++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXTL XLMP CRYSTAL STRUCTURE REFINEMENT - MULTI-CPU VERSION + + Copyright(c) Bruker AXS Inc. 1993-2018 Version 2018/3 + + bilm001 started at 12:45:55 on 21-Aug-2020 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Command line parameters: bilm001 -a50000 -b3000 -c624 -g0 -m0 -t6 -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 6 threads on 6 processors TITL bilm001_a.res in P2(1)2(1)2(1) REM Old TITL bilm001 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.106, Rweak 0.021, Alpha 0.001, Orientation as input REM Flack x = 0.164 ( 0.087 ) from Parsons' quotients REM Formula found by SHELXT: C17 O2 CELL 1.54178 6.9787 12.4957 16.133 90 90 90 ZERR 4 0.0004 0.0008 0.0011 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O UNIT 72 76 4 4 V = 1406.86 F(000) = 568.0 Mu = 0.60 mm-1 Cell Wt = 1061.36 Rho = 1.253 L.S. 20 PLAN 20 SIZE 0.059 0.08 0.214 TEMP -153.16 CONF BOND $H LIST 6 MORE -1 fmap 2 acta OMIT 1 1 1 OMIT -1 -2 -3 OMIT 0 2 0 WGHT 0.0374 0.2309 FVAR 0.27295 REM REM REM O1 4 0.62182 0.32365 0.60906 11.00000 0.02786 0.02112 0.03473 = 0.00458 0.00217 0.00443 N1 3 0.64669 0.42608 0.49363 11.00000 0.02212 0.02011 0.02525 = -0.00196 0.00109 0.00332 C1 1 0.59028 0.40883 0.57403 11.00000 0.01624 0.02006 0.02673 = -0.00080 -0.00274 -0.00039 C2 1 0.49672 0.50285 0.61794 11.00000 0.01792 0.01916 0.02076 = 0.00101 -0.00125 -0.00117 C3 1 0.36308 0.56133 0.55752 11.00000 0.02082 0.02091 0.02020 = -0.00014 -0.00142 0.00408 H3 2 0.31483 0.62441 0.58671 11.00000 0.01886 C4 1 0.47484 0.59495 0.48258 11.00000 0.02047 0.02341 0.01986 = -0.00052 -0.00323 0.00105 C5 1 0.44105 0.69103 0.44145 11.00000 0.02806 0.02618 0.02357 = 0.00058 -0.00247 0.00471 H5 2 0.34427 0.73935 0.46372 11.00000 0.02541 C6 1 0.54051 0.71678 0.36943 11.00000 0.02962 0.02715 0.02485 = 0.00392 -0.00579 -0.00084 H6 2 0.51589 0.78460 0.34141 11.00000 0.03632 C7 1 0.67696 0.64652 0.33910 11.00000 0.02510 0.03204 0.02124 = 0.00045 -0.00007 -0.00476 H7 2 0.74591 0.65828 0.28812 11.00000 0.02296 C8 1 0.71647 0.55105 0.38035 11.00000 0.02158 0.02678 0.02438 = -0.00394 -0.00035 -0.00007 H8 2 0.81475 0.50197 0.35981 11.00000 0.03317 C9 1 0.61457 0.52479 0.45199 11.00000 0.02100 0.02133 0.02102 = -0.00283 -0.00351 -0.00177 C10 1 0.65302 0.57734 0.65416 11.00000 0.02262 0.02212 0.02425 = 0.00248 -0.00263 -0.00432 H10a 2 0.71657 0.62111 0.61237 11.00000 0.03099 H10b 2 0.75693 0.53063 0.67850 11.00000 0.02239 C11 1 0.54703 0.64248 0.72038 11.00000 0.03236 0.02281 0.02409 = -0.00140 -0.00386 -0.00347 H11a 2 0.63325 0.66427 0.76794 11.00000 0.02960 H11b 2 0.49177 0.70924 0.69457 11.00000 0.02846 C12 1 0.38357 0.57097 0.74835 11.00000 0.03048 0.02279 0.01971 = 0.00114 -0.00591 -0.00101 C13 1 0.38570 0.46926 0.69571 11.00000 0.02362 0.02001 0.02040 = 0.00132 0.00133 0.00088 H13 2 0.46253 0.41572 0.72452 11.00000 0.02336 C14 1 0.19173 0.42239 0.67785 11.00000 0.02344 0.02370 0.02840 = -0.00240 0.00675 -0.00259 H14 2 0.12792 0.38322 0.72369 11.00000 0.03669 C15 1 0.10744 0.43072 0.60493 11.00000 0.01784 0.03085 0.03206 = -0.00716 0.00302 -0.00155 H15 2 -0.02038 0.39593 0.59552 11.00000 0.03898 C16 1 0.19262 0.48954 0.53281 11.00000 0.01990 0.03287 0.02552 = -0.00194 -0.00315 -0.00007 H16a 2 0.23363 0.43714 0.48999 11.00000 0.02548 H16b 2 0.09563 0.53681 0.50614 11.00000 0.04029 C17 1 0.74394 0.33918 0.44919 11.00000 0.03656 0.02382 0.03111 = -0.00377 0.00490 0.00677 H17a 2 0.87672 0.35732 0.43633 11.00000 0.03843 H17b 2 0.73941 0.27661 0.48316 11.00000 0.04139 H17c 2 0.67795 0.32608 0.39570 11.00000 0.04678 C18 1 0.25610 0.59347 0.80657 11.00000 0.04494 0.03262 0.02626 = -0.00662 0.00518 -0.00621 H18a 2 0.15003 0.54152 0.82001 11.00000 0.03882 H18b 2 0.26304 0.66073 0.83707 11.00000 0.03788 HKLF 4 Covalent radii and connectivity table for bilm001_a.res