++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXTL XLMP CRYSTAL STRUCTURE REFINEMENT - MULTI-CPU VERSION + + Copyright(c) Bruker AXS Inc. 1993-2017 Version 2017/1 + + lobo002 started at 11:49:32 on 28-Feb-2020 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Command line parameters: lobo002 -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 lobo002 in P2(1)/c CELL 1.54178 7.0807 12.7320 9.8149 90.000 102.330 90.000 ZERR 4.000 0.0002 0.0004 0.0003 0.000 0.002 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H O UNIT 40 40 8 V = 864.42 F(000) = 344.0 Mu = 0.70 mm-1 Cell Wt = 648.72 Rho = 1.246 TEMP -163.200 SIZE 0.074 0.087 0.144 L.S. 10 BOND $H ACTA CONF LIST 4 FMAP 2 PLAN 20 WGHT 0.100000 WGHT 0.1161 0.0715 FVAR 0.23328 O1 3 0.034267 0.586928 0.168610 11.00000 0.01880 0.02779 = 0.02683 -0.00081 0.00116 -0.00074 O2 3 0.515311 0.661296 0.348631 11.00000 0.01967 0.02693 = 0.02525 -0.00100 0.00118 -0.00190 C1 1 0.200465 0.587808 0.270609 11.00000 0.01740 0.02379 = 0.02618 -0.00328 0.00214 0.00244 C2 1 0.188184 0.515968 0.370468 11.00000 0.02341 0.02737 = 0.02980 0.00112 0.00314 0.00295 C3 1 0.002943 0.467010 0.327905 11.00000 0.02751 0.02641 = 0.03410 0.00105 0.00638 -0.00117 C4 1 -0.085235 0.512092 0.206086 11.00000 0.02149 0.02459 = 0.03115 -0.00524 0.00654 -0.00235 C5 1 -0.276803 0.498472 0.110980 11.00000 0.02369 0.03751 = 0.03570 -0.00766 0.00333 -0.00436 C6 1 0.345384 0.661555 0.250089 11.00000 0.01855 0.02408 = 0.02582 -0.00285 0.00229 0.00226 C7 1 0.353203 0.734756 0.150756 11.00000 0.02475 0.02708 = 0.03047 0.00224 0.00220 0.00251 C8 1 0.537497 0.783779 0.190240 11.00000 0.02686 0.02511 = 0.03329 0.00094 0.00543 -0.00180 C9 1 0.631852 0.737320 0.309412 11.00000 0.02151 0.02523 = 0.02926 -0.00411 0.00611 -0.00202 C10 1 0.826336 0.750196 0.399836 11.00000 0.02331 0.03603 = 0.03446 -0.00418 0.00185 -0.00592 H1 2 0.295316 0.499409 0.455478 11.00000 0.03660 H2 2 -0.055021 0.409857 0.379752 11.00000 0.03465 H3 2 -0.353655 0.442474 0.141787 11.00000 0.04302 H4 2 -0.264766 0.478130 0.021861 11.00000 0.05523 H5 2 -0.355428 0.565611 0.111289 11.00000 0.05039 H6 2 0.243090 0.750687 0.068610 11.00000 0.04892 H7 2 0.599303 0.838603 0.141059 11.00000 0.04421 H8 2 0.893438 0.806693 0.362916 11.00000 0.05629 H9 2 0.817431 0.769139 0.496577 11.00000 0.05220 H10 2 0.899751 0.683335 0.396713 11.00000 0.05188 HKLF 4 Covalent radii and connectivity table for lobo002 in P2(1)/c C 0.770 H 0.320 O 0.660 O1 - C1 C4 O2 - C6 C9 C1 - C2 O1 C6 C2 - C1 C3 C3 - C4 C2 C4 - C3 O1 C5 C5 - C4 C6 - C7 O2 C1 C7 - C6 C8 C8 - C9 C7 C9 - C8 O2 C10 C10 - C9 h k l Fo^2 Sigma Why rejected (first 50 of each listed) 0 1 0 0.09 0.01 systematically absent but >3sig(I) -1 0 3 0.68 0.06 systematically absent but >3sig(I) 2 0 3 0.07 0.02 systematically absent but >3sig(I) 341 Systematically absent reflections rejected 10976 Reflections read, of which 341 rejected -8 =< h =< 8, -15 =< k =< 15, -12 =< l =< 12, Max. 2-theta = 150.54 3 Systematic absence violations (I>3sig(I)) before merging 0 Inconsistent equivalents 1759 Unique reflections, of which 0 suppressed R(int) = 0.0514 R(sigma) = 0.0416 Friedel opposites merged Maximum memory for data reduction = 1495 / 17394 Number of data for d > 0.797A (CIF: max) and d > 0.833A (CIF: full) (ignoring systematic absences): Unique reflections found (point group) 1759 1560 Unique reflections possible (point group) 1779 1561 Unique reflections found (Laue group) 1759 1560 Unique reflections possible (Laue group) 1779 1561 Least-squares cycle 1 Maximum vector length = 623 Memory required = 29 / 1848 / 223916 wR2 = 0.1599 before cycle 1 for 1759 data and 149 / 149 parameters GooF = S = 1.097; Restrained GooF = 1.097 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1161 * P )^2 + 0.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23351 0.00118 0.199 OSF Mean shift/esd = 0.144 Maximum = -0.562 for y H9 Max. shift = 0.011 A for H9 Max. dU =-0.002 for H10 Least-squares cycle 2 Maximum vector length = 623 Memory required = 29 / 1848 / 223916 wR2 = 0.1595 before cycle 2 for 1759 data and 149 / 149 parameters GooF = S = 1.096; Restrained GooF = 1.096 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1161 * P )^2 + 0.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23340 0.00117 -0.095 OSF Mean shift/esd = 0.052 Maximum = -0.268 for y H9 Max. shift = 0.006 A for H9 Max. dU =-0.001 for H6 Least-squares cycle 3 Maximum vector length = 623 Memory required = 29 / 1848 / 223916 wR2 = 0.1594 before cycle 3 for 1759 data and 149 / 149 parameters GooF = S = 1.096; Restrained GooF = 1.096 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1161 * P )^2 + 0.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23339 0.00117 -0.010 OSF Mean shift/esd = 0.006 Maximum = -0.044 for y H9 Max. shift = 0.001 A for H9 Max. dU = 0.000 for H2 Least-squares cycle 4 Maximum vector length = 623 Memory required = 29 / 1848 / 223916 wR2 = 0.1594 before cycle 4 for 1759 data and 149 / 149 parameters GooF = S = 1.096; Restrained GooF = 1.096 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1161 * P )^2 + 0.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23339 0.00117 -0.001 OSF Mean shift/esd = 0.002 Maximum = 0.013 for x H5 Max. shift = 0.000 A for H5 Max. dU = 0.000 for H6 Least-squares cycle 5 Maximum vector length = 623 Memory required = 29 / 1848 / 223916 wR2 = 0.1594 before cycle 5 for 1759 data and 149 / 149 parameters GooF = S = 1.096; Restrained GooF = 1.096 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1161 * P )^2 + 0.