++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXTL XLMP CRYSTAL STRUCTURE REFINEMENT - MULTI-CPU VERSION + + Copyright(c) Bruker AXS Inc. 1993-2018 Version 2018/3 + + lobo001 started at 09:37:45 on 04-Nov-2019 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Command line parameters: lobo001 -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 lobo001_a.res in P2(1)/n lobo001.res created by SHELXL-2018/3 at 09:37:17 on 04-Nov-2019 CELL 0.71073 3.7404 9.8818 14.8004 90.000 92.532 90.000 ZERR 2.00 0.0003 0.0009 0.0012 0.000 0.002 0.000 LATT 1 SYMM -x+1/2, y+1/2, -z+1/2 SFAC C H O UNIT 24 20 12 V = 546.52 F(000) = 260.0 Mu = 0.12 mm-1 Cell Wt = 500.40 Rho = 1.520 LIST 4 TEMP -166.920 SIZE 0.162 0.203 0.381 L.S. 10 ACTA CONF FMAP 2 PLAN -15 0 0.00 BOND $H WGHT 0.086000 0.062100 FVAR 1.12357 O1 3 0.320542 0.523629 0.634103 11.00000 0.02271 0.01303 = 0.01608 0.00132 -0.00120 -0.00152 O2 3 0.633597 0.677039 0.719099 11.00000 0.02658 0.01819 = 0.01415 0.00021 -0.00475 -0.00099 O3 3 0.529165 0.865798 0.582468 11.00000 0.02054 0.01251 = 0.01139 0.00042 -0.00162 -0.00021 C1 1 0.363611 0.429101 0.708634 11.00000 0.02548 0.01772 = 0.02150 0.00709 -0.00067 -0.00186 C2 1 0.468509 0.645595 0.649765 11.00000 0.01677 0.01280 = 0.01289 0.00027 0.00048 0.00120 C3 1 0.406967 0.735349 0.571973 11.00000 0.01768 0.01240 = 0.01223 0.00000 -0.00049 0.00002 C4 1 0.252778 0.717040 0.487282 11.00000 0.01943 0.01457 = 0.01343 -0.00063 -0.00133 -0.00053 C5 1 0.279986 0.843485 0.441663 11.00000 0.02085 0.01609 = 0.01215 -0.00004 -0.00235 0.00012 C6 1 0.448603 0.929850 0.502325 11.00000 0.01813 0.01384 = 0.01094 0.00096 -0.00083 0.00083 H1 2 0.234150 0.462219 0.759439 11.00000 0.02665 H2 2 0.257963 0.348639 0.686797 11.00000 0.03608 H3 2 0.606247 0.413450 0.720516 11.00000 0.02967 H4 2 0.151972 0.637621 0.465934 11.00000 0.02286 H5 2 0.200994 0.865068 0.379057 11.00000 0.02602 HKLF 4 1 1 0 0 0 1 0 0 0 1 Covalent radii and connectivity table for lobo001_a.res in P2(1)/n C 0.770 H 0.320 O 0.660 O1 - C2 C1 O2 - C2 O3 - C6 C3 C1 - O1 C2 - O2 O1 C3 C3 - C4 O3 C2 C4 - C3 C5 C5 - C6 C4 C6 - O3 C5 C6_$1 Operators for generating equivalent atoms: $1 -x+1, -y+2, -z+1 h k l Fo^2 Sigma Why rejected (first 50 of each listed) 0 1 0 1.20 0.10 systematically absent but >3sig(I) 0 1 0 1.00 0.10 systematically absent but >3sig(I) -1 0 2 0.80 0.20 systematically absent but >3sig(I) 1 0 2 1.90 0.30 systematically absent but >3sig(I) 1 0 2 1.30 0.20 systematically absent but >3sig(I) -1 0 4 1.10 0.30 systematically absent but >3sig(I) -1 0 4 1.00 0.30 systematically absent but >3sig(I) -1 0 4 0.60 0.20 systematically absent but >3sig(I) -1 0 4 0.60 0.20 systematically absent but >3sig(I) 1 0 6 0.90 0.20 systematically absent but >3sig(I) 1 0 6 0.60 0.20 systematically