+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL - CRYSTAL STRUCTURE REFINEMENT - MULTI-CPU VERSION + + Copyright(C) George M. Sheldrick 1993-2017 Version 2017/1 + + gore001 started at 14:06:01 on 17-Jun-2021 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Command line parameters: gore001 -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 gore001_a.res in P2(1) REM Old TITL gore001 in P2(1) REM SHELXT solution in P2(1) REM R1 0.084, Rweak 0.040, Alpha 0.004, Orientation as input REM Flack x = 0.007 ( 0.019 ) from Parsons' quotients REM Formula found by SHELXT: C10 N O3 S CELL 1.54178 5.3119 18.1819 6.2695 90 98.887 90 ZERR 2 0.0004 0.0014 0.0005 0 0.002 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H N O S UNIT 20 34 2 6 2 V = 598.24 F(000) = 248.0 Mu = 2.33 mm-1 Cell Wt = 462.61 Rho = 1.284 EQIV $1 1+X,+Y,+Z L.S. 20 PLAN 4 SIZE 0.16 0.318 0.382 TEMP -173.15 CONF HTAB N1 O3_$1 BOND $H list 4 MORE -1 fmap 2 53 acta EXTI 0.036 OMIT -1 2 1 OMIT -1 -8 0 OMIT 0 -2 0 OMIT 0 2 0 WGHT 0.0813 0.6412 FVAR 1.72362 REM REM REM S1 5 0.94328 0.69122 0.06509 11.00000 0.02559 0.02193 0.02208 = 0.00144 0.00694 -0.00282 O1 4 0.97339 0.67041 0.49939 11.00000 0.02908 0.02830 0.02167 = -0.00258 0.00131 -0.00357 O2 4 0.60706 0.42547 0.47062 11.00000 0.02004 0.01898 0.02942 = 0.00635 0.00599 -0.00081 O3 4 0.30243 0.51139 0.35390 11.00000 0.01839 0.02699 0.02769 = 0.00487 0.00377 0.00035 N1 3 0.72046 0.52600 0.31251 11.00000 0.01726 0.01843 0.02439 = 0.00332 0.00355 0.00230 H1 2 0.86643 0.50397 0.34736 11.00000 -1.20000 C1 1 0.88729 0.65533 0.31512 11.00000 0.01840 0.01925 0.02484 = -0.00179 0.00780 0.00211 C2 1 0.69226 0.59830 0.21874 11.00000 0.01997 0.02038 0.01723 = 0.00318 0.00365 -0.00063 AFIX 13 H2 2 0.51776 0.61701 0.22989 11.00000 -1.20000 AFIX 0 C3 1 0.74290 0.60887 -0.02005 11.00000 0.01896 0.02383 0.01951 = 0.00039 0.00653 -0.00104 C4 1 0.89790 0.54707 -0.09912 11.00000 0.02398 0.02477 0.02129 = -0.00095 0.00655 -0.00038 AFIX 137 H4a 2 0.94941 0.56116 -0.23697 11.00000 -1.50000 H4b 2 0.79423 0.50229 -0.11894 11.00000 -1.50000 H4c 2 1.04993 0.53793 0.00758 11.00000 -1.50000 AFIX 0 C5 1 0.51235 0.62743 -0.18225 11.00000 0.02299 0.03920 0.02390 = 0.00387 0.00715 0.00319 AFIX 137 H5a 2 0.41719 0.66727 -0.12585 11.00000 -1.50000 H5b 2 0.40310 0.58393 -0.20899 11.00000 -1.50000 H5c 2 0.56659 0.64319 -0.31758 11.00000 -1.50000 AFIX 0 C6 1 0.52218 0.48905 0.37683 11.00000 0.02371 0.01793 0.01348 = 0.00062 0.00271 -0.00425 C7 1 0.42901 0.37061 0.53450 11.00000 0.02113 0.02069 0.02865 = 0.00407 0.00932 -0.00242 C8 1 0.60682 0.30961 0.62731 11.00000 0.02738 0.02797 0.06011 = 0.01779 0.01151 0.00432 AFIX 137 H8a 2 0.70327 0.29178 0.51647 11.00000 -1.50000 H8b 2 0.50716 0.26911 0.67488 11.00000 -1.50000 H8c 2 0.72516 0.32845 0.75066 11.00000 -1.50000 AFIX 0 C9 1 0.24976 0.34476 0.33897 11.00000 0.03359 0.02785 0.03613 = -0.00431 0.00568 -0.00895 AFIX 137 H9a 2 0.13658 0.38521 0.28291 11.00000 -1.50000 H9b 2 0.14784 0.30357 0.37931 11.00000 -1.50000 H9c 2 0.34825 0.32870 0.22749 11.00000 -1.50000 AFIX 0 C10 1 0.28853 0.40071 0.71091 11.00000 0.02781 0.03036 0.02545 = 0.00483 0.00736 -0.00378 AFIX 137 H10a 2 0.41163 0.42255 0.82604 11.00000 -1.50000 H10b 2 0.19762 0.36057 0.77040 11.00000 -1.50000 H10c 2 0.16623 0.43830 0.64945 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for