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23339 0.00117 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.003 for y H9 Max. shift = 0.000 A for H5 Max. dU = 0.000 for H6 Least-squares cycle 6 Maximum vector length = 623 Memory required = 29 / 1848 / 223916 wR2 = 0.1594 before cycle 6 for 1759 data and 149 / 149 parameters GooF = S = 1.096; Restrained GooF = 1.096 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1161 * P )^2 + 0.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23339 0.00117 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y H9 Max. shift = 0.000 A for H9 Max. dU = 0.000 for H10 Least-squares cycle 7 Maximum vector length = 623 Memory required = 29 / 1848 / 223916 wR2 = 0.1594 before cycle 7 for 1759 data and 149 / 149 parameters GooF = S = 1.096; Restrained GooF = 1.096 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1161 * P )^2 + 0.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23339 0.00117 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C8 Max. shift = 0.000 A for H3 Max. dU = 0.000 for H6 Least-squares cycle 8 Maximum vector length = 623 Memory required = 29 / 1848 / 223916 wR2 = 0.1594 before cycle 8 for 1759 data and 149 / 149 parameters GooF = S = 1.096; Restrained GooF = 1.096 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1161 * P )^2 + 0.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23339 0.00117 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C9 Max. shift = 0.000 A for H5 Max. dU = 0.000 for H6 Least-squares cycle 9 Maximum vector length = 623 Memory required = 29 / 1848 / 223916 wR2 = 0.1594 before cycle 9 for 1759 data and 149 / 149 parameters GooF = S = 1.096; Restrained GooF = 1.096 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1161 * P )^2 + 0.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23339 0.00117 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C9 Max. shift = 0.000 A for H10 Max. dU = 0.000 for H4 Least-squares cycle 10 Maximum vector length = 623 Memory required = 29 / 1848 / 223916 wR2 = 0.1594 before cycle 10 for 1759 data and 149 / 149 parameters GooF = S = 1.096; Restrained GooF = 1.096 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1161 * P )^2 + 0.