absent but >3sig(I) 1 0 6 0.70 0.20 systematically absent but >3sig(I) 0 0 7 0.80 0.20 systematically absent but >3sig(I) 427 Systematically absent reflections rejected 15688 Reflections read, of which 427 rejected -6 =< h =< 6, -15 =< k =< 15, -23 =< l =< 23, Max. 2-theta = 70.17 13 Systematic absence violations (I>3sig(I)) before merging 0 Inconsistent equivalents 2396 Unique reflections, of which 0 suppressed R(int) = 0.0208 R(sigma) = 0.0135 Friedel opposites merged Maximum memory for data reduction = 1099 / 24011 Reflection statistics for all twin components combined (TWST 0 set) Number of data for d > 0.618A (CIF: max) and d > 0.833A (CIF: full) (ignoring systematic absences): Unique reflections found (point group) 2396 996 Unique reflections possible (point group) 2404 996 Unique reflections found (Laue group) 2396 996 Unique reflections possible (Laue group) 2404 996 Least-squares cycle 1 Maximum vector length = 623 Memory required = 24 / 1339 / 159338 wR2 = 0.1186 before cycle 1 for 2396 data and 102 / 102 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0860 * P )^2 + 0.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.12356 0.00316 -0.002 OSF Mean shift/esd = 0.006 Maximum = -0.021 for U23 O3 Max. shift = 0.000 A for H3 Max. dU = 0.000 for H1 Least-squares cycle 2 Maximum vector length = 623 Memory required = 24 / 1339 / 159338 wR2 = 0.1186 before cycle 2 for 2396 data and 102 / 102 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0860 * P )^2 + 0.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.12357 0.00316 0.001 OSF Mean shift/esd = 0.002 Maximum = -0.008 for U23 O3 Max. shift = 0.000 A for H3 Max. dU = 0.000 for H2 Least-squares cycle 3 Maximum vector length = 623 Memory required = 24 / 1339 / 159338 wR2 = 0.1187 before cycle 3 for 2396 data and 102 / 102 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0860 * P )^2 + 0.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.12357 0.00316 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z O2 Max. shift = 0.000 A for H3 Max. dU = 0.000 for H3 Least-squares cycle 4 Maximum vector length = 623 Memory required = 24 / 1339 / 159338 wR2 = 0.1186 before cycle 4 for 2396 data and 102 / 102 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0860 * P )^2 + 0.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.12357 0.00316 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for y C6 Max. shift = 0.000 A for H3 Max. dU = 0.000 for H2 Least-squares cycle 5 Maximum vector length = 623 Memory required = 24 / 1339 / 159338 wR2 = 0.1187 before cycle 5 for 2396 data and 102 / 102 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0860 * P )^2 + 0.