gore001_a.res in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 S1 - C1 C3 O1 - C1 O2 - C6 C7 O3 - C6 N1 - C6 C2 C1 - O1 C2 S1 C2 - N1 C1 C3 C3 - C5 C4 C2 S1 C4 - C3 C5 - C3 C6 - O3 O2 N1 C7 - O2 C9 C8 C10 C8 - C7 C9 - C7 C10 - C7 Operators for generating equivalent atoms: $1 x+1, y, z Floating origin restraints generated h k l Fo^2 Sigma Why rejected (first 50 of each listed) 0 -1 0 0.60 0.10 systematically absent but >3sig(I) 0 -1 0 0.60 0.10 systematically absent but >3sig(I) 0 -3 0 1.90 0.20 systematically absent but >3sig(I) 0 -5 0 1.20 0.30 systematically absent but >3sig(I) 0 5 0 2.50 0.40 systematically absent but >3sig(I) 0 -7 0 1.20 0.30 systematically absent but >3sig(I) 29 Systematically absent reflections rejected 6794 Reflections read, of which 32 rejected -6 =< h =< 6, -22 =< k =< 22, -7 =< l =< 7, Max. 2-theta = 144.04 6 Systematic absence violations (I>3sig(I)) before merging 0 Inconsistent equivalents 2210 Unique reflections, of which 0 suppressed R(int) = 0.0412 R(sigma) = 0.0465 Friedel opposites not merged Maximum memory for data reduction = 2026 / 22185 Number of data for d > 0.810A (CIF: max) and d > 0.833A (CIF: full) (ignoring systematic absences): Unique reflections found (point group) 2210 2062 Unique reflections possible (point group) 2362 2180 Unique reflections found (Laue group) 1206 1118 Unique reflections possible (Laue group) 1220 1128 Unique Friedel pairs found 1004 944 Unique Friedel pairs possible 1142 1052 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 = 47 / 2441 / 220826 wR2 = 0.1524 before cycle 1 for 2210 data and 145 / 145 parameters GooF = S = 1.178; Restrained GooF = 1.177 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0813 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.72360 0.01233 -0.001 OSF 2 0.03617 0.00654 0.025 EXTI Mean shift/esd = 0.019 Maximum = 0.087 for U11 N1 Max. shift = 0.007 A for H1 Max. dU = 0.000 for N1 Least-squares cycle 2 Maximum vector length = 623 Memory required = 47 / 2441 / 220826 wR2 = 0.1524 before cycle 2 for 2210 data and 145 / 145 parameters GooF = S = 1.177; Restrained GooF = 1.177 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0813 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.72374 0.01233 0.011 OSF 2 0.03626 0.00655 0.015 EXTI Mean shift/esd = 0.008 Maximum = 0.039 for U11 N1 Max. shift = 0.003 A for H1 Max. dU = 0.000 for N1 Least-squares cycle 3 Maximum vector length = 623 Memory required = 47 / 2441 / 220826 wR2 = 0.1524 before cycle 3 for 2210 data and 145 / 145 parameters GooF = S = 1.177; Restrained GooF = 1.177 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0813 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.72378 0.01234 0.003 OSF 2 0.03629 0.00656 0.004 EXTI Mean shift/esd = 0.001 Maximum = 0.005 for U11 C8 Max. shift = 0.000 A for H1 Max. dU = 0.000 for C9 Least-squares cycle 4 Maximum vector length = 623 Memory required = 47 / 2441 / 220826 wR2 = 0.1524 before cycle 4 for 2210 data and 145 / 145 parameters GooF = S = 1.177; Restrained GooF = 1.177 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0813 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.72378 0.01234 0.001 OSF 2 0.03629 0.00656 0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for U11 C3 Max. shift = 0.000 A for H1 Max. dU = 0.000 