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23339 0.00117 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C9 Max. shift = 0.000 A for H2 Max. dU = 0.000 for H5 Largest correlation matrix elements 0.514 U11 O1 / OSF 0.501 U11 O2 / OSF 0.501 U33 O2 / OSF lobo002 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq O1 0.03427 0.58693 0.16863 1.00000 0.01884 0.02756 0.02664 -0.00075 0.00116 -0.00073 0.02490 0.00158 0.00012 0.00007 0.00009 0.00000 0.00051 0.00053 0.00047 0.00031 0.00035 0.00033 0.00031 O2 0.51529 0.66128 0.34864 1.00000 0.01969 0.02681 0.02512 -0.00094 0.00120 -0.00183 0.02441 0.00154 0.00012 0.00007 0.00008 0.00000 0.00052 0.00051 0.00048 0.00031 0.00036 0.00033 0.00031 C1 0.20045 0.58779 0.27064 1.00000 0.01755 0.02361 0.02594 -0.00325 0.00212 0.00243 0.02274 0.00217 0.00017 0.00009 0.00012 0.00000 0.00062 0.00063 0.00059 0.00042 0.00046 0.00045 0.00034 C2 0.18816 0.51598 0.37047 1.00000 0.02339 0.02734 0.02963 0.00108 0.00314 0.00286 0.02716 0.00239 0.00019 0.00010 0.00013 0.00000 0.00070 0.00068 0.00063 0.00046 0.00050 0.00049 0.00035 C3 0.00291 0.46700 0.32781 1.00000 0.02759 0.02613 0.03411 0.00103 0.00646 -0.00108 0.02930 0.00240 0.00019 0.00010 0.00013 0.00000 0.00072 0.00066 0.00064 0.00048 0.00053 0.00050 0.00035 C4 -0.08523 0.51206 0.20615 1.00000 0.02137 0.02455 0.03115 -0.00536 0.00649 -0.00227 0.02556 0.00226 0.00019 0.00010 0.00013 0.00000 0.00067 0.00062 0.00064 0.00044 0.00050 0.00046 0.00035 C5 -0.27679 0.49849 0.11097 1.00000 0.02348 0.03750 0.03569 -0.00773 0.00322 -0.00469 0.03269 0.00257 0.00020 0.00012 0.00015 0.00000 0.00073 0.00078 0.00069 0.00052 0.00056 0.00057 0.00038 C6 0.34538 0.66157 0.25006 1.00000 0.01856 0.02394 0.02578 -0.00305 0.00234 0.00224 0.02312 0.00216 0.00017 0.00009 0.00012 0.00000 0.00065 0.00062 0.00060 0.00043 0.00048 0.00044 0.00034 C7 0.35313 0.73475 0.15080 1.00000 0.02470 0.02701 0.03023 0.00212 0.00223 0.00233 0.02786 0.00244 0.00019 0.00010 0.00013 0.00000 0.00072 0.00065 0.00065 0.00046 0.00051 0.00050 0.00035 C8 0.53757 0.78380 0.19028 1.00000 0.02679 0.02507 0.03296 0.00094 0.00539 -0.00186 0.02842 0.00247 0.00019 0.00010 0.00013 0.00000 0.00069 0.00065 0.00065 0.00047 0.00052 0.00049 0.00035 C9 0.63182 0.73734 0.30938 1.00000 0.02157 0.02507 0.02922 -0.00429 0.00609 -0.00199 0.02519 0.00229 0.00018 0.00010 0.00013 0.00000 0.00067 0.00062 0.00064 0.00044 0.00051 0.00047 0.00034 C10 0.82641 0.75018 0.39992 1.00000 0.02330 0.03585 0.03443 -0.00410 0.00187 -0.00591 0.03184 0.00253 0.00020 0.00012 0.00015 0.00000 0.00072 0.00075 0.00072 0.00052 0.00055 0.00055 0.00037 H1 0.29431 0.50047 0.45520 1.00000 0.03693 0.03190 0.00255 0.00141 0.00169 0.00000 0.00435 H2 -0.05507 0.41042 0.37864 1.00000 0.03434 0.03235 0.00247 0.00137 0.00171 0.00000 0.00409 H3 -0.35319 0.44277 0.14212 1.00000 0.04468 0.03469 0.00267 0.00158 0.00185 0.00000 0.00477 H4 -0.26446 0.47862 0.02077 1.00000 0.05481 0.03806 0.00293 0.00164 0.00198 0.00000 0.00556 H5 -0.35614 0.56605 0.11033 