR2 = 0.137032 before cycle 12 for 2488 data and 221 / 221 parameters GooF = S = 1.088; Restrained GooF = 1.088 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0993 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57939 0.00251 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H1A Max. shift = 0.000 A for H1B Max. dU = 0.000 for C10 Least-squares cycle 13 Maximum vector length = 623 Memory required = 56 / 3452 / 329620 wR2 = 0.137032 before cycle 13 for 2488 data and 221 / 221 parameters GooF = S = 1.088; Restrained GooF = 1.088 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0993 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57939 0.00251 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H1A Max. shift = 0.000 A for H1B Max. dU = 0.000 for C10 Least-squares cycle 14 Maximum vector length = 623 Memory required = 56 / 3452 / 329620 wR2 = 0.137032 before cycle 14 for 2488 data and 221 / 221 parameters GooF = S = 1.088; Restrained GooF = 1.088 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0993 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57939 0.00251 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H1A Max. shift = 0.000 A for H1B Max. dU = 0.000 for C10 Least-squares cycle 15 Maximum vector length = 623 Memory required = 56 / 3452 / 329620 wR2 = 0.137032 before cycle 15 for 2488 data and 221 / 221 parameters GooF = S = 1.088; Restrained GooF = 1.088 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0993 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57939 0.00251 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H1A Max. shift = 0.000 A for H1B Max. dU = 0.000 for C10 Least-squares cycle 16 Maximum vector length = 623 Memory required = 56 / 3452 / 329620 wR2 = 0.137032 before cycle 16 for 2488 data and 221 / 221 parameters GooF = S = 1.088; Restrained GooF = 1.088 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0993 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57939 0.00251 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H1A Max. shift = 0.000 A for H1B Max. dU = 0.000 for C10 Least-squares cycle 17 Maximum vector length = 623 Memory required = 56 / 3452 / 329620 wR2 = 0.137032 before cycle 17 for 2488 data and 221 / 221 parameters GooF = S = 1.088; Restrained GooF = 1.088 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0993 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57939 0.00251 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H1A Max. shift = 0.000 A for H1B Max. dU = 0.000 for C10 Least-squares cycle 18 Maximum vector length = 623 Memory required = 56 / 3452 / 329620 wR2 = 0.137032 before cycle 18 for 2488 data and 221 / 221 parameters GooF = S = 1.088; Restrained GooF = 1.088 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0993 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57939 0.00251 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H1A Max. shift = 0.000 A for H1B Max. dU = 0.000 for C10 Least-squares cycle 19 Maximum