for C2 Least-squares cycle 5 Maximum vector length = 623 Memory required = 47 / 2441 / 220826 wR2 = 0.1524 before cycle 5 for 2210 data and 145 / 145 parameters GooF = S = 1.177; Restrained GooF = 1.177 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0813 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.72379 0.01234 0.000 OSF 2 0.03630 0.00656 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for U11 C8 Max. shift = 0.000 A for H9A Max. dU = 0.000 for C7 Least-squares cycle 6 Maximum vector length = 623 Memory required = 47 / 2441 / 220826 wR2 = 0.1524 before cycle 6 for 2210 data and 145 / 145 parameters GooF = S = 1.177; Restrained GooF = 1.177 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0813 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.72379 0.01234 0.000 OSF 2 0.03630 0.00656 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y S1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for C2 Least-squares cycle 7 Maximum vector length = 623 Memory required = 47 / 2441 / 220826 wR2 = 0.1524 before cycle 7 for 2210 data and 145 / 145 parameters GooF = S = 1.177; Restrained GooF = 1.177 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0813 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.72379 0.01234 0.000 OSF 2 0.03630 0.00656 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y C1 Max. shift = 0.000 A for H5A Max. dU = 0.000 for C7 Least-squares cycle 8 Maximum vector length = 623 Memory required = 47 / 2441 / 220826 wR2 = 0.1524 before cycle 8 for 2210 data and 145 / 145 parameters GooF = S = 1.177; Restrained GooF = 1.177 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0813 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.72379 0.01234 0.000 OSF 2 0.03630 0.00656 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for C1 Least-squares cycle 9 Maximum vector length = 623 Memory required = 47 / 2441 / 220826 wR2 = 0.1524 before cycle 9 for 2210 data and 145 / 145 parameters GooF = S = 1.177; Restrained GooF = 1.177 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0813 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.72379 0.01234 0.000 OSF 2 0.03630 0.00656 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y O3 Max. shift = 0.000 A for H1 Max. dU = 0.000 for C5 Least-squares cycle 10 Maximum vector length = 623 Memory required = 47 / 2441 / 220826 wR2 = 0.1524 before cycle 10 for 2210 data and 145 / 145 parameters GooF = S = 1.177; Restrained GooF = 1.177 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0813 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.72379 0.01234 0.000 OSF 2 0.03630 0.00656 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y O3 Max. shift = 0.000 A for O1 Max. dU = 0.000 for C3 Least-squares cycle 11 Maximum vector length = 623 Memory required = 47 / 2441 / 220826 wR2 = 0.1524 before cycle 11 for 2210 data and 145 / 145 parameters GooF = S = 1.177; Restrained GooF = 1.177 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0813 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.72379 0.01234 0.000 OSF 2 0.03630 0.00656 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H8C Max. dU = 0.000 for O3 Least-squares cycle 12 Maximum vector length = 623 Memory required = 47 / 2441 / 220826 wR2 = 0.1524 before cycle 12 for 2210 data and 145 / 145 parameters GooF = S = 1.177; Restrained GooF = 1.177 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0813 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.72379 0.01234 0.000 OSF 2 0.03630 0.00656 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for O1 Max. dU = 0.000 for C8 Least-squares cycle 13 Maximum vector length = 623 Memory required = 47 / 2441 / 220826 wR2 = 0.1524 before cycle 13 for 2210 data and 145 / 145 parameters GooF = S = 1.177; Restrained GooF = 1.177 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0813 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.72379 0.01234 0.000 OSF 2 0.03630 0.00656 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x S1 Max. shift = 0.000 A for H9B Max. dU = 0.000 for O3 Least-squares cycle 14 Maximum vector length = 623 Memory required = 47 / 2441 / 220826 wR2 = 0.1524 before cycle 14 for 2210 data and 145 / 145 parameters GooF = S = 1.177; Restrained GooF = 1.177 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0813 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.72379 0.01234 0.000 OSF 2 0.03630 0.00656 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x S1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for C7 Least-squares cycle 15 Maximum vector length = 623 Memory required = 47 / 2441 / 220826 wR2 = 0.1524 before cycle 15 for 2210 data and 145 / 145 parameters GooF = S = 1.177; Restrained GooF = 1.177 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0813 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.72379 0.01234 0.000 OSF 2 0.03630 0.00656 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for O3 Least-squares cycle 16 Maximum vector length = 623 Memory required = 47 / 2441 / 220826 wR2 = 0.1524 before cycle 16 for 2210 data and 145 / 145 parameters GooF = S = 1.177; Restrained GooF = 1.177 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0813 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.72379 0.01234 0.000 OSF 2 0.03630 0.00656 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for H10C Max. dU = 0.000 for C5 Least-squares cycle 17 Maximum vector length = 623 Memory required = 47 / 2441 / 220826 wR2 = 0.1524 before cycle 17 for 2210 data and 145 / 145 parameters GooF = S = 1.177; Restrained GooF = 1.177 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0813 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.72379 0.01234 0.000 OSF 2 0.03630 0.00656 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x S1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for C7 Least-squares cycle 18 Maximum vector length = 623 Memory required = 47 / 2441 / 220826 wR2 = 0.1524 before cycle 18 for 2210 data and 145 / 145 parameters GooF = S = 1.177; Restrained GooF = 1.177 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0813 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.72379 0.01234 0.000 OSF 2 0.03630 0.00656 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for H10B Max. dU = 0.000 for C3 Least-squares cycle 19 Maximum vector length = 623 Memory required = 47 / 2441 / 220826 wR2 = 0.1524 before cycle 19 for 2210 data and 145 / 145 parameters GooF = S = 1.177; Restrained GooF = 1.177 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0813 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.72379 0.01234 0.000 OSF 2 0.03630 0.00656 