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.12357 0.00316 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z O2 Max. shift = 0.000 A for H2 Max. dU = 0.000 for H3 Least-squares cycle 6 Maximum vector length = 623 Memory required = 24 / 1339 / 159338 wR2 = 0.1186 before cycle 6 for 2396 data and 102 / 102 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0860 * P )^2 + 0.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.12357 0.00316 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z O2 Max. shift = 0.000 A for H3 Max. dU = 0.000 for H1 Least-squares cycle 7 Maximum vector length = 623 Memory required = 24 / 1339 / 159338 wR2 = 0.1187 before cycle 7 for 2396 data and 102 / 102 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0860 * P )^2 + 0.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.12357 0.00316 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z O2 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H3 Least-squares cycle 8 Maximum vector length = 623 Memory required = 24 / 1339 / 159338 wR2 = 0.1187 before cycle 8 for 2396 data and 102 / 102 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0860 * P )^2 + 0.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.12357 0.00316 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z O2 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 9 Maximum vector length = 623 Memory required = 24 / 1339 / 159338 wR2 = 0.1187 before cycle 9 for 2396 data and 102 / 102 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0860 * P )^2 + 0.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.12357 0.00316 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z O2 Max. shift = 0.000 A for H2 Max. dU = 0.000 for H4 Least-squares cycle 10 Maximum vector length = 623 Memory required = 24 / 1339 / 159338 wR2 = 0.1186 before cycle 10 for 2396 data and 102 / 102 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0860 * P )^2 + 0.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.12357 0.00316 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z O2 Max. shift = 0.000 A for H2 Max. dU = 0.000 for H3 No correlation matrix elements larger than 0.500 lobo001_a.res in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq O1 0.32054 0.52363 0.63410 1.00000 0.02271 0.01303 0.01608 0.00132 -0.00120 -0.00152 0.01733 0.00085 0.00013 0.00005 0.00003 0.00000 0.00024 0.00020 0.00021 0.00014 0.00016 0.00016 0.00012 O2 0.63360 0.67704 0.71910 1.00000 0.02658 0.01819 0.01415 0.00021 -0.00475 -0.00099 0.01981 0.00089 0.00014 0.00005 0.00003 0.00000 0.00026 0.00023 0.00021 0.00015 0.00017 0.00017 0.00012 O3 0.52917 0.86580 0.58247 1.00000 0.02054 0.01251 0.01139 0.00042 -0.00162 -0.00021 0.01488 0.00082 0.00013 0.00005 0.00003 0.00000 0.00022 0.00020 0.00019 0.00013 0.00015 0.00014 0.00011 C1 0.36361 0.42910 0.70863 1.00000 0.02548 0.01772 0.02150 0.00709 -0.00067 -0.00186 0.02161 0.00137 0.00020 0.00007 0.00005 0.00000 0.00032 0.00028 0.00029 0.00021 0.00023 0.00022 0.00015 C2 0.46851 0.64560 0.64977 1.00000 0.01677 0.01280 0.01289 0.00027 0.00048 0.00120 0.01416 0.00108 0.00017 0.00006 0.00004 0.00000 0.00025 0.00024 0.00024 0.00017 0.00019 0.00017 0.00013 C3 0.40697 0.73535 0.57197 1.00000 0.01768 0.01240 0.01223 0.00000 -0.00049 0.00002 0.01414 0.00105 0.00016 0.00006 0.00004 0.00000 0.00025 0.00023 0.00023 0.00017 0.00018 0.00018 0.00012 C4 0.25278 0.71704 0.48728 1.00000 0.01943 0.01457 0.01343 -0.00063 -0.00133 -0.00053 0.01587 0.00107 0.00017 0.00006 0.00004 0.00000 0.00027 0.00025 0.00024 0.00018 0.00019 0.00019 0.00013 C5 0.27999 0.84349 0.44166 1.00000 0.02085 0.01609 0.01215 -0.00004 -0.00235 0.00012 0.01646 0.00113 0.00018 0.00006 0.00004 0.00000 0.00028 0.00026 0.00023 0.00018 0.00019 0.00019 0.00013 C6 0.44860 0.92985 0.50232 1.00000 0.01813 0.01384 0.01094 0.00096 -0.00083 0.00083 0.01435 0.00106 0.00016 0.00006 0.00004 0.00000 0.00026 0.00024 0.00022 0.00017 0.00018 0.00018 0.00012 H1 0.23415 0.46222 0.75944 1.00000 0.02665 0.02302 0.00332 0.00137 0.00089 0.00000 0.00280 H2 0.25796 0.34864 0.68680 1.00000 0.03608 0.02492 0.00367 0.00142 0.00099 0.00000 0.00339 H3 0.60625 0.41345 0.72052 1.00000 0.02967 0.02327 0.00352 0.00137 0.00090 0.00000 0.00302 H4 0.15197 0.63762 0.46593 1.00000 0.02286 0.02133 0.00328 0.00126 0.00082 0.00000 0.00264 H5 0.20099 0.86507 0.37906 1.00000 0.02602 0.02204 0.00336 0.00130 0.00085 0.00000 0.00285 Final Structure Factor Calculation for lobo001_a.res in P2(1)/n Total number of l.s. parameters = 102 Maximum vector length = 623 Memory required = 24 / 1237 / 26789 wR2 = 0.1187 before cycle 11 for 2396 data and 0 / 102 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0860 * P )^2 + 0.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 wR2 = 0.1187, GooF = S = 1.021, Restrained GooF = 1.021 for all data R1 = 0.0398 for 2143 Fo > 4sig(Fo) and 0.0429 for all 2396 data Occupancy sum of asymmetric unit = 9.00 for non-hydrogen and 5.00 for H and D atoms Principal mean square atomic displacements U 0.0237 0.0158 0.0125 O1 0.0291 0.0181 0.0122 O2 0.0212 0.0126 0.0109 O3 0.0290 0.0236 0.0122 C1 0.0171 0.0130 0.0123 C2 0.0180 0.0124 0.0120 C3 0.0202 0.0148 0.0126 C4 0.0220 0.0161 0.0113 C5 0.0186 0.0141 0.0104 C6 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 0.008 0.017 0.026 0.036 0.047 0.060 0.077 0.100 0.144 1.000 Number in group 256. 236. 231. 254. 229. 244. 235. 231. 241. 239. GooF 0.939 1.094 1.136 1.121 1.144 1.068 0.893 0.928 0.904 0.940 K 1.319 0.970 0.959 0.948 0.980 0.991 1.009 1.018 1.028 1.061 Resolution(A) 0.62 0.64 0.67 0.70 0.74 0.78 0.84 0.93 1.06 1.33 inf Number in group 248. 232. 240. 240. 239. 239. 241. 238. 240. 