vector length = 623 Memory required = 56 / 3452 / 329620 wR2 = 0.137032 before cycle 19 for 2488 data and 221 / 221 parameters GooF = S = 1.088; Restrained GooF = 1.088 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0993 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57939 0.00251 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H1A Max. shift = 0.000 A for H1B Max. dU = 0.000 for C10 Least-squares cycle 20 Maximum vector length = 623 Memory required = 56 / 3452 / 329620 wR2 = 0.137032 before cycle 20 for 2488 data and 221 / 221 parameters GooF = S = 1.088; Restrained GooF = 1.088 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0993 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57939 0.00251 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H1A Max. shift = 0.000 A for H1B Max. dU = 0.000 for C10 Largest correlation matrix elements 0.608 U11 I1 / OSF 0.591 U22 I1 / OSF 0.584 U33 I1 / OSF Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.1772 0.8232 0.4938 43 0.880 0.000 N1 C2 C1 H5 0.6596 0.6318 0.2838 13 1.000 0.000 C5 O4 C4 C6 H4A 0.1986 0.6312 0.2615 23 0.990 0.000 C4 C5 C3 H4B 0.3553 0.7407 0.2682 23 0.990 0.000 C4 C5 C3 H9A 0.7373 0.4747 0.7350 137 0.980 0.000 C9 C8 H9A H9B 0.6877 0.5379 0.8384 137 0.980 0.000 C9 C8 H9A H9C 0.7727 0.6093 0.7467 137 0.980 0.000 C9 C8 H9A H11A 0.4522 0.7354 0.7510 137 0.980 0.000 C11 C8 H11A H11B 0.3449 0.6588 0.8327 137 0.980 0.000 C11 C8 H11A H11C 0.2156 0.6844 0.7218 137 0.980 0.000 C11 C8 H11A H16 0.8836 0.4934 0.2389 43 0.950 0.000 C16 C17 C15 H10A 0.1736 0.4686 0.6845 137 0.980 0.000 C10 C8 H10A H10B 0.2792 0.4561 0.8019 137 0.980 0.000 C10 C8 H10A H10C 0.3833 0.3912 0.7118 137 0.980 0.000 C10 C8 H10A H12 0.4069 0.4402 0.0056 43 0.950 0.000 C12 C13 C17 H6A 0.4277 0.4317 0.3281 23 0.990 0.000 C6 N2 C5 H6B 0.6722 0.4646 0.3711 23 0.990 0.000 C6 N2 C5 H13 0.6221 0.3115 -0.0685 43 0.950 0.000 C13 C12 C14 H1A -0.2396 0.7904 0.4683 137 0.980 0.000 C1 N1 H1A H1B -0.1201 0.8712 0.5559 137 0.980 0.000 C1 N1 H1A H1C -0.1519 0.7387 0.5789 137 0.980 0.000 C1 N1 H1A H15 1.1062 0.3686 0.1612 43 0.950 0.000 C15 C16 C14 H3 0.4400 0.7251 0.4436 13 1.000 0.000 C3 N2 C4 C2 neal054_d.res in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq I1 1.07196 0.20812 -0.02950 1.00000 0.04176 0.03809 0.02669 -0.00942 0.00154 0.00789 0.03571 0.00102 0.00009 0.00005 0.00004 0.00000 0.00046 0.00047 0.00040 0.00034 0.00026 0.00040 0.00030 O3 0.59812 0.42744 0.56120 1.00000 0.02070 0.01431 0.02327 -0.00211 0.00588 0.00671 0.01917 0.01300 0.00115 0.00059 0.00053 0.00000 0.00375 0.00362 0.00377 0.00285 0.00279 0.00294 0.00150 N1 0.07755 0.76993 0.48961 1.00000 0.01987 0.01365 0.02591 -0.00586 0.00580 -0.00092 0.01956 0.01746 0.00135 0.00087 0.00077 0.00000 0.00546 0.00512 0.00480 0.00388 0.00382 0.00324 0.00216 H1 0.17724 0.82319 0.49375 1.00000 0.02347 0.00000 0.00000 O1 -0.00697 0.58851 0.43809 1.00000 0.01902 0.02164 0.04281 -0.00757 0.00253 -0.00170 0.02791 0.01378 0.00115 0.00064 0.00062 