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for C10 Least-squares cycle 20 Maximum vector length = 623 Memory required = 47 / 2441 / 220826 wR2 = 0.1524 before cycle 20 for 2210 data and 145 / 145 parameters GooF = S = 1.177; Restrained GooF = 1.177 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0813 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.72379 0.01234 0.000 OSF 2 0.03630 0.00656 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for C10 Max. dU = 0.000 for C7 Largest correlation matrix elements 0.661 EXTI / OSF 0.537 U22 S1 / OSF 0.553 U33 S1 / OSF 0.518 U11 S1 / OSF Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.5178 0.6170 0.2298 13 1.000 0.000 C2 N1 C1 C3 H4A 0.9497 0.5612 -0.2368 137 0.980 0.000 C4 C3 H4A H4B 0.7942 0.5023 -0.1191 137 0.980 0.000 C4 C3 H4A H4C 1.0498 0.5379 0.0077 137 0.980 0.000 C4 C3 H4A H5A 0.4171 0.6673 -0.1259 137 0.980 0.000 C5 C3 H5A H5B 0.4032 0.5839 -0.2091 137 0.980 0.000 C5 C3 H5A H5C 0.5666 0.6432 -0.3176 137 0.980 0.000 C5 C3 H5A H8A 0.7035 0.2919 0.5166 137 0.980 0.000 C8 C7 H8A H8B 0.5071 0.2691 0.6747 137 0.980 0.000 C8 C7 H8A H8C 0.7249 0.3284 0.7509 137 0.980 0.000 C8 C7 H8A H9A 0.1361 0.3851 0.2832 137 0.980 0.000 C9 C7 H9A H9B 0.1483 0.3034 0.3792 137 0.980 0.000 C9 C7 H9A H9C 0.3482 0.3289 0.2273 137 0.980 0.000 C9 C7 H9A H10A 0.4116 0.4227 0.8259 137 0.980 0.000 C10 C7 H10A H10B 0.1980 0.3606 0.7707 137 0.980 0.000 C10 C7 H10A H10C 0.1659 0.4382 0.6494 137 0.980 0.000 C10 C7 H10A gore001_a.res in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S1 0.94327 0.69122 0.06509 1.00000 0.02559 0.02192 0.02210 0.00144 0.00695 -0.00280 0.02286 0.00204 0.00021 0.00006 0.00018 0.00000 0.00063 0.00061 0.00060 0.00045 0.00042 0.00048 0.00039 O1 0.97339 0.67041 0.49940 1.00000 0.02901 0.02838 0.02167 -0.00256 0.00131 -0.00354 0.02663 0.00690 0.00076 0.00021 0.00063 0.00000 0.00189 0.00197 0.00172 0.00132 0.00143 0.00141 0.00087 O2 0.60708 0.42547 0.47059 1.00000 0.02005 0.01902 0.02949 0.00641 0.00597 -0.00077 0.02262 0.00680 0.00064 0.00020 0.00058 0.00000 0.00160 0.00166 0.00172 0.00149 0.00130 0.00144 0.00076 O3 0.30245 0.51139 0.35393 1.00000 0.01840 0.02701 0.02758 0.00481 0.00372 0.00036 0.02431 0.00675 0.00065 0.00021 0.00059 0.00000 0.00170 0.00180 0.00188 0.00147 0.00138 0.00139 0.00080 N1 0.72045 0.52600 0.31249 1.00000 0.01752 0.01851 0.02430 0.00321 0.00357 0.00222 0.02007 0.00775 0.00079 0.00023 0.00069 0.00000 0.00195 0.00206 0.00208 0.00161 0.00159 0.00161 0.00087 H1 0.86766 0.50386 0.34860 1.00000 0.02409 0.11805 0.01268 0.00385 0.01035 0.00000 0.00000 C1 0.88728 0.65533 0.31510 1.00000 0.01846 0.01923 0.02473 -0.00187 0.00777 0.00208 0.02034 0.00904 0.00092 0.00027 0.00080 0.00000 0.00217 0.00220 0.00247 0.00194 0.00180 0.00185 0.00098 C2 0.69228 0.59830 0.21869 1.00000 0.01998 0.02033 0.01725 0.00306 0.00370 -0.00066 0.01910 0.00896 0.00090 0.00026 0.00076 0.00000 0.00222 0.00229 0.00214 0.00179 0.00173 0.00191 0.00098 H2 0.51778 0.61702 0.22984 1.00000 0.02292 0.00000 0.00000 C3 0.74291 0.60887 -0.02003 1.00000 0.01899 0.02384 0.01949 0.00037 0.00650 -0.00112 0.02040 0.00902 0.00092 0.00029 0.00078 0.00000 0.00210 0.00227 0.00220 0.00186 0.00173 0.00192 0.00096 C4 0.89792 0.54709 -0.09910 1.00000 0.02396 0.02494 0.02122 -0.00100 0.00650 -0.00040 0.02306 0.00939 0.00099 0.00028 0.00082 