239. GooF 0.770 0.754 0.737 0.709 0.808 0.839 1.099 1.184 1.383 1.531 K 1.072 1.062 1.043 1.038 1.009 1.016 0.987 0.989 1.004 1.085 R1 0.053 0.055 0.040 0.037 0.043 0.039 0.042 0.036 0.040 0.047 Recommended weighting scheme: WGHT 0.0766 0.0711 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) 1 7 1 7.08 3.34 5.40 0.021 1.31 0 0 12 7.29 14.56 4.75 0.044 1.23 2 6 1 3.01 1.15 4.58 0.012 1.23 0 2 7 22.55 14.24 4.55 0.043 1.94 1 1 3 71.38 48.48 4.40 0.080 2.80 1 11 4 4.02 8.07 4.38 0.033 0.85 0 7 9 3.20 6.50 4.28 0.029 1.07 -1 8 3 12.95 21.01 4.19 0.053 1.14 -1 1 5 0.70 0.08 4.05 0.003 2.31 0 7 12 0.96 2.73 4.04 0.019 0.93 0 5 5 0.48 1.73 4.01 0.015 1.64 2 1 0 6.37 10.75 3.93 0.038 1.84 0 6 11 24.57 36.58 3.80 0.070 1.04 2 10 2 8.44 13.60 3.73 0.042 0.87 1 8 4 2.41 4.72 3.72 0.025 1.11 0 4 4 0.47 0.02 3.72 0.002 2.05 1 4 9 0.50 1.68 3.67 0.015 1.27 1 5 5 3.93 2.09 3.65 0.017 1.49 -1 9 4 14.88 22.37 3.62 0.054 1.02 3 0 15 3.86 7.28 3.56 0.031 0.76 2 1 8 12.23 18.17 3.44 0.049 1.28 2 7 10 2.94 5.39 3.43 0.027 0.88 0 2 14 5.57 9.17 3.42 0.035 1.03 -2 4 1 30.43 21.93 3.42 0.054 1.49 0 4 15 20.80 29.92 3.40 0.063 0.92 2 3 4 0.46 0.00 3.38 0.001 1.47 0 0 4 172.20 128.17 3.38 0.130 3.70 -2 5 13 1.94 3.82 3.31 0.023 0.89 -1 3 3 19.02 26.76 3.19 0.060 2.24 3 3 11 11.33 16.74 3.19 0.047 0.86 1 9 0 3.23 1.76 3.19 0.015 1.05 -2 2 2 22.40 16.30 3.17 0.047 1.72 -1 1 8 4.59 2.82 3.17 0.019 1.66 -1 4 14 1.18 2.51 3.16 0.018 0.95 1 6 12 0.62 1.70 3.14 0.015 0.95 -1 4 4 0.09 0.66 3.10 0.009 1.82 -3 0 3 -0.07 0.60 3.07 0.009 1.22 -1 0 7 37.81 50.98 3.01 0.082 1.87 0 10 2 14.57 20.36 2.98 0.052 0.98 2 7 0 21.31 15.73 2.97 0.046 1.13 2 10 3 6.34 9.51 2.94 0.036 0.86 1 2 4 9.52 13.42 2.84 0.042 2.28 1 4 7 1.32 2.47 2.79 0.018 1.46 1 9 8 15.91 21.79 2.78 0.054 0.91 0 7 2 28.50 21.78 2.78 0.054 1.39 3 1 9 12.88 17.71 2.77 0.048 0.97 -1 4 8 10.82 14.92 2.74 0.045 1.39 -2 0 2 168.63 133.47 2.71 0.133 1.83 -1 6 12 0.48 1.27 2.70 0.013 0.96 2 2 12 4.65 7.01 2.67 0.031 0.99 Bond lengths and angles O1 - Distance Angles C2 1.3421 (0.0008) C1 1.4490 (0.0008) 114.60 (0.05) O1 C2 O2 - Distance Angles C2 1.2144 (0.0008) O2 O3 - Distance Angles C6 1.3663 (0.0007) C3 1.3742 (0.0008) 106.08 (0.05) O3 C6 C1 - Distance Angles O1 1.4490 (0.0008) H1 0.9691 (0.0130) 109.29 (0.79) H2 0.9389 (0.0141) 104.65 (0.89) 109.63 (1.15) H3 0.9297 (0.0134) 109.03 (0.84) 115.24 (1.13) 108.46 (1.15) C1 O1 H1 H2 C2 - Distance Angles O2 1.2144 (0.0008) O1 1.3421 (0.0008) 124.48 (0.06) C3 1.4635 (0.0009) 124.48 (0.06) 111.04 (0.05) C2 O2 O1 C3 - Distance Angles C4 1.3684 (0.0008) O3 1.3742 (0.0008) 110.62 (0.05) C2 1.4635 (0.0009) 133.30 (0.06) 116.08 (0.05) C3 C4 O3 C4 - Distance Angles C3 1.3684 (0.0008) C5 1.4260 (0.0009) 106.37 (0.05) H4 0.9205 (0.0124) 125.22 (0.75) 128.41 (0.75) C4 C3 C5 