1.00000 0.04927 0.03701 0.00278 0.00161 0.00194 0.00000 0.00497 H6 0.24418 0.74995 0.06846 1.00000 0.04640 0.03588 0.00269 0.00159 0.00188 0.00000 0.00490 H7 0.59787 0.83841 0.14108 1.00000 0.04362 0.03517 0.00268 0.00155 0.00189 0.00000 0.00458 H8 0.89282 0.80645 0.36337 1.00000 0.05684 0.03904 0.00307 0.00171 0.00211 0.00000 0.00560 H9 0.81758 0.76774 0.49693 1.00000 0.05173 0.03838 0.00296 0.00157 0.00208 0.00000 0.00514 H10 0.89959 0.68307 0.39672 1.00000 0.04920 0.03622 0.00285 0.00160 0.00188 0.00000 0.00505 Final Structure Factor Calculation for lobo002 in P2(1)/c Total number of l.s. parameters = 149 Maximum vector length = 623 Memory required = 29 / 1699 / 26790 wR2 = 0.1594 before cycle 11 for 1759 data and 0 / 149 parameters GooF = S = 1.096; Restrained GooF = 1.096 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1161 * P )^2 + 0.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 wR2 = 0.1594, GooF = S = 1.096, Restrained GooF = 1.096 for all data R1 = 0.0556 for 1537 Fo > 4sig(Fo) and 0.0597 for all 1759 data Occupancy sum of asymmetric unit = 12.00 for non-hydrogen and 10.00 for H and D atoms Principal mean square atomic displacements U 0.0292 0.0275 0.0179 O1 0.0279 0.0272 0.0181 O2 0.0302 0.0214 0.0167 C1 0.0312 0.0288 0.0215 C2 0.0344 0.0282 0.0253 C3 0.0342 0.0224 0.0201 C4 0.0444 0.0326 0.0211 C5 0.0299 0.0217 0.0177 C6 0.0331 0.0285 0.0220 C7 0.0337 0.0278 0.0238 C8 0.0319 0.0230 0.0207 C9 0.0393 0.0362 0.0200 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 0.006 0.011 0.017 0.024 0.034 0.044 0.057 0.079 0.111 1.000 Number in group 199. 171. 167. 168. 186. 170. 171. 180. 171. 176. GooF 0.819 1.132 1.238 1.382 1.144 0.966 1.047 1.080 0.903 1.178 K 1.171 0.961 0.972 1.023 1.017 1.019 1.046 1.020 1.018 0.980 Resolution(A) 0.80 0.83 0.86 0.90 0.95 1.01 1.09 1.19 1.37 1.72 inf Number in group 176. 179. 173. 177. 175. 179. 172. 178. 173. 177. GooF 1.197 1.020 0.867 1.017 0.955 0.867 0.995 1.169 1.285 1.442 K 1.047 1.074 1.052 1.066 1.013 0.972 0.922 1.007 1.068 0.970 R1 0.087 0.068 0.055 0.056 0.040 0.038 0.056 0.055 0.061 0.074 Recommended weighting scheme: WGHT 0.1134 0.0749 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 6 4 543.88 1062.00 4.64 0.223 1.10 5 0 6 23.96 12.20 4.09 0.024 0.95 3 1 5 19.46 10.98 3.96 0.023 1.33 0 8 0 916.89 563.36 3.81 0.162 1.59 2 2 1 5.79 2.76 3.79 0.011 2.75 0 6 1 163.50 105.89 3.42 0.070 2.07 6 1 4 21.94 13.09 3.39 0.025 0.96 -4 6 3 3.14 1.01 3.31 0.007 1.32 1 8 1 1599.01 1071.21 3.31 0.224 1.52 8 3 0 28.53 18.14 3.29 0.029 0.85 1 9 0 96.34 64.02 3.23 0.055 1.39 5 0 2 3.50 7.12 3.20 0.018 1.26 0 5 1 215.37 143.12 3.08 0.082 2.46 0 6 3 85.81 57.79 3.06 0.052 1.77 0 6 5 0.31 