0.00000 0.00251 0.00257 0.00236 0.00193 0.00192 0.00209 0.00106 H4A 0.94968 0.56121 -0.23681 1.00000 0.03459 0.00000 0.00000 H4B 0.79419 0.50232 -0.11915 1.00000 0.03459 0.00000 0.00000 H4C 1.04982 0.53790 0.00772 1.00000 0.03459 0.00000 0.00000 C5 0.51237 0.62743 -0.18229 1.00000 0.02289 0.03923 0.02378 0.00383 0.00710 0.00325 0.02827 0.01068 0.00102 0.00034 0.00085 0.00000 0.00240 0.00298 0.00246 0.00218 0.00198 0.00217 0.00116 H5A 0.41714 0.66725 -0.12590 1.00000 0.04240 0.00000 0.00000 H5B 0.40316 0.58392 -0.20908 1.00000 0.04240 0.00000 0.00000 H5C 0.56664 0.64320 -0.31759 1.00000 0.04240 0.00000 0.00000 C6 0.52216 0.48905 0.37681 1.00000 0.02373 0.01793 0.01358 0.00056 0.00275 -0.00426 0.01843 0.00909 0.00093 0.00027 0.00079 0.00000 0.00234 0.00224 0.00218 0.00181 0.00175 0.00195 0.00096 C7 0.42898 0.37063 0.53453 1.00000 0.02116 0.02067 0.02872 0.00406 0.00936 -0.00245 0.02293 0.01057 0.00095 0.00031 0.00092 0.00000 0.00232 0.00249 0.00276 0.00205 0.00206 0.00190 0.00109 C8 0.60681 0.30962 0.62734 1.00000 0.02758 0.02772 0.06021 0.01763 0.01157 0.00420 0.03800 0.01299 0.00112 0.00033 0.00120 0.00000 0.00287 0.00293 0.00406 0.00273 0.00272 0.00238 0.00146 H8A 0.70348 0.29185 0.51658 1.00000 0.05700 0.00000 0.00000 H8B 0.50712 0.26907 0.67466 1.00000 0.05700 0.00000 0.00000 H8C 0.72495 0.32843 0.75086 1.00000 0.05700 0.00000 0.00000 C9 0.24973 0.34476 0.33897 1.00000 0.03361 0.02782 0.03627 -0.00433 0.00564 -0.00892 0.03254 0.01041 0.00116 0.00033 0.00101 0.00000 0.00291 0.00282 0.00312 0.00227 0.00248 0.00232 0.00128 H9A 0.13607 0.38514 0.28324 1.00000 0.04881 0.00000 0.00000 H9B 0.14832 0.30344 0.37920 1.00000 0.04881 0.00000 0.00000 H9C 0.34821 0.32889 0.22729 1.00000 0.04881 0.00000 0.00000 C10 0.28853 0.40072 0.71094 1.00000 0.02797 0.03037 0.02542 0.00481 0.00751 -0.00375 0.02756 0.01091 0.00109 0.00032 0.00092 0.00000 0.00267 0.00278 0.00265 0.00214 0.00214 0.00221 0.00117 H10A 0.41159 0.42267 0.82587 1.00000 0.04134 0.00000 0.00000 H10B 0.19801 0.36056 0.77070 1.00000 0.04134 0.00000 0.00000 H10C 0.16590 0.43822 0.64940 1.00000 0.04134 0.00000 0.00000 Final Structure Factor Calculation for gore001_a.res in P2(1) Total number of l.s. parameters = 145 Maximum vector length = 623 Memory required = 47 / 2296 / 29282 wR2 = 0.1524 before cycle 21 for 2210 data and 0 / 145 parameters GooF = S = 1.177; Restrained GooF = 1.177 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0813 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 wR2 = 0.1524, GooF = S = 1.177, Restrained GooF = 1.177 for all data R1 = 0.0545 for 2204 Fo > 4sig(Fo) and 0.0546 for all 2210 data Flack x = 0.017(40) by classical fit to all intensities 0.014(21) from 987 selected quotients (Parsons' method) Occupancy sum of asymmetric unit = 15.00 for non-hydrogen and 17.00 for H and D atoms Principal mean square atomic displacements U 0.0277 0.0234 0.0175 S1 0.0324 0.0277 0.0199 O1 0.0325 0.0205 0.0149 O2 0.0321 0.0225 0.0183 O3 0.0258 0.0189 0.0156 N1 0.0265 0.0207 0.0138 C1 0.0223 0.0201 0.0149 C2 0.0241 0.0222 0.0149 C3 0.0261 0.0244 0.0187 C4 0.0408 0.0249 0.0192 C5 0.0261 0.0159 0.0133 C6 0.0315 0.0232 0.0141 C7 0.0681 0.0259 0.0200 C8 0.0411 0.0355 0.0210 C9 0.0342 0.0298 0.0187 C10 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 0.077 0.098 0.115 0.135 0.157 0.184 0.225 0.296 1.000 Number in group 224. 