C5 - Distance Angles C6 1.3719 (0.0009) C4 1.4260 (0.0009) 106.00 (0.05) H5 0.9834 (0.0127) 126.30 (0.75) 127.69 (0.75) C5 C6 C4 C6 - Distance Angles O3 1.3663 (0.0007) C5 1.3719 (0.0009) 110.94 (0.05) C6_$1 1.4412 (0.0012) 115.98 (0.07) 133.08 (0.07) C6 O3 C5 Selected torsion angles 1.51 ( 0.09) C1 - O1 - C2 - O2 -178.92 ( 0.05) C1 - O1 - C2 - C3 0.01 ( 0.07) C6 - O3 - C3 - C4 179.19 ( 0.05) C6 - O3 - C3 - C2 174.86 ( 0.07) O2 - C2 - C3 - C4 -4.70 ( 0.10) O1 - C2 - C3 - C4 -4.08 ( 0.09) O2 - C2 - C3 - O3 176.36 ( 0.05) O1 - C2 - C3 - O3 0.09 ( 0.07) O3 - C3 - C4 - C5 -178.89 ( 0.07) C2 - C3 - C4 - C5 -0.16 ( 0.07) C3 - C4 - C5 - C6 -0.12 ( 0.07) C3 - O3 - C6 - C5 179.65 ( 0.06) C3 - O3 - C6 - C6_$1 0.17 ( 0.07) C4 - C5 - C6 - O3 -179.54 ( 0.09) C4 - C5 - C6 - C6_$1 FMAP and GRID set by program FMAP 2 1 9 GRID -4.167 -2 -2 4.167 2 2 R1 = 0.0429 for 2396 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.62 at 0.0609 0.1950 0.8854 [ 0.72 A from C2 ] Deepest hole -0.22 at 0.1765 0.3227 0.9756 [ 1.15 A from C3 ] Molecule 1 scale 0.880 inches = 2.236 cm per Angstrom C1 Q10 O1 Q11 Q12 C4 Q8 Q3 Q13 Q4 Q15 C5 C2 C3 Q1 Q6 Q5 Q7 O2 C6 O3 Q9 Q2 Q14 C6 Atom Peak x y z Sof Height Code/Atom Distances and Angles O1 0.42 0.3205 0.5236 0.6341 1.000 0.67 0 C2 1.342 0 Q8 0.675 2.4 0 Q10 0.737 108.5 106.6 O2 0.41 0.6336 0.6770 0.7191 1.000 0.58 0 C2 1.214 0 Q6 0.586 2.8 0 Q9 0.847 142.6 139.9 O3 0.43 0.5292 0.8658 0.5825 1.000 0.66 0 C3 1.374 0 C6 1.366 106.1 0 Q7 0.628 1.6 107.7 0 Q14 1.247 113.1 140.7 111.5 C1 0.19 0.3636 0.4291 0.7086 1.000 0.69 0 H1 0.969 0 H2 0.939 109.6 0 H3 0.930 115.2 108.5 0 Q12 0.640 29.6 136.6 90.7 0 Q10 0.723 109.8 110.6 102.9 101.9 0 Q13 1.372 56.5 130.8 58.8 34.3 118.5 C2 0.00 0.4685 0.6456 0.6498 1.000 0.63 0 O1 1.342 0 O2 1.214 124.5 0 C3 1.464 111.0 124.5 0 Q6 0.629 122.5 2.6 126.5 0 Q8 0.668 2.4 122.5 113.0 120.5 0 Q1 0.718 115.9 119.6 5.6 121.5 117.7 C3 0.00 0.4070 0.7353 0.5720 1.000 0.64 0 O3 1.374 0 C2 1.464 116.1 0 C4 1.368 110.6 133.3 0 Q4 0.682 109.7 133.8 5.6 0 Q7 0.747 1.4 114.7 112.0 111.0 0 Q1 0.752 111.2 5.3 138.1 138.9 109.9 0 Q11 1.167 171.3 72.5 60.9 62.1 172.5 77.2 C4 0.29 0.2528 0.7170 0.4873 1.000 0.61 0 C3 1.368 0 C5 1.426 106.4 0 H4 0.921 125.2 128.4 0 Q3 0.689 110.7 5.4 124.0 0 Q4 0.693 5.5 105.4 125.9 109.4 0 Q11 1.296 51.9 158.2 73.4 162.5 53.1 C5 0.25 0.2800 0.8435 0.4417 1.000 0.62 0 C4 1.426 0 C6 1.372 106.0 0 H5 0.983 127.7 126.3 0 Q5 0.725 109.6 6.7 122.6 0 Q3 0.743 5.0 110.0 123.6 113.9 C6 0.00 0.4486 0.9298 0.5023 1.000 0.65 0 O3 1.366 0 C5 1.372 110.9 0 Q5 0.658 114.9 7.4 0 Q2 0.721 116.0 133.1 128.7 1 C6 1.441 116.0 133.1 128.7 0.0 H1 0.00 0.2341 0.4622 0.7594 1.000 1.41 0 C1 0.969 0 Q12 0.520 37.4 H2 0.09 0.2580 0.3486 0.6868 1.000 0.68 0 C1 0.939 H3 0.00 0.6062 0.4134 0.7205 