in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 O1 - C1 N1 - C1 C9 C17 C1 - O1 N1 C2 C2 - C1 C13 C3 C10 C3 - C4 C2 C16 C4 - C5 C9 C3 C5 - C6 C4 C6 - C7 C5 C7 - C6 C8 C8 - C7 C9 C9 - C8 C4 N1 C10 - C11 C2 C11 - C12 C10 C12 - C18 C11 C13 C13 - C14 C12 C2 C14 - C15 C13 C15 - C14 C16 C16 - C15 C3 C17 - N1 C18 - C12 38 Systematically absent reflections rejected 10229 Reflections read, of which 41 rejected -7 =< h =< 8, -15 =< k =< 15, -19 =< l =< 20, Max. 2-theta = 150.53 0 Systematic absence violations (I>3sig(I)) before merging 4 Inconsistent equivalents 2889 Unique reflections, of which 0 suppressed R(int) = 0.0246 R(sigma) = 0.0245 Friedel opposites not merged Maximum memory for data reduction = 2662 / 28595 Reflection statistics for all twin components combined (TWST 0 set) Number of data for d > 0.797A (CIF: max) and d > 0.833A (CIF: full) (ignoring systematic absences): Unique reflections found (point group) 2889 2548 Unique reflections possible (point group) 2911 2551 Unique reflections found (Laue group) 1686 1490 Unique reflections possible (Laue group) 1693 1492 Unique Friedel pairs found 1203 1058 Unique Friedel pairs possible 1218 1059 Least-squares cycle 1 Maximum vector length = 623 Memory required = 47 / 3264 / 381924 wR2 = 0.073810 before cycle 1 for 2889 data and 257 / 257 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0374 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27295 0.00060 -0.002 OSF Mean shift/esd = 0.005 Maximum = -0.037 for z C12 Max. shift = 0.000 A for H11A Max. dU = 0.000 for H15 Least-squares cycle 2 Maximum vector length = 623 Memory required = 47 / 3264 / 381924 wR2 = 0.073809 before cycle 2 for 2889 data and 257 / 257 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0374 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27295 0.00060 0.000 OSF Mean shift/esd = 0.001 Maximum = -0.012 for z C12 Max. shift = 0.000 A for H14 Max. dU = 0.000 for H8 Least-squares cycle 3 Maximum vector length = 623 Memory required = 47 / 3264 / 381924 wR2 = 0.073809 before cycle 3 for 2889 data and 257 / 257 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0374 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27295 0.00060 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for U23 C13 Max. shift = 0.000 A for H17B Max. dU = 0.000 for H18B Least-squares cycle 4 Maximum vector length = 623 Memory required = 47 / 3264 / 381924 wR2 = 0.073809 before cycle 4 for 2889 data and 257 / 257 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0374 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27295 0.00060 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y H16A Max. shift = 0.000 A for H16A Max. dU = 0.000 for H16A Least-squares cycle 5 Maximum vector length = 623 Memory required = 47 / 3264 / 381924 wR2 = 0.073809 before cycle 5 for 2889 data and 257 / 257 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0374 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27295 0.00060 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y H16A Max. shift = 0.000 A for H16A Max. dU = 0.000 for H8 Least-squares cycle 6 Maximum vector length = 623 Memory required = 47 / 3264 / 381924 wR2 = 0.073809 before cycle 6 for 2889 data and 257 / 257 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0374 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27295 0.00060 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y H16A Max. shift = 0.000 A for H17A Max. dU = 0.000 for H16B Least-squares cycle 7 Maximum vector length = 623 Memory required = 47 / 3264 / 381924 wR2 = 0.073809 before cycle 7 for 2889 data and 257 / 257 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0374 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27295 0.00060 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y H16A Max. shift = 