0.00000 0.00359 0.00399 0.00458 0.00341 0.00340 0.00318 0.00169 O2 0.44227 0.59315 0.60556 1.00000 0.02683 0.01394 0.01959 -0.00156 0.00375 0.00562 0.02004 0.01295 0.00111 0.00058 0.00055 0.00000 0.00375 0.00340 0.00363 0.00277 0.00286 0.00294 0.00149 O4 0.47989 0.55059 0.16913 1.00000 0.03164 0.03541 0.01580 -0.00422 0.00287 0.00112 0.02761 0.01380 0.00128 0.00067 0.00058 0.00000 0.00423 0.00459 0.00365 0.00313 0.00301 0.00346 0.00175 C5 0.52188 0.58775 0.27369 1.00000 0.02899 0.01857 0.01372 0.00057 0.00520 -0.00835 0.02021 0.01794 0.00167 0.00086 0.00073 0.00000 0.00559 0.00497 0.00494 0.00384 0.00398 0.00424 0.00209 H5 0.65964 0.63179 0.28382 1.00000 0.02425 0.00000 0.00000 C4 0.33709 0.66248 0.29423 1.00000 0.02192 0.02418 0.02134 -0.00059 -0.00289 0.00111 0.02291 0.01868 0.00164 0.00093 0.00081 0.00000 0.00511 0.00499 0.00534 0.00391 0.00405 0.00413 0.00219 H4A 0.19857 0.63120 0.26152 1.00000 0.02749 0.00000 0.00000 H4B 0.35528 0.74066 0.26817 1.00000 0.02749 0.00000 0.00000 C8 0.45372 0.56479 0.71648 1.00000 0.03464 0.02671 0.01434 -0.00684 0.00634 -0.00154 0.02496 0.01898 0.00184 0.00089 0.00077 0.00000 0.00608 0.00581 0.00504 0.00400 0.00428 0.00463 0.00233 C9 0.68293 0.54493 0.76324 1.00000 0.04117 0.03005 0.02599 -0.00302 -0.00129 -0.00120 0.03282 0.02178 0.00208 0.00105 0.00094 0.00000 0.00699 0.00660 0.00597 0.00479 0.00507 0.00540 0.00272 H9A 0.73731 0.47471 0.73499 1.00000 0.04923 0.00000 0.00000 H9B 0.68774 0.53788 0.83838 1.00000 0.04923 0.00000 0.00000 H9C 0.77267 0.60928 0.74673 1.00000 0.04923 0.00000 0.00000 C11 0.35823 0.67004 0.75923 1.00000 0.06491 0.03611 0.03382 -0.00971 0.01445 0.01220 0.04426 0.02632 0.00252 0.00108 0.00101 0.00000 0.00885 0.00749 0.00699 0.00496 0.00627 0.00591 0.00333 H11A 0.45220 0.73541 0.75103 1.00000 0.06639 0.00000 0.00000 H11B 0.34487 0.65876 0.83269 1.00000 0.06639 0.00000 0.00000 H11C 0.21556 0.68438 0.72175 1.00000 0.06639 0.00000 0.00000 N2 0.44911 0.55151 0.44105 1.00000 0.01624 0.01825 0.01594 -0.00285 0.00621 0.00246 0.01647 0.01535 0.00135 0.00069 0.00064 0.00000 0.00432 0.00451 0.00411 0.00322 0.00322 0.00353 0.00178 C7 0.50458 0.51720 0.53916 1.00000 0.00814 0.01084 0.02445 -0.00855 0.00383 -0.00467 0.01432 0.01612 0.00152 0.00080 0.00073 0.00000 0.00425 0.00473 0.00555 0.00395 0.00352 0.00394 0.00199 C16 0.83071 0.45691 0.17593 1.00000 0.02618 0.02791 0.02274 -0.00722 0.00537 -0.00735 0.02541 0.01970 0.00182 0.00094 0.00086 0.00000 0.00564 0.00613 0.00551 0.00426 0.00444 0.00458 0.00237 H16 0.88363 0.49340 0.23887 1.00000 0.03049 0.00000 0.00000 C10 0.30928 0.46070 0.72988 1.00000 0.03148 0.04035 0.02529 0.00414 0.01532 0.00448 0.03142 0.02421 0.00204 0.00109 0.00092 0.00000 0.00609 0.00723 0.00587 0.00503 0.00488 0.00544 0.00269 H10A 0.17360 0.46862 0.68451 1.00000 0.04714 0.00000 0.00000 H10B 0.27917 0.45608 0.80186 1.00000 0.04714 0.00000 0.00000 H10C 0.38326 0.39123 0.71180 1.00000 0.04714 0.00000 0.00000 C2 0.11983 0.66949 0.44973 1.00000 0.01256 0.01051 0.02829 0.00374 -0.00011 -0.00552 0.01732 0.01778 0.00170 0.00083 0.00087 0.00000 0.00453 0.00506 0.00517 0.00389 0.00436 0.00364 0.00208 C12 0.54802 0.42431 0.03778 1.00000 0.04105 0.03305 0.01680 0.00366 -0.00022 -0.00369 0.03059 0.02098 0.00205 0.00100 0.00084 0.00000 0.00696 0.00594 0.00536 0.00462 0.00453 0.00535 0.00251 H12 0.40689 0.44016 0.00558 1.00000 0.03671 0.00000 0.00000 C14 0.88235 0.33053 0.03814 1.00000 0.02370 0.02911 0.03129 -0.00163 0.01111 0.00647 0.02741 0.02107 0.00180 0.00105 0.00085 0.00000 0.00545 0.00646 0.00659 0.00451 0.00464 0.00484 0.00250 C6 0.52482 0.49490 0.35317 1.00000 0.02334 0.01541 0.01852 -0.00343 0.01015 0.00242 0.01848 0.01874 0.00171 0.00084 0.00077 0.00000 0.00524 0.00520 0.00515 0.00379 0.00414 0.00415 0.00213 H6A 0.42767 0.43167 0.32814 1.00000 0.02218 0.00000 0.00000 H6B 0.67222 0.46457 0.37109 1.00000 0.02218 0.00000 0.00000 C13 0.67563 0.34995 -0.00662 1.00000 0.03525 0.03397 0.01463 -0.00776 0.00644 -0.00328 0.02767 0.01997 0.00184 0.00099 0.00079 0.00000 0.00628 0.00621 0.00514 0.00441 0.00435 0.00513 0.00241 H13 0.62212 0.31147 -0.06846 1.00000 0.03321 0.00000 0.00000 C1 -0.12442 0.79450 0.52604 1.00000 0.01975 0.01738 0.06123 0.00007 0.01361 0.00085 0.03208 0.02346 0.00192 0.00103 0.00105 0.00000 0.00557 0.00561 0.00885 0.00493 0.00515 0.00471 0.00281 H1A -0.23964 0.79044 0.46831 1.00000 0.04813 0.00000 0.00000 H1B -0.12014 0.87116 0.55593 1.00000 0.04813 0.00000 0.00000 H1C -0.15194 0.73872 0.57886 1.00000 0.04813 0.00000 0.00000 C15 0.96343 0.38314 0.13046 1.00000 0.02954 0.02633 0.02203 0.00010 0.00362 -0.01002 0.02592 0.01899 0.00180 0.00091 0.00082 0.00000 0.00582 0.00568 0.00540 0.00412 0.00437 0.00468 0.00232 H15 1.10618 0.36862 0.16124 1.00000 0.03110 0.00000 0.00000 C3 0.34695 0.66144 0.41329 1.00000 0.01426 0.01129 0.02655 -0.00253 0.00026 0.00124 0.01754 0.01743 0.00154 0.00082 0.00078 0.00000 0.00463 0.00429 0.00566 0.00374 0.00393 0.00377 0.00204 H3 0.44001 0.72512 0.44364 1.00000 0.02104 0.00000 0.00000 C17 0.62559 0.47867 0.13271 1.00000 0.02945 0.02366 0.01567 -0.00096 0.00534 -0.00238 0.02271 0.01909 0.00171 0.00091 0.00079 0.00000 0.00560 0.00518 0.00476 0.00404 0.00425 0.00464 0.00215 Final Structure Factor Calculation for neal054_d.res in P2(1) Total number of l.s. parameters = 221 Maximum vector length = 623 Memory required = 56 / 3231 / 29281 wR2 = 0.137032 before cycle 21 for 2488 data and 0 / 221 parameters GooF = S = 1.088; Restrained GooF = 1.088 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0993 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 wR2 = 0.137032, GooF = S = 1.08815, Restrained GooF = 1.08791 for all data R1 = 0.047781 for 2418 Fo > 4sig(Fo) and 0.048712 for all 2488 data Flack x = -0.015(13) by classical fit to all intensities -0.034(13) from 869 selected quotients (Parsons' method) ** Classical Flack determination preferred because s.u. lower ** Occupancy sum of asymmetric unit = 24.00 for non-hydrogen and 23.00 for H and D atoms Principal mean