1.000 0.00 0 C1 0.930 H4 0.00 0.1520 0.6376 0.4659 1.000 0.60 0 C4 0.921 H5 0.00 0.2010 0.8651 0.3791 1.000 0.58 0 C5 0.983 0 Q15 0.726 141.9 Q1 0.62 0.4391 0.6950 0.6146 1.000 0.66 0 C2 0.718 0 C3 0.752 169.1 0 Q6 1.177 27.1 162.1 0 Q8 1.187 29.9 140.5 56.9 0 Q7 1.227 154.7 34.9 127.7 175.4 0 Q11 1.241 103.6 66.5 130.8 74.0 101.4 0 Q4 1.343 150.0 19.5 172.9 121.1 54.4 47.3 Q2 0.60 0.5000 1.0000 0.5000 0.500 0.67 0 C6 0.721 1 C6 0.721 180.0 0 Q5 1.243 24.4 155.6 Q3 0.55 0.2685 0.7747 0.4616 1.000 0.58 0 C4 0.689 0 C5 0.743 169.7 0 Q4 1.128 35.4 136.5 0 Q5 1.230 138.3 32.6 104.0 Q4 0.52 0.3466 0.7254 0.5283 1.000 0.57 0 C3 0.682 0 C4 0.693 168.9 0 Q11 1.040 82.5 94.7 0 Q3 1.128 146.0 35.2 129.9 0 Q7 1.178 36.3 144.3 118.7 110.2 0 Q1 1.343 21.6 155.0 61.2 167.3 57.8 Q5 0.51 0.3510 0.8942 0.4729 1.000 0.70 0 C5 0.725 0 C6 0.658 165.9 0 Q3 1.230 33.5 137.1 0 Q2 1.243 159.1 26.9 163.3 Q6 0.40 0.5490 0.6604 0.6867 1.000 0.62 0 O2 0.586 0 C2 0.629 174.6 0 Q8 1.126 153.4 30.7 0 Q1 1.177 144.5 31.4 62.0 0 Q9 1.349 23.9 161.3 136.3 152.3 Q7 0.39 0.4743 0.8059 0.5788 1.000 0.66 0 O3 0.628 0 C3 0.747 177.0 0 Q4 1.178 144.3 32.7 0 Q1 1.227 147.8 35.2 67.8 Q8 0.36 0.3930 0.5848 0.6438 1.000 0.67 0 O1 0.675 0 C2 0.668 175.2 0 Q6 1.126 155.0 28.8 0 Q10 1.134 38.6 145.1 116.5 0 Q1 1.187 143.8 32.4 61.1 177.1 0 Q11 1.461 89.2 86.9 115.7 127.6 54.7 Q9 0.28 0.6167 0.6813 0.7759 1.000 0.93 0 O2 0.847 0 Q6 1.349 16.3 Q10 0.21 0.3630 0.4799 0.6735 1.000 0.64 0 O1 0.737 0 C1 0.723 165.9 0 Q12 1.059 148.0 36.2 0 Q8 1.134 34.8 156.5 120.9 Q11 0.17 0.2806 0.6306 0.5531 1.000 0.65 0 C3 1.167 0 C4 1.296 67.3 0 Q4 1.040 35.4 32.2 0 Q1 1.241 36.2 103.5 71.5 0 Q8 1.461 87.6 154.8 122.7 51.3 Q12 0.16 0.3566 0.4654 0.7443 1.000 0.98 0 C1 0.640 0 H1 0.520 113.0 0 Q13 0.917 122.6 104.8 0 Q10 1.059 41.9 119.6 135.6 Q13 0.15 0.5243 0.4595 0.7913 1.000 0.72 0 C1 1.372 0 Q12 0.917 23.1 Q14 0.14 0.6842 0.8864 0.6575 1.000 0.65 0 O3 1.247 Q15 0.12 0.1527 0.9216 0.3497 1.000 0.72 0 H5 0.726 Code/Atom x y z Height Symmetry Transformation 1 C6 0.5514 1.0702 0.4977 0.7 1.0000-X 2.0000-Y 1.0000-Z Time profile in seconds ----------------------- 0.09: 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. 0.15: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.03: OSF, H-atoms from difference map 0.14: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.12: Structure factors and derivatives 0.00: 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 0.05: Other dependent quantities, CIF, tables 0.00: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.01: 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. +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + lobo001 finished at 09:37:46 Total elapsed time: 0.69 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++