1.86 3.01 0.009 1.42 6 4 3 6.12 11.62 3.00 0.023 0.97 5 3 8 6.71 3.69 2.99 0.013 0.81 -8 3 7 45.35 28.34 2.95 0.036 0.80 7 5 0 14.92 8.26 2.95 0.020 0.92 2 1 4 18.10 11.92 2.89 0.024 1.78 0 4 0 7631.10 5086.82 2.88 0.487 3.18 0 5 2 779.47 545.08 2.86 0.159 2.25 0 8 2 1.25 3.12 2.86 0.012 1.51 -1 0 12 3.79 7.32 2.85 0.018 0.81 4 0 4 8.80 4.98 2.83 0.015 1.28 2 5 1 1.21 0.31 2.78 0.004 1.96 1 8 9 1.85 3.65 2.77 0.013 0.86 1 7 1 84.95 59.97 2.77 0.053 1.71 0 8 8 4.05 2.13 2.77 0.010 0.96 4 3 3 17.44 11.45 2.72 0.023 1.33 4 3 4 24.49 16.49 2.71 0.028 1.22 -6 7 6 17.64 11.09 2.71 0.023 0.91 -3 5 2 2.24 4.23 2.71 0.014 1.70 0 7 1 97.34 69.63 2.69 0.057 1.79 -1 5 3 174.35 108.96 2.66 0.071 1.99 1 10 0 450.54 323.77 2.62 0.123 1.25 6 1 7 8.62 5.08 2.62 0.015 0.80 -1 5 2 353.09 254.47 2.60 0.109 2.20 0 0 2 7864.81 11329.18 2.57 0.727 4.79 -1 8 1 654.74 478.73 2.54 0.149 1.54 -1 6 2 1536.29 1127.95 2.51 0.229 1.91 -6 6 3 7.09 11.08 2.49 0.023 1.02 7 6 1 56.60 40.94 2.46 0.044 0.88 0 4 2 5.32 8.35 2.46 0.020 2.65 7 1 5 14.97 10.13 2.46 0.022 0.81 -6 6 1 8.34 12.61 2.46 0.024 1.03 7 2 5 11.90 7.50 2.45 0.019 0.80 -2 6 1 110.59 81.22 2.44 0.062 1.81 7 3 1 12.90 19.81 2.44 0.030 0.94 7 0 4 38.92 26.56 2.43 0.035 0.85 Bond lengths and angles O1 - Distance Angles C1 1.3726 (0.0014) C4 1.3760 (0.0015) 106.90 (0.09) O1 C1 O2 - Distance Angles C6 1.3735 (0.0014) C9 1.3794 (0.0015) 106.71 (0.09) O2 C6 C1 - Distance Angles C2 1.3564 (0.0017) O1 1.3726 (0.0014) 110.14 (0.10) C6 1.4370 (0.0018) 134.43 (0.12) 115.43 (0.10) C1 C2 O1 C2 - Distance Angles C1 1.3564 (0.0017) C3 1.4318 (0.0018) 106.17 (0.11) H1 1.0142 (0.0166) 124.95 (1.04) 128.85 (1.03) C2 C1 C3 C3 - Distance Angles C4 1.3514 (0.0018) C2 1.4318 (0.0018) 107.15 (0.12) H2 1.0119 (0.0168) 125.34 (0.99) 127.49 (0.98) C3 C4 C2 C4 - Distance Angles C3 1.3514 (0.0018) O1 1.3760 (0.0015) 109.65 (0.11) C5 1.4836 (0.0018) 133.99 (0.13) 116.36 (0.11) C4 C3 O1 C5 - Distance Angles C4 1.4836 (0.0018) H3 0.9799 (0.0195) 112.29 (1.07) H4 0.9426 (0.0195) 111.53 (1.25) 105.47 (1.60) H5 1.0267 (0.0202) 109.38 (1.11) 105.70 (1.46) 112.31 (1.62) C5 C4 H3 H4 C6 - Distance Angles C7 1.3576 (0.0017) O2 1.3735 (0.0014) 110.11 (0.11) C1 1.4370 (0.0018) 133.56 (0.12) 116.34 (0.10) C6 C7 O2 C7 - Distance Angles C6 1.3576 (0.0017) C8 1.4246 (0.0019) 106.31 (0.12) H6 1.0097 (0.0187) 124.39 (1.11) 129.27 (1.11) C7 C6 C8 C8 - Distance Angles C9 1.3523 (0.0017) C7 1.4246 (0.0019) 107.33 (0.11) H7 0.9935 (0.0192) 122.85 (1.08) 129.70 (1.07) C8 C9 C7 C9 - Distance Angles C8 1.3523 (0.0017) O2 1.3794 (0.0015) 109.53 (0.11) C10 1.4805 (0.0018) 134.01 (0.12) 116.45 (0.11) C9 C8 O2 C10 - Distance Angles C9 1.4805 (0.0018) H8 0.9671 (0.0218) 