square atomic displacements U 0.0517 0.0345 0.0209 I1 0.0258 0.0230 0.0087 O3 0.0290 0.0185 0.0112 N1 0.0454 0.0207 0.0176 O1 0.0289 0.0200 0.0112 O2 0.0367 0.0313 0.0148 O4 0.0337 0.0158 0.0112 C5 0.0282 0.0238 0.0167 C4 0.0356 0.0287 0.0106 C8 0.0435 0.0315 0.0234 C9 0.0696 0.0445 0.0187 C11 0.0202 0.0198 0.0094 N2 0.0289 0.0100 0.0041 C7 0.0372 0.0219 0.0172 C16 0.0457 0.0342 0.0144 C10 0.0304 0.0159 0.0057 C2 0.0440 0.0318 0.0159 C12 0.0361 0.0315 0.0146 C14 0.0282 0.0184 0.0088 C6 0.0397 0.0320 0.0113 C13 0.0622 0.0179 0.0161 C1 0.0381 0.0221 0.0175 C15 0.0277 0.0143 0.0106 C3 0.0306 0.0228 0.0148 C17 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 0.053 0.081 0.106 0.128 0.153 0.180 0.211 0.255 0.319 1.000 Number in group 249. 253. 244. 250. 254. 248. 246. 246. 250. 248. GooF 0.957 1.029 1.207 1.105 1.081 1.012 1.202 1.275 0.891 1.073 K 1.083 1.027 1.032 1.020 1.020 1.023 1.018 1.001 1.010 1.012 Resolution(A) 0.86 0.91 0.96 1.01 1.08 1.15 1.24 1.37 1.56 1.98 inf Number in group 252. 249. 251. 253. 240. 252. 245. 252. 244. 250. GooF 1.051 1.081 1.038 1.189 1.144 1.097 1.110 0.903 1.077 1.169 K 1.006 1.014 1.034 1.017 1.012 1.008 1.017 1.006 1.015 1.011 R1 0.061 0.056 0.054 0.058 0.057 0.053 0.049 0.037 0.042 0.043 Recommended weighting scheme: WGHT 0.0993 0.2502 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) -3 -6 9 604.36 1562.94 6.94 0.245 1.05 -3 -4 9 1618.59 3207.78 5.35 0.352 1.15 -4 -4 9 702.66 1387.75 5.21 0.231 1.05 -3 -2 8 1556.33 3003.26 5.17 0.340 1.32 -3 -10 8 531.08 1040.01 5.11 0.200 0.89 -4 -6 9 325.27 604.99 4.54 0.153 0.97 0 0 1 686.28 1205.15 4.49 0.215 12.95 -4 -7 9 143.88 282.23 4.40 0.104 0.93 -4 -2 9 713.09 1250.80 4.37 0.220 1.10 -2 -4 8 477.76 846.09 4.32 0.181 1.34 -4 -5 9 100.98 192.67 3.77 0.086 1.01 1 -3 5 125.11 220.41 3.68 0.092 1.98 -4 -10 7 230.24 379.84 3.67 0.121 0.86 -2 -8 9 658.58 1052.56 3.61 0.201 1.00 -2 -6 9 1296.30 2036.15 3.59 0.280 1.12 -2 -7 9 201.64 346.10 3.59 0.115 1.06 0 2 7 745.53 463.77 3.54 0.134 1.76 -4 -8 8 268.97 434.83 3.47 0.129 0.93 5 -3 7 699.09 1093.36 3.47 0.205 0.95 2 0 6 2666.45 4077.78 3.47 0.396 1.68 -2 -9 8 193.30 325.05 3.44 0.112 0.99 4 -2 7 1066.33 1633.24 3.37 0.251 1.11 4 -3 7 235.90 386.90 3.35 0.122 1.08 3 -4 7 1839.59 2770.31 3.30 0.327 1.19 2 -4 0 80.13 131.61 3.18 0.071 2.13 5 -1 7 413.74 629.49 3.16 0.156 0.98 4 -5 7 297.86 467.41 3.15 0.134 1.02 4 0 7 771.15 1151.60 3.15 0.211 1.13 -2 -7 8 957.63 1411.71 3.06 0.233 1.12 -2 -6 8 912.05 1340.99 3.04 0.227 1.20 4 2 5 345.52 521.89 3.04 0.142 1.24 -1 -9 8 1123.82 1643.19 3.02 0.252 1.01 2 -6 8 709.81 1046.01 3.01 0.201 1.12 2 1 6 201.34 305.99 2.99 0.109 1.66 -2 -10 8 118.56 195.27 2.95 0.087 0.93 -3 -8 8 694.03 1013.24 2.94 0.198 1.00 -2 0 1 28.60 58.44 2.94 0.047 3.10 -3 0 3 49.45 13.20 2.87 0.023 1.96 5 1 3 943.93 1356.72 2.87 0.229 1.15 3 3 5 1150.33 1642.46 2.86 0.252 1.43 2 2 6 2547.29 3608.67 2.86 0.373 1.62 4 -1 7 181.98 282.52 2.84 0.104 1.12 3 -6 7 754.77 1085.73 2.82 0.205 1.09 -3 -2 