0.000 A for H16A Max. dU = 0.000 for H17C Least-squares cycle 8 Maximum vector length = 623 Memory required = 47 / 3264 / 381924 wR2 = 0.073809 before cycle 8 for 2889 data and 257 / 257 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0374 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27295 0.00060 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y H16A Max. shift = 0.000 A for H16A Max. dU = 0.000 for H17C Least-squares cycle 9 Maximum vector length = 623 Memory required = 47 / 3264 / 381924 wR2 = 0.073809 before cycle 9 for 2889 data and 257 / 257 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0374 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27295 0.00060 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y H16A Max. shift = 0.000 A for H17A Max. dU = 0.000 for H16B Least-squares cycle 10 Maximum vector length = 623 Memory required = 47 / 3264 / 381924 wR2 = 0.073809 before cycle 10 for 2889 data and 257 / 257 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0374 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27295 0.00060 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y H16A Max. shift = 0.000 A for H17A Max. dU = 0.000 for H17C Least-squares cycle 11 Maximum vector length = 623 Memory required = 47 / 3264 / 381924 wR2 = 0.073809 before cycle 11 for 2889 data and 257 / 257 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0374 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27295 0.00060 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y H16A Max. shift = 0.000 A for H18A Max. dU = 0.000 for H17C Least-squares cycle 12 Maximum vector length = 623 Memory required = 47 / 3264 / 381924 wR2 = 0.073809 before cycle 12 for 2889 data and 257 / 257 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0374 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27295 0.00060 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x H18A Max. shift = 0.000 A for H18A Max. dU = 0.000 for H17C Least-squares cycle 13 Maximum vector length = 623 Memory required = 47 / 3264 / 381924 wR2 = 0.073809 before cycle 13 for 2889 data and 257 / 257 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0374 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27295 0.00060 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x H18A Max. shift = 0.000 A for H18A Max. dU = 0.000 for H17C Least-squares cycle 14 Maximum vector length = 623 Memory required = 47 / 3264 / 381924 wR2 = 0.073809 before cycle 14 for 2889 data and 257 / 257 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0374 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27295 0.00060 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x H18A Max. shift = 0.000 A for H18A Max. dU = 0.000 for H17C Least-squares cycle 15 Maximum vector length = 623 Memory required = 47 / 3264 / 381924 wR2 = 0.073809 before cycle 15 for 2889 data and 257 / 257 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0374 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27295 0.00060 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x H18A Max. shift = 0.000 A for H18A Max. dU = 0.000 for H17C Least-squares cycle 16 Maximum vector length = 623 Memory required = 47 / 3264 / 381924 wR2 = 0.073809 before cycle 16 for 2889 data and 257 / 257 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0374 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27295 0.00060 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x H18A Max. shift = 0.000 A for H18A Max. dU = 0.000 for H18A Least-squares cycle 17 Maximum vector length = 623 Memory required = 47 / 3264 / 381924 wR2 = 0.073809 before cycle 17 for 2889 data and 257 / 257 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0374 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27295 0.00060 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x