224. 216. 220. 222. 225. 218. 221. 223. 217. GooF 0.866 1.052 1.199 1.227 1.536 1.375 1.393 0.914 0.917 1.096 K 1.135 1.021 1.013 1.023 1.007 1.026 1.020 1.025 1.010 1.016 Resolution(A) 0.81 0.84 0.88 0.92 0.97 1.02 1.09 1.21 1.36 1.69 inf Number in group 222. 225. 219. 224. 220. 224. 217. 216. 221. 222. GooF 2.235 1.422 1.047 0.908 0.971 0.869 0.801 0.720 0.784 1.181 K 0.841 0.995 1.055 1.079 1.090 1.063 1.039 1.013 0.963 1.017 R1 0.156 0.085 0.067 0.052 0.054 0.042 0.038 0.032 0.036 0.052 Recommended weighting scheme: WGHT 0.0809 0.6395 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) -4 -14 4 18.83 66.84 5.82 0.135 0.83 -4 8 6 35.27 95.16 5.49 0.161 0.82 -2 19 3 32.25 84.47 5.20 0.152 0.84 -2 18 4 33.22 83.67 5.03 0.151 0.83 -4 -8 6 37.16 90.96 5.00 0.157 0.82 -5 -12 3 33.43 81.25 4.79 0.149 0.83 -5 -13 3 11.86 37.91 4.52 0.102 0.81 6 7 0 38.50 83.69 4.39 0.151 0.83 -5 -4 5 55.68 112.39 4.31 0.175 0.85 3 -4 6 15.72 42.75 4.30 0.108 0.82 -5 -14 2 43.23 90.24 4.24 0.157 0.81 -5 -3 5 19.02 48.67 4.22 0.115 0.86 2 18 3 26.46 61.60 4.21 0.129 0.84 -5 -2 5 22.95 55.32 4.20 0.123 0.87 -4 12 5 32.47 70.33 4.14 0.138 0.82 0 8 7 32.56 69.98 4.12 0.138 0.82 0 15 5 29.87 66.32 4.11 0.134 0.87 -4 -16 3 57.57 111.17 4.09 0.174 0.82 2 13 5 31.64 66.06 3.99 0.134 0.84 -5 -10 4 60.74 113.15 3.89 0.175 0.83 2 9 6 25.44 55.08 3.85 0.122 0.83 6 1 1 29.26 61.37 3.83 0.129 0.85 0 20 3 31.38 64.28 3.80 0.132 0.83 -1 19 3 62.81 116.40 3.79 0.178 0.87 -4 -12 5 42.68 81.62 3.72 0.149 0.82 -3 -16 4 59.62 107.92 3.70 0.171 0.84 5 13 1 31.57 63.82 3.65 0.132 0.82 3 14 4 22.75 48.74 3.59 0.115 0.83 4 -5 5 31.74 61.57 3.58 0.129 0.82 -4 -11 5 7.18 22.20 3.54 0.078 0.84 -1 13 6 13.84 32.97 3.45 0.095 0.84 -1 14 6 71.83 120.26 3.34 0.181 0.81 1 12 6 20.71 42.36 3.27 0.107 0.83 0 22 0 24.24 48.37 3.24 0.115 0.83 2 16 4 12.08 28.73 3.24 0.088 0.84 2 -9 6 30.28 56.35 3.21 0.124 0.83 1 -8 0 895.07 1304.48 3.20 0.596 2.09 4 17 1 20.99 42.00 3.17 0.107 0.81 -1 -17 5 15.98 33.19 3.06 0.095 0.81 2 0 1 22.64 41.69 2.98 0.107 2.29 -6 9 1 31.15 55.59 2.98 0.123 0.81 -5 7 5 23.08 42.98 2.96 0.108 0.82 1 2 0 4857.38 3552.79 2.96 0.983 4.55 0 17 4 98.57 151.47 2.94 0.203 0.88 -3 16 4 76.66 119.61 2.93 0.180 0.84 -1 22 1 39.80 67.67 2.91 0.136 0.81 4 15 2 25.99 47.09 2.88 0.113 0.83 2 14 5 39.37 65.84 2.85 0.134 0.82 1 16 5 6.51 17.05 2.84 0.068 0.81 3 12 4 20.99 39.36 2.81 0.103 0.88 Bond lengths and angles S1 - Distance Angles C1 1.7650 (0.0052) C3 1.8664 (0.0052) 77.90 (0.22) S1 C1 O1 - Distance Angles C1 1.2068 (0.0066) O1 O2 - Distance Angles C6 1.3429 (0.0063) C7 1.4721 (0.0059) 121.04 (0.38) O2 C6 O3 - Distance Angles C6 1.2231 (0.0062) O3 N1 - Distance Angles C6 1.3619 (0.0063) C2 1.4385 (0.0060) 122.38 (0.42) H1 0.8775 (0.0700) 113.36 (4.29) 123.84 (4.34) N1 C6 C2 C1 - Distance Angles O1 1.2068 (0.0066) C2 1.5230 (0.0067) 131.96 (0.48) S1 1.7650 (0.0052) 132.48 (0.42) 95.56 (0.31) C1 O1 C2 C2 - Distance Angles N1 1.4385 (0.0060) C1 1.5230 (0.0067) 116.01 (0.40) C3 1.5728 (0.0061) 118.58 (0.42) 95.09 (0.37) H2 1.0000 108.75 108.75 108.75 C2 N1 C1 C3 C3 - Distance Angles C5 1.5045 (0.0071) C4 1.5205 (0.0070) 111.75 (0.42) C2 1.5728 (0.0061) 115.46 (0.40) 113.63 (0.41) S1 1.8664 (0.0052) 112.46 (0.38) 111.86 (0.33) 89.98 (0.29) C3 C5 C4 C2 C4 - Distance Angles C3 1.5205 (0.0070) H4A 0.9800 109.47 H4B 0.9800 109.47 109.47 H4C 0.9800 109.47 109.47 109.47 C4 C3 H4A H4B C5 - Distance Angles C3 1.5045 (0.0071) H5A 0.9800 109.47 H5B 0.9800 109.47 109.47 H5C 0.9800 109.47 109.47 109.47 C5 C3 H5A H5B C6 - Distance Angles O3 1.2231 (0.0062) O2 1.3429 (0.0063) 125.96 (0.43) N1 1.3619 (0.0063) 124.69 (0.45) 109.35 (0.42) C6 O3 O2 C7 - Distance Angles O2 1.4721 (0.0059) C9 1.5067 (0.0082) 109.99 (0.43) C8 1.5139 (0.0077) 102.23 (0.38) 111.25 (0.52) C10 1.5277 (0.0076) 111.15 (0.44) 112.52 (0.45) 109.24 (0.49) C7 O2 C9 C8 C8 - Distance Angles C7 1.5139 (0.0077) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 C7 H8A H8B C9 - Distance Angles C7 1.5067 (0.0082) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 C7 H9A H9B C10 - Distance Angles C7 1.5277 (0.0076) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 C7 H10A H10B Selected torsion angles 171.20 ( 0.58) C3 - S1 - C1 - O1 -8.69 ( 0.29) C3 - S1 - C1 - C2 130.52 ( 0.48) C6 - N1 - C2 - C1 -117.26 ( 0.51) C6 - N1 - C2 - C3 -44.46 ( 0.77) O1 - C1 - C2 - N1 135.44 ( 0.37) S1 - C1 - C2 - N1 -169.76 ( 0.56) O1 - C1 - C2 - C3 10.14 ( 0.34) S1 - C1 - C2 - C3 112.09 ( 0.52) N1 - C2 - C3 - C5 -124.56 ( 0.48) C1 - C2 - C3 - C5 -18.92 ( 0.59) N1 - C2 - C3 - C4 104.43 ( 0.44) C1 - C2 - C3 - C4 -132.89 ( 0.38) N1 - C2 - C3 - S1 -9.54 ( 0.32) C1 - C2 - C3 - S1 126.09 ( 0.39) C1 - S1 - C3 - C5 -107.20 ( 0.37) C1 - S1 - C3 - C4 8.37 ( 0.28) C1 - S1 - C3 - C2 7.50 ( 0.71) C7 - O2 - C6 - O3 -173.31 ( 0.45) C7 - O2 - C6 - N1 3.22 ( 0.78) C2 - N1 - C6 - O3 -175.99 ( 0.41) C2 - N1 - C6 - O2 60.94 ( 0.56) C6 - O2 - C7 - C9 179.19 ( 0.48) C6 - O2 - C7 - C8 -64.35 ( 0.58) C6 - O2 - C7 - C10 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88(7) 2.31(7) 3.074(5) 146(6) N1-H1...O3_$1 R1 = 0.0475 for 1206 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.48 at 0.7870 0.6410 0.1029 [ 0.97 A from C3 ] Deepest hole -0.34 at 0.9590 0.4383 0.0704 [ 1.79 A from H4B ] Mean = 0.00, Rms deviation from mean = 0.09, Highest memory used = 2341 / 33221 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including eq.) Q1 1 0.7870 0.6410 0.1029 1.00000 0.05 0.48 0.97 C3 1.22 C2 1.28 S1 1.38 C1 Q2 1 1.0495 0.7000 0.2780 1.00000 0.05 0.43 1.23 C1 1.38 S1 1.60 O1 2.38 H8A Q3 1 1.1023 0.6436 0.0362 1.00000 0.05 0.42 1.24 S1 1.95 H4C 1.99 C3 2.13 H5A Q4 1 0.8855 0.6373 0.1813 1.00000 0.05 0.40 0.90 C1 1.29 S1 1.30 C2 1.46 C3 Shortest distances between peaks (including symmetry equivalents) 1 4 0.66 2 4 1.50 3 4 1.58 1 3 1.79 2 3 1.89 1 2 1.96 Time profile in seconds ----------------------- 0.16: 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. 0.21: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.10: OSF, H-atoms from difference map 0.89: Set up l.s. refinement 0.00: Generate idealized H-atoms 4.00: Structure factors, sum l.s. matrics 0.16: final structure factors 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.02: Solve l.s. equations 0.00: Generate HTAB table 0.18: Other dependent quantities, CIF, tables 0.00: Analysis of variance 0.09: Merge reflections for Fourier and .fcf 0.01: 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. +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + gore001 finished at 14:06:07 Total elapsed time: 5.81 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++