1 265.09 164.74 2.82 0.080 1.96 -2 -5 8 472.10 678.47 2.75 0.162 1.27 0 1 2 788.13 1104.41 2.74 0.206 5.67 4 8 5 276.87 396.76 2.70 0.124 0.96 2 -7 8 142.99 224.05 2.67 0.093 1.06 -3 -11 7 242.16 348.92 2.65 0.116 0.86 2 5 6 406.59 576.38 2.63 0.149 1.37 Bond lengths and angles I1 - Distance Angles C14 2.1199 (0.0110) I1 O3 - Distance Angles C7 1.2230 (0.0123) O3 N1 - Distance Angles C2 1.3279 (0.0131) C1 1.4297 (0.0139) 122.23 (0.99) H1 0.8800 118.88 118.88 N1 C2 C1 O1 - Distance Angles C2 1.2359 (0.0127) O1 O2 - Distance Angles C7 1.3326 (0.0116) C8 1.4773 (0.0122) 120.05 (0.76) O2 C7 O4 - Distance Angles C17 1.3674 (0.0133) C5 1.4260 (0.0124) 117.74 (0.83) O4 C17 C5 - Distance Angles O4 1.4260 (0.0124) C4 1.4997 (0.0152) 106.89 (0.83) C6 1.5027 (0.0135) 115.03 (0.81) 104.40 (0.81) H5 1.0000 110.09 110.09 110.09 C5 O4 C4 C6 C4 - Distance Angles C5 1.4997 (0.0152) C3 1.5462 (0.0144) 103.52 (0.77) H4A 0.9900 111.06 111.06 H4B 0.9900 111.06 111.06 109.03 C4 C5 C3 H4A C8 - Distance Angles O2 1.4773 (0.0122) C11 1.5074 (0.0155) 101.61 (0.86) C9 1.5081 (0.0167) 111.41 (0.88) 112.09 (0.98) C10 1.5417 (0.0164) 109.14 (0.85) 110.20 (1.00) 111.90 (0.98) C8 O2 C11 C9 C9 - Distance Angles C8 1.5081 (0.0166) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 C8 H9A H9B C11 - Distance Angles C8 1.5074 (0.0155) 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 N2 - Distance Angles C7 1.3469 (0.0133) C6 1.4511 (0.0119) 122.76 (0.80) C3 1.4665 (0.0125) 123.63 (0.81) 112.42 (0.79) N2 C7 C6 C7 - Distance Angles O3 1.2230 (0.0123) O2 1.3326 (0.0116) 126.31 (0.91) N2 1.3469 (0.0133) 122.93 (0.83) 110.75 (0.81) C7 O3 O2 C16 - Distance Angles C17 1.3630 (0.0159) C15 1.3804 (0.0165) 121.59 (1.03) H16 0.9500 119.20 119.20 C16 C17 C15 C10 - Distance Angles C8 1.5417 (0.0164) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 C8 H10A H10B C2 - Distance Angles O1 1.2359 (0.0127) N1 1.3279 (0.0131) 125.25 (1.08) C3 1.5522 (0.0148) 120.81 (0.98) 113.90 (0.84) C2 O1 N1 C12 - Distance Angles C13 1.3573 (0.0173) C17 1.4260 (0.0156) 120.07 (1.10) H12 0.9500 119.97 119.97 C12 C13 C17 C14 - Distance Angles C13 1.3733 (0.0156) C15 1.3942 (0.0154) 121.46 (1.01) I1 2.1199 (0.0110) 118.69 (0.82) 119.68 (0.81) C14 C13 C15 C6 - Distance Angles N2 1.4511 (0.0119) C5 1.5027 (0.0136) 103.49 (0.77) H6A 0.9900 111.06 111.06 H6B 0.9900 111.06 111.06 109.04 C6 N2 C5 H6A C13 - Distance Angles C12 1.3573 (0.0173) C14 1.3733 (0.0156) 119.77 (1.04) H13 0.9500 120.11 120.11 C13 C12 C14 C1 - Distance Angles N1 1.4297 (0.0139) H1A 0.9800 109.47 H1B 0.9800 109.47 109.47 H1C 0.9800 109.47 109.47 109.47 C1 N1 H1A H1B C15 - Distance Angles C16 1.3804 (0.0164) C14 1.3942 (0.0154) 118.21 (1.06) H15 0.9500 120.89 120.89 C15 C16 C14 C3 - Distance Angles N2 1.4665 (0.0125) C4 1.5462 (0.0144) 102.68 (0.78) C2 1.5522 (0.0148) 111.45 (0.79) 112.13 (0.82) H3 1.0000 110.12 110.12 110.12 C3 N2 C4 C2 C17 - Distance Angles C16 1.3630 (0.0159) O4 1.3674 (0.0133) 127.23 (0.96) C12 1.4260 (0.0156) 