H18A Max. shift = 0.000 A for H18A Max. dU = 0.000 for H17C Least-squares cycle 18 Maximum vector length = 623 Memory required = 47 / 3264 / 381924 wR2 = 0.073809 before cycle 18 for 2889 data and 257 / 257 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0374 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27295 0.00060 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x H18A Max. shift = 0.000 A for H18A Max. dU = 0.000 for H18A Least-squares cycle 19 Maximum vector length = 623 Memory required = 47 / 3264 / 381924 wR2 = 0.073809 before cycle 19 for 2889 data and 257 / 257 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0374 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27295 0.00060 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x H18A Max. shift = 0.000 A for H18A Max. dU = 0.000 for H17C Least-squares cycle 20 Maximum vector length = 623 Memory required = 47 / 3264 / 381924 wR2 = 0.073809 before cycle 20 for 2889 data and 257 / 257 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0374 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27295 0.00060 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C3 Max. shift = 0.000 A for H18A Max. dU = 0.000 for H17A No correlation matrix elements larger than 0.500 bilm001_a.res in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq O1 0.62182 0.32365 0.60906 1.00000 0.02786 0.02112 0.03473 0.00458 0.00217 0.00443 0.02791 0.00219 0.00018 0.00009 0.00008 0.00000 0.00062 0.00054 0.00067 0.00046 0.00055 0.00048 0.00028 N1 0.64669 0.42608 0.49363 1.00000 0.02212 0.02011 0.02525 -0.00196 0.00109 0.00332 0.02249 0.00234 0.00020 0.00011 0.00008 0.00000 0.00066 0.00062 0.00066 0.00054 0.00057 0.00054 0.00029 C1 0.59028 0.40883 0.57403 1.00000 0.01624 0.02006 0.02673 -0.00080 -0.00274 -0.00039 0.02101 0.00262 0.00022 0.00012 0.00010 0.00000 0.00069 0.00070 0.00080 0.00061 0.00062 0.00058 0.00033 C2 0.49672 0.50285 0.61794 1.00000 0.01792 0.01916 0.02076 0.00101 -0.00125 -0.00117 0.01928 0.00262 0.00022 0.00012 0.00010 0.00000 0.00075 0.00070 0.00073 0.00057 0.00059 0.00055 0.00032 C3 0.36308 0.56133 0.55752 1.00000 0.02082 0.02091 0.02020 -0.00014 -0.00142 0.00408 0.02064 0.00268 0.00023 0.00012 0.00009 0.00000 0.00073 0.00071 0.00071 0.00058 0.00065 0.00062 0.00032 H3 0.31484 0.62441 0.58671 1.00000 0.01886 0.03275 0.00279 0.00151 0.00113 0.00000 0.00452 C4 0.47484 0.59495 0.48258 1.00000 0.02047 0.02341 0.01986 -0.00052 -0.00323 0.00105 0.02124 0.00274 0.00024 0.00013 0.00010 0.00000 0.00076 0.00074 0.00073 0.00058 0.00063 0.00062 0.00033 C5 0.44105 0.69103 0.44145 1.00000 0.02806 0.02618 0.02357 0.00058 -0.00247 0.00471 0.02593 0.00298 0.00025 0.00013 0.00011 0.00000 0.00087 0.00079 0.00080 0.00065 0.00072 0.00069 0.00036 H5 0.34427 0.73935 0.46372 1.00000 0.02541 0.03364 0.00308 0.00159 0.00120 0.00000 0.00492 C6 0.54051 0.71678 0.36943 1.00000 0.02962 0.02715 0.02485 0.00392 -0.00579 -0.00084 0.02721 0.00303 0.00027 0.00014 0.00011 0.00000 0.00086 0.00080 0.00084 0.00067 0.00073 0.00068 0.00037 H6 0.51589 0.78460 0.34141 1.00000 0.03632 0.03849 0.00348 0.00179 0.00138 0.00000 0.00569 C7 0.67696 0.64652 0.33910 1.00000 0.02510 0.03204 0.02124 0.00045 -0.00007 -0.00476 0.02613 0.00296 0.00025 0.00014 0.00011 0.00000 0.00085 0.00084 0.00079 0.00067 0.00070 0.00068 0.00036 H7 0.74591 0.65828 0.28812 1.00000 0.02296 0.03482 0.00291 0.00161 0.00124 0.00000 0.00498 C8 0.71647 0.55105 0.38035 1.00000 0.02158 0.02678 0.02438 -0.00394 -0.00035 -0.00007 0.02425 0.00280 0.00024 0.00013 0.00011 0.00000 0.00077 0.00082 0.00079 0.00066 0.00068 0.00065 0.00035 H8 0.81475 0.50197 0.35981 1.00000 0.03317 0.03659 0.00321 0.00176 0.00130 0.00000 0.00551 C9 0.61457 0.52479 0.45199 1.00000 0.02100 0.02133 0.02102 -0.00283 -0.00351 -0.00177 0.02112 0.00257 0.00023 0.00012 0.00010 