118.85 (1.01) 113.90 (0.98) C17 C16 O4 Selected torsion angles -178.68 ( 0.84) C17 - O4 - C5 - C4 -63.30 ( 1.17) C17 - O4 - C5 - C6 159.33 ( 0.77) O4 - C5 - C4 - C3 37.02 ( 1.01) C6 - C5 - C4 - C3 -177.00 ( 0.92) C7 - O2 - C8 - C11 63.46 ( 1.18) C7 - O2 - C8 - C9 -60.61 ( 1.15) C7 - O2 - C8 - C10 -9.63 ( 1.44) C8 - O2 - C7 - O3 169.89 ( 0.86) C8 - O2 - C7 - N2 -10.21 ( 1.45) C6 - N2 - C7 - O3 -176.74 ( 0.88) C3 - N2 - C7 - O3 170.26 ( 0.87) C6 - N2 - C7 - O2 3.73 ( 1.23) C3 - N2 - C7 - O2 1.22 ( 1.79) C1 - N1 - C2 - O1 179.04 ( 1.02) C1 - N1 - C2 - C3 -152.67 ( 0.89) C7 - N2 - C6 - C5 15.22 ( 1.05) C3 - N2 - C6 - C5 -149.05 ( 0.84) O4 - C5 - C6 - N2 -32.25 ( 1.00) C4 - C5 - C6 - N2 -2.44 ( 1.70) C17 - C12 - C13 - C14 1.89 ( 1.80) C15 - C14 - C13 - C12 177.18 ( 0.87) I1 - C14 - C13 - C12 -0.03 ( 1.65) C17 - C16 - C15 - C14 -0.64 ( 1.70) C13 - C14 - C15 - C16 -175.87 ( 0.82) I1 - C14 - C15 - C16 175.15 ( 0.88) C7 - N2 - C3 - C4 7.39 ( 1.01) C6 - N2 - C3 - C4 -64.63 ( 1.19) C7 - N2 - C3 - C2 127.60 ( 0.89) C6 - N2 - C3 - C2 -27.07 ( 0.97) C5 - C4 - C3 - N2 -146.82 ( 0.83) C5 - C4 - C3 - C2 -43.52 ( 1.35) O1 - C2 - C3 - N2 138.56 ( 0.91) N1 - C2 - C3 - N2 70.96 ( 1.20) O1 - C2 - C3 - C4 -106.96 ( 1.06) N1 - C2 - C3 - C4 -179.10 ( 1.00) C15 - C16 - C17 - O4 -0.53 ( 1.64) C15 - C16 - C17 - C12 -15.78 ( 1.51) C5 - O4 - C17 - C16 165.59 ( 0.89) C5 - O4 - C17 - C12 1.78 ( 1.61) C13 - C12 - C17 - C16 -179.47 ( 1.01) C13 - C12 - C17 - O4 FMAP and GRID set by program FMAP 2 1 16 GRID -3.846 -2 -2 3.846 2 2 R1 = 0.043660 for 1552 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.75 at 0.1113 0.2071 0.0477 [ 1.01 A from I1 ] Deepest hole -1.31 at 0.0117 0.7092 0.1720 [ 1.80 A from H4A ] Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including eq.) Q1 1 1.1113 0.2071 0.0477 1.00000 0.05 1.75 1.01 I1 2.03 C14 2.41 H15 2.55 C15 Q2 1 1.0332 0.2080 -0.1065 1.00000 0.05 1.64 1.00 I1 2.51 H4A 2.63 C14 2.94 H13 Q3 1 1.2263 0.2096 -0.0335 1.00000 0.05 0.86 0.97 I1 2.83 C14 2.83 H13 2.95 H12 Q4 1 0.8687 0.2125 -0.0361 1.00000 0.05 0.72 1.26 I1 1.69 C14 1.94 H13 2.08 C13 Q5 1 1.0001 0.2062 0.1060 1.00000 0.05 0.62 1.82 C14 1.87 I1 2.12 H15 2.12 C15 Shortest distances between peaks (including symmetry equivalents) 1 5 1.09 1 3 1.35 2 3 1.45 2 4 1.46 1 4 1.76 4 5 1.94 1 2 2.01 3 4 2.23 3 5 2.43 2 5 2.80 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 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. 0.04: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.22: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.18: Structure factors and derivatives 0.13: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.07: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.00: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.00: 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. +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + neal054_d finished at 16:35:02 Total elapsed time: 0.76 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++