0.00000 0.00076 0.00070 0.00072 0.00059 0.00066 0.00065 0.00032 C10 0.65302 0.57734 0.65416 1.00000 0.02262 0.02212 0.02425 0.00248 -0.00263 -0.00432 0.02300 0.00274 0.00024 0.00013 0.00010 0.00000 0.00078 0.00073 0.00075 0.00065 0.00066 0.00066 0.00034 H10A 0.71657 0.62111 0.61237 1.00000 0.03099 0.03695 0.00312 0.00175 0.00139 0.00000 0.00543 H10B 0.75693 0.53063 0.67850 1.00000 0.02239 0.03376 0.00286 0.00158 0.00120 0.00000 0.00478 C11 0.54703 0.64248 0.72038 1.00000 0.03236 0.02281 0.02409 -0.00140 -0.00386 -0.00347 0.02642 0.00296 0.00028 0.00013 0.00011 0.00000 0.00093 0.00077 0.00081 0.00063 0.00072 0.00072 0.00037 H11A 0.63325 0.66427 0.76795 1.00000 0.02960 0.03721 0.00320 0.00162 0.00126 0.00000 0.00507 H11B 0.49177 0.70924 0.69457 1.00000 0.02846 0.03607 0.00330 0.00161 0.00128 0.00000 0.00515 C12 0.38357 0.57097 0.74835 1.00000 0.03048 0.02279 0.01971 0.00114 -0.00591 -0.00101 0.02433 0.00279 0.00026 0.00013 0.00010 0.00000 0.00085 0.00073 0.00073 0.00062 0.00069 0.00071 0.00034 C13 0.38570 0.46926 0.69571 1.00000 0.02362 0.02001 0.02040 0.00132 0.00133 0.00088 0.02134 0.00278 0.00024 0.00012 0.00010 0.00000 0.00080 0.00067 0.00071 0.00060 0.00066 0.00065 0.00033 H13 0.46253 0.41572 0.72452 1.00000 0.02336 0.03316 0.00291 0.00161 0.00117 0.00000 0.00475 C14 0.19173 0.42239 0.67785 1.00000 0.02344 0.02370 0.02840 -0.00240 0.00675 -0.00259 0.02518 0.00295 0.00024 0.00014 0.00011 0.00000 0.00080 0.00075 0.00083 0.00065 0.00067 0.00067 0.00035 H14 0.12792 0.38322 0.72369 1.00000 0.03669 0.03735 0.00347 0.00164 0.00134 0.00000 0.00584 C15 0.10744 0.43072 0.60493 1.00000 0.01784 0.03085 0.03206 -0.00716 0.00302 -0.00155 0.02691 0.00298 0.00024 0.00014 0.00011 0.00000 0.00076 0.00082 0.00088 0.00070 0.00069 0.00069 0.00036 H15 -0.02038 0.39593 0.59552 1.00000 0.03898 0.03988 0.00348 0.00182 0.00132 0.00000 0.00602 C16 0.19262 0.48954 0.53281 1.00000 0.01990 0.03287 0.02552 -0.00194 -0.00315 -0.00007 0.02610 0.00302 0.00025 0.00015 0.00011 0.00000 0.00084 0.00086 0.00083 0.00070 0.00066 0.00071 0.00037 H16A 0.23363 0.43714 0.48999 1.00000 0.02548 0.03478 0.00297 0.00162 0.00123 0.00000 0.00498 H16B 0.09562 0.53681 0.50614 1.00000 0.04029 0.03843 0.00345 0.00177 0.00136 0.00000 0.00599 C17 0.74394 0.33918 0.44919 1.00000 0.03656 0.02382 0.03111 -0.00377 0.00490 0.00677 0.03050 0.00354 0.00029 0.00014 0.00012 0.00000 0.00105 0.00084 0.00097 0.00072 0.00082 0.00073 0.00040 H17A 0.87672 0.35732 0.43633 1.00000 0.03843 0.04035 0.00368 0.00173 0.00138 0.00000 0.00580 H17B 0.73941 0.27661 0.48316 1.00000 0.04139 0.04241 0.00353 0.00195 0.00154 0.00000 0.00650 H17C 0.67794 0.32608 0.39570 1.00000 0.04678 0.04487 0.00383 0.00192 0.00158 0.00000 0.00673 C18 0.25610 0.59347 0.80657 1.00000 0.04494 0.03262 0.02626 -0.00662 0.00518 -0.00621 0.03461 0.00343 0.00032 0.00016 0.00012 0.00000 0.00114 0.00094 0.00088 0.00076 0.00083 0.00083 0.00044 H18A 0.15003 0.54152 0.82001 1.00000 0.03882 0.04118 0.00353 0.00181 0.00140 0.00000 0.00576 H18B 0.26303 0.66073 0.83707 1.00000 0.03788 0.04063 0.00321 0.00190 0.00143 0.00000 0.00608 Final Structure Factor Calculation for bilm001_a.res in P2(1)2(1)2(1) Total number of l.s. parameters = 257 Maximum vector length = 623 Memory required = 47 / 3007 / 28035 wR2 = 0.073809 before cycle 21 for 2889 data and 0 / 257 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0374 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 wR2 = 0.073809, GooF = S = 1.06664, Restrained GooF = 1.06664 for all data R1 = 0.028778 for 2770 Fo > 4sig(Fo) and 0.030125 for all 2889 data Flack x = -0.034(307) by classical fit to all intensities 0.027(96) from 1133 selected quotients (Parsons' method) Occupancy sum of asymmetric unit = 20.00 for non-hydrogen and 19.00 for H and D atoms Principal mean square atomic displacements U 0.0374 0.0280 0.0183 O1 0.0259 0.0245 0.0170 N1 0.0275 0.0201 0.0155 C1 0.0219 0.0188 0.0171 C2 0.0252 0.0202 0.0165 C3 0.0245 0.0223 0.0169 C4 0.0322 0.0248 0.0208 C5 0.0347 0.0271 0.0198 C6 0.0345 0.0227 0.0212 C7 0.0297 0.0218 0.0212 C8 0.0248 0.0229 0.0156 C9 0.0293 0.0217 0.0180 C10 0.0345 0.0249 0.0199 C11 0.0333 0.0227 0.0170 C12 0.0245 0.0207 0.0189 C13 0.0342 0.0227 0.0186 C14 0.0391 0.0244 0.0172 C15 0.0334 0.0265 0.0184 C16 0.0406 0.0324 0.0185 C17 0.0499 0.0319 0.0220 C18 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 0.027 0.041 0.056 0.068 0.080 0.097 0.116 0.145 0.204 1.000 Number in group 298. 291. 287. 303. 265. 293. 288. 295. 278. 291. GooF 0.975 0.971 1.149 1.083 1.196 1.118 1.117 0.977 0.981 1.084 K 0.932 0.990 0.987 0.991 0.991 1.000 1.003 1.003 1.000 1.008 Resolution(A) 0.80 0.83 0.86 0.90 0.95 1.01 1.08 1.19 1.36 1.71 inf Number in group 293. 292. 284. 288. 304. 275. 290. 286. 286. 291. GooF 1.252 1.061 0.940 0.890 1.062 1.106 1.042 0.912 1.083 1.246 K 1.031 1.048 1.029 1.019 0.978 0.974 0.987 1.010 1.023 1.003 R1 0.060 0.044 0.039 0.040 0.035 0.029 0.025 0.021 0.025 0.023 Recommended weighting scheme: WGHT 0.0374 0.2309 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) 8 1 8 37.85 61.86 4.99 0.079 0.80 0 6 4 482.39 394.03 4.43 0.199 1.85 -8 5 1 58.39 83.37 4.11 0.092 0.82 0 0 8 11.81 4.92 3.98 0.022 2.02 -4 4 11 31.79 48.38 3.76 0.070 1.06 7 5 10 25.91 39.68 3.70 0.063 0.80 8 3 4 49.66 69.90 3.65 0.084 0.84 2 0 0 272.61 330.66 3.44 0.183 3.49 8 4 6 20.13 31.39 3.41 0.056 0.80 0 1 3 289.10 340.40 3.14 0.185 4.94 -3 12 11 37.31 24.89 3.07 0.050 0.80 0 12 11 27.74 19.22 3.05 0.044 0.85 -6 11 2 50.20 66.48 3.02 0.082 0.81 0 4 1 118.30 97.07 3.01 0.099 3.07 -5 8 5 17.32 25.45 2.99 0.051 0.99 0 11 7 18.44 26.58 2.92 0.052 1.02 -2 7 17 111.62 91.81 2.89 0.096 0.81 0 4 8 57.69 72.91 2.86 0.086 1.69 -2 3 7 82.84 100.43 2.84 0.101 1.75 -5 12 6 34.23 46.56 2.84 0.069 0.80 5 6 8 23.45 32.22 2.82 0.057 1.01 5 6 2 37.73 48.82 2.82 0.070 1.15 5 0 1 630.52 556.01 2.78 0.237 1.39 5 5 2 24.41 17.35 2.77 0.042 1.20 -2 6 4 488.03 429.43 2.76 0.208 1.63 0 6 18 140.15 118.47 2.75 0.109 0.82 4 0 17 14.09 22.27 2.74 0.047 0.83 0 7 8 138.83 117.91 2.71 0.109 1.34 -1 7 16 121.79 98.75 2.71 0.100 0.87 4 1 17 3.09 7.80 2.69 0.028 0.83 2 3 7 84.16 100.86 2.69 0.101 1.75 4 4 11 38.75 49.37 2.67 0.071 1.06 4 4 12 152.56 177.80 2.63 0.134 1.01 -3 5 5 396.94 350.02 2.62 0.188 1.51 -4 8 5 45.06 56.36 2.62 0.075 1.09 0 1 12 3.54 7.16 2.61 0.027 1.34 3 0 3 25.57 33.52 2.61 0.058 2.14 1 3 9 42.78 53.57 2.60 0.074 1.60 -1 8 9 23.91 32.40 2.59 0.057 1.16 5 8 12 20.59 13.70 2.59 0.037 0.82 -5 8 12 23.14 13.56 2.57 0.037 0.82 0 12 12 84.79 70.13 2.55 0.084 0.82 3 0 7 102.08 120.23 2.55 0.110 1.64 -5 3 16 29.26 20.97 2.53 0.046 0.80 -2 10 8 440.31 503.11 2.52 0.225 1.02 6 11 0 366.40 308.66 2.52 0.177 0.81 -4 12 7 51.98 41.37 2.50 0.065 0.83 3 8 11 29.31 37.89 2.50 0.062 0.97 -1 10 7 151.60 174.98 2.48 0.133 1.09 5 4 10 47.92 59.10 2.47 0.077 1.00 Bond lengths and angles O1 - Distance Angles C1 1.2250 (0.0020) O1 N1 - Distance Angles C1 1.3726 (0.0021) C9 1.4222 (0.0020) 122.50 (0.13) C17 1.4676 (0.0021) 118.56 (0.14) 118.94 (0.14) N1 C1 C9 C1 - Distance Angles O1 1.2250 (0.0020) N1 1.3726 (0.0021) 121.39 (0.15) C2 1.5192 (0.0021) 122.28 (0.15) 116.26 (0.13) C1 O1 N1 C2 - Distance Angles C1 1.5192 (0.0021) C13 1.5333 (0.0022) 112.77 (0.13) C3 1.5342 (0.0021) 109.48 (0.13) 110.07 (0.13) C10 1.5485 (0.0021) 109.76 (0.13) 102.22 (0.12) 112.43 (0.12) C2 C1 C13 C3 C3 - Distance Angles C4 1.4988 (0.0022) C2 1.5342 (0.0021) 109.25 (0.13) C16 1.5423 (0.0023) 110.85 (0.13) 110.86 (0.13) H3 0.9780 (0.0192) 109.97 (1.09) 106.69 (1.08) 109.13 (1.15) C3 C4 C2 C16 C4 - Distance Angles C5 1.3919 (0.0022) C9 1.4011 (0.0022) 119.32 (0.15) C3 1.4988 (0.0022) 122.56 (0.15) 118.09 (0.14) C4 C5 C9 C5 - Distance Angles C6 1.3912 (0.0025) C4 1.3919 (0.0022) 120.87 (0.16) H5 0.9746 (0.0212) 120.69 (1.17) 118.43 (1.18) C5 C6 C4 C6 - Distance Angles C7 1.3846 (0.0026) C5 1.3912 (0.0025) 119.45 (0.16) H6 0.9757 (0.0228) 120.54 (1.40) 120.00 (1.39) C6 C7 C5 C7 - Distance Angles C6 1.3846 (0.0026) C8 1.3936 (0.0024) 120.67 (0.16) H7 0.9641 (0.0205) 123.23 (1.19) 116.05 (1.20) C7 C6 C8 C8 - Distance Angles C7 1.3936 (0.0024) C9 1.3961 (0.0023) 119.72 (0.16) H8 0.9779 (0.0230) 120.91 (1.25) 119.37 (1.25) C8 C7 C9 C9 - Distance Angles C8 1.3961 (0.0023) C4 1.4011 (0.0022) 119.93 (0.14) N1 1.4222 (0.0020) 120.96 (0.14) 119.08 (0.14) C9 C8 C4 C10 - Distance Angles C11 1.5333 (0.0024) C2 1.5485 (0.0021) 104.02 (0.13) H10A 0.9748 (0.0232) 113.80 (1.26) 113.37 (1.28) H10B 1.0103 (0.0204) 112.47 (1.12) 107.75 (1.12) 105.45 (1.68) C10 C11 C2 H10A C11 - Distance Angles C12 1.5177 (0.0024) C10 1.5333 (0.0024) 104.90 (0.13) H11A 1.0124 (0.0213) 112.31 (1.21) 112.59 (1.22) H11B 1.0089 (0.0211) 108.80 (1.29) 109.62 (1.20) 108.52 (1.64) C11 C12 C10 H11A C12 - Distance Angles C18 1.3239 (0.0026) C11 1.5177 (0.0024) 126.22 (0.16) C13 1.5285 (0.0021) 125.26 (0.16) 108.49 (0.14) C12 C18 C11 C13 - Distance Angles C14 1.5028 (0.0023) C12 1.5285 (0.0021) 114.95 (0.14) C2 1.5333 (0.0022) 113.88 (0.13) 103.41 (0.12) H13 0.9753 (0.0205) 108.61 (1.17) 108.12 (1.14) 107.45 (1.17) C13 C14 C12 C2 C14 - Distance Angles C15 1.3194 (0.0025) C13 1.5028 (0.0023) 122.81 (0.16) H14 0.9924 (0.0225) 120.22 (1.35) 116.97 (1.34) C14 C15 C13 C15 - Distance Angles C14 1.3194 (0.0025) C16 1.4991 (0.0025) 123.63 (0.16) H15 1.0038 (0.0242) 119.80 (1.27) 116.57 (1.26) C15 C14 C16 C16 - Distance Angles C15 1.4991 (0.0025) C3 1.5423 (0.0023) 112.98 (0.14) H16A 0.9940 (0.0205) 109.31 (1.17) 109.92 (1.21) H16B 0.9961 (0.0236) 110.88 (1.33) 106.91 (1.31) 106.62 (1.69) C16 C15 C3 H16A C17 - Distance Angles N1 1.4676 (0.0021) H17A 0.9763 (0.0254) 111.77 (1.31) H17B 0.9554 (0.0241) 108.06 (1.50) 110.08 (1.99) H17C 0.9918 (0.0258) 109.42 (1.47) 107.11 (1.96) 110.41 (1.97) C17 N1 H17A H17B C18 - Distance Angles C12 1.3239 (0.0026) H18A 1.0082 (0.0244) 120.61 (1.30) H18B 0.9751 (0.0240) 120.52 (1.38) 118.87 (1.93) C18 C12 H18A Selected torsion angles -178.97 ( 0.15) C9 - N1 - C1 - O1 0.98 ( 0.23) C17 - N1 - C1 - O1 -2.05 ( 0.22) C9 - N1 - C1 - C2 177.90 ( 0.14) C17 - N1 - C1 - C2 -20.28 ( 0.21) O1 - C1 - C2 - C13 162.83 ( 0.14) N1 - C1 - C2 - C13 -143.18 ( 0.15) O1 - C1 - C2 - C3 39.93 ( 0.18) N1 - C1 - C2 - C3 92.97 ( 0.18) O1 - C1 - C2 - C10 -83.92 ( 0.16) N1 - C1 - C2 - C10 -56.38 ( 0.16) C1 - C2 - C3 - C4 179.13 ( 0.13) C13 - C2 - C3 - C4 65.89 ( 0.16) C10 - C2 - C3 - C4 66.06 ( 0.16) C1 - C2 - C3 - C16 -58.43 ( 0.17) C13 - C2 - C3 - C16 -171.67 ( 0.13) C10 - C2 - C3 - C16 -143.46 ( 0.15) C2 - C3 - C4 - C5 94.10 ( 0.18) C16 - C3 - C4 - C5 38.42 ( 0.19) C2 - C3 - C4 - C9 -84.03 ( 0.17) C16 - C3 - C4 - C9 1.68 ( 0.25) C9 - C4 - C5 - C6 -176.42 ( 0.16) C3 - C4 - C5 - C6 -1.01 ( 0.26) C4 - C5 - C6 - C7 -0.55 ( 0.26) C5 - C6 - C7 - C8 1.41 ( 0.25) C6 - C7 - C8 - C9 -0.73 ( 0.23) C7 - C8 - C9 - C4 177.61 ( 0.15) C7 - C8 - C9 - N1 -0.80 ( 0.23) C5 - C4 - C9 - C8 177.39 ( 0.14) C3 - C4 - C9 - C8 -179.17 ( 0.15) C5 - C4 - C9 - N1 -0.98 ( 0.21) C3 - C4 - C9 - N1 162.28 ( 0.15) C1 - N1 - C9 - C8 -17.67 ( 0.23) C17 - N1 - C9 - C8 -19.37 ( 0.22) C1 - N1 - C9 - C4 160.68 ( 0.15) C17 - N1 - C9 - C4 -160.51 ( 0.13) C1 - C2 - C10 - C11 -40.60 ( 0.15) C13 - C2 - C10 - C11 77.38 ( 0.16) C3 - C2 - C10 - C11 27.25 ( 0.16) C2 - C10 - C11 - C12 178.37 ( 0.18) C10 - C11 - C12 - C18 -3.61 ( 0.17) C10 - C11 - C12 - C13 31.70 ( 0.24) C18 - C12 - C13 - C14 -146.34 ( 0.15) C11 - C12 - C13 - C14 156.45 ( 0.17) C18 - C12 - C13 - C2 -21.59 ( 0.17) C11 - C12 - C13 - C2 -79.03 ( 0.16) C1 - C2 - C13 - C14 43.54 ( 0.17) C3 - C2 - C13 - C14 163.19 ( 0.13) C10 - C2 - C13 - C14 155.52 ( 0.13) C1 - C2 - C13 - C12 -81.91 ( 0.15) C3 - C2 - C13 - C12 37.75 ( 0.15) C10 - C2 - C13 - C12 104.97 ( 0.18) C12 - C13 - C14 - C15 -14.10 ( 0.22) C2 - C13 - C14 - C15 -1.47 ( 0.26) C13 - C14 - C15 - C16 -13.70 ( 0.25) C14 - C15 - C16 - C3 164.96 ( 0.14) C4 - C3 - C16 - C15 43.45 ( 0.19) C2 - C3 - C16 - C15 FMAP and GRID set by program FMAP 2 1 11 GRID -3.125 -2 -2 3.125 2 2 R1 = 0.029572 for 1686 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.16 at 0.0817 0.4233 0.0188 [ 0.74 A from C4 ] Deepest hole -0.16 at 0.2470 0.5183 0.4992 [ 0.75 A from C16 ] Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including eq.) Q1 1 0.4183 0.5767 0.5188 1.00000 0.05 0.16 0.74 C4 0.76 C3 1.44 H3 1.86 C9 Q2 1 0.3670 0.5201 0.7223 1.00000 0.05 0.16 0.77 C12 0.78 C13 1.47 H13 1.81 C18 Q3 1 0.4336 0.5255 0.5862 1.00000 0.05 0.16 0.73 C2 0.81 C3 1.49 H3 1.83 C1 Q4 1 0.5481 0.4637 0.5971 1.00000 0.05 0.15 0.69 C2 0.83 C1 1.83 O1 1.84 C10 Q5 1 0.3779 0.5622 0.7929 1.00000 0.05 0.15 0.73 C12 0.96 C18 1.63 H18B 1.67 H18A Q6 1 0.5873 0.5341 0.6352 1.00000 0.05 0.13 0.77 C10 0.79 C2 1.38 H10B 1.46 H10A Q7 1 0.2948 0.4404 0.6808 1.00000 0.05 0.13 0.76 C14 0.77 C13 1.40 H13 1.53 H14 Q8 1 0.5654 0.5663 0.4750 1.00000 0.05 0.13 0.72 C9 0.74 C4 1.86 C5 1.87 C8 Q9 1 0.4411 0.4846 0.6552 1.00000 0.05 0.13 0.75 C2 0.78 C13 1.42 H13 1.88 C10 Q10 1 0.1219 0.4633 0.6512 1.00000 0.05 0.12 0.83 C14 0.86 C15 1.54 H14 1.58 H15 Q11 1 0.4643 0.6035 0.7425 1.00000 0.05 0.11 0.70 C12 0.84 C11 1.46 H11A 1.54 H11B Q12 1 0.1503 0.4619 0.5679 1.00000 0.05 0.11 0.73 C16 0.77 C15 1.42 H16A 1.42 H16B Q13 1 0.2722 0.5285 0.5446 1.00000 0.05 0.11 0.76 C16 0.78 C3 1.38 H16B 1.41 H3 Q14 1 0.6318 0.5140 0.4051 1.00000 0.05 0.11 0.78 C9 0.85 C8 1.48 H8 1.80 N1 Q15 1 0.6808 0.5878 0.3562 1.00000 0.05 0.10 0.65 C8 0.78 C7 1.42 H8 1.48 H7 Q16 1 0.6482 0.4760 0.4794 1.00000 0.05 0.10 0.66 N1 0.79 C9 1.79 C1 1.90 C17 Q17 1 0.4489 0.6354 0.4563 1.00000 0.05 0.10 0.68 C4 0.74 C5 1.50 H5 1.80 C9 Q18 1 0.7463 0.6213 0.3791 1.00000 0.05 0.10 0.87 C7 0.90 C8 1.54 H7 1.60 H8 Q19 1 0.6591 0.5383 0.4201 1.00000 0.05 0.10 0.62 C9 0.77 C8 1.53 H8 1.78 C4 Q20 1 0.6004 0.4170 0.5235 1.00000 0.05 0.09 0.59 N1 0.82 C1 1.78 C9 1.81 O1 Shortest distances between peaks (including symmetry equivalents) 14 19 0.43 15 18 0.72 16 20 1.08 4 6 1.11 3 4 1.12 5 11 1.14 8 19 1.15 15 19 1.21 8 17 1.22 3 9 1.23 4 9 1.23 7 9 1.23 6 9 1.24 16 19 1.24 12 13 1.25 1 8 1.25 1 13 1.26 2 5 1.26 14 15 1.26 1 17 1.27 1 3 1.27 8 16 1.27 2 9 1.28 2 11 1.29 14 16 1.29 2 7 1.30 3 13 1.31 7 10 1.33 3 6 1.34 10 12 1.36 4 20 1.37 18 19 1.37 8 14 1.38 14 18 1.62 17 19 1.99 4 16 2.03 8 20 2.04 9 11 2.05 3 20 2.05 3 8 2.08 2 6 2.09 3 7 2.10 8 15 2.10 7 12 2.10 1 4 2.10 8 18 2.11 6 11 2.12 1 16 2.14 14 17 2.15 3 12 2.15 10 13 2.17 2 10 2.18 9 13 2.21 4 7 2.24 2 3 2.24 9 10 2.24 4 13 2.25 14 20 2.27 1 6 2.28 19 20 2.29 13 17 2.31 6 20 2.32 4 8 2.35 15 17 2.36 1 19 2.36 3 16 2.36 1 20 2.37 8 13 2.38 17 18 2.43 5 7 2.44 15 16 2.44 16 17 2.46 7 13 2.46 5 9 2.46 6 7 2.47 2 4 2.48 1 12 2.49 9 12 2.49 1 9 2.49 1 14 2.49 3 17 2.51 16 18 2.53 3 10 2.54 9 20 2.54 7 11 2.56 6 8 2.62 6 13 2.64 6 16 2.65 13 20 2.70 3 11 2.71 4 12 2.82 13 16 2.90 2 13 2.94 5 6 2.96 4 11 2.98 Time profile in seconds ----------------------- 0.00: 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. 0.02: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.15: Structure factors and derivatives 0.10: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.10: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.00: Analysis of variance 0.00: 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. +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + bilm001 finished at 12:45:56 Total elapsed time: 0.39 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++