108.85 (1.24) H9 0.9929 (0.0195) 111.06 (1.21) 108.91 (1.60) H10 1.0032 (0.0203) 107.93 (1.12) 108.90 (1.60) 111.13 (1.57) C10 C9 H8 H9 Selected torsion angles -0.07 ( 0.13) C4 - O1 - C1 - C2 179.87 ( 0.09) C4 - O1 - C1 - C6 0.20 ( 0.14) O1 - C1 - C2 - C3 -179.72 ( 0.13) C6 - C1 - C2 - C3 -0.26 ( 0.15) C1 - C2 - C3 - C4 0.23 ( 0.14) C2 - C3 - C4 - O1 -178.76 ( 0.14) C2 - C3 - C4 - C5 -0.10 ( 0.13) C1 - O1 - C4 - C3 179.08 ( 0.10) C1 - O1 - C4 - C5 0.33 ( 0.13) C9 - O2 - C6 - C7 -179.75 ( 0.09) C9 - O2 - C6 - C1 -178.13 ( 0.13) C2 - C1 - C6 - C7 1.95 ( 0.20) O1 - C1 - C6 - C7 1.97 ( 0.21) C2 - C1 - C6 - O2 -177.96 ( 0.08) O1 - C1 - C6 - O2 -0.63 ( 0.14) O2 - C6 - C7 - C8 179.46 ( 0.13) C1 - C6 - C7 - C8 0.70 ( 0.14) C6 - C7 - C8 - C9 -0.51 ( 0.14) C7 - C8 - C9 - O2 178.36 ( 0.13) C7 - C8 - C9 - C10 0.13 ( 0.13) C6 - O2 - C9 - C8 -178.96 ( 0.10) C6 - O2 - C9 - C10 FMAP and GRID set by program FMAP 2 3 14 GRID -2.273 -2 -2 2.273 2 2 R1 = 0.0596 for 1759 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.32 at 0.9121 0.0056 0.1225 [ 0.74 A from C2 ] Deepest hole -0.43 at 0.0152 0.5480 0.2487 [ 0.87 A from C4 ] Mean = 0.00, Rms deviation from mean = 0.10, Highest memory used = 1793 / 14597 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including eq.) Q1 1 0.0879 0.5056 0.3775 1.00000 0.05 0.32 0.74 C2 0.85 C3 1.50 H1 1.58 H2 Q2 1 0.4524 0.7600 0.1493 1.00000 0.05 0.30 0.72 C8 0.78 C7 1.45 H7 1.52 H6 Q3 1 0.9392 0.7382 0.3741 1.00000 0.05 0.28 0.80 H10 0.90 C10 0.93 H8 1.67 H9 Q4 1 0.7397 0.7441 0.3551 1.00000 0.05 0.28 0.68 C10 0.80 C9 1.33 H8 1.36 H10 Q5 1 0.0000 0.5000 0.0000 0.50000 0.05 0.27 1.95 H4 1.96 O1 2.24 C4 2.44 C5 Q6 1 -0.3789 0.5152 0.1347 1.00000 0.05 0.27 0.72 H5 0.83 C5 0.94 H3 1.59 H4 Q7 1 -0.1731 0.5072 0.1609 1.00000 0.05 0.27 0.69 C4 0.80 C5 1.44 H4 1.49 H5 Q8 1 0.4005 0.6680 0.3807 1.00000 0.05 0.27 0.94 O2 1.26 C6 1.89 C1 2.11 C9 Q9 1 0.6025 0.7583 0.5296 1.00000 0.05 0.26 1.63 H9 1.65 H7 1.82 C8 2.14 O2 Q10 1 0.1630 0.5791 0.1547 1.00000 0.05 0.26 0.96 O1 1.12 C1 1.77 C6 2.11 C4 Q11 1 -0.1682 0.5010 -0.0649 1.00000 0.05 0.25 1.22 H4 1.90 O1 2.03 C5 2.28 C1 Q12 1 -0.0718 0.5971 0.1763 1.00000 0.05 0.24 0.78 O1 1.13 C4 1.92 C5 1.96 C1 Q13 1 0.2582 0.6436 0.2772 1.00000 0.05 0.24 0.76 C6 0.82 C1 1.82 O2 1.86 O1 Q14 1 0.3033 0.6039 0.2458 1.00000 0.05 0.24 0.79 C6 0.84 C1 1.78 O2 1.91 O1 Q15 1 -0.2456 0.5058 -0.0053 1.00000 0.05 0.23 0.47 H4 1.21 C5 1.69 H5 1.95 H3 Q16 1 0.6329 0.6546 0.3469 1.00000 0.05 0.22 0.84 O2 1.12 C9 1.82 C10 1.88 H10 Q17 1 0.1907 0.5042 0.5514 1.00000 0.05 0.21 1.31 H1 1.69 H2 1.78 C2 2.03 C3 Q18 1 0.2603 0.7571 0.1154 1.00000 0.05 0.21 0.46 H6 0.73 C7 1.80 C6 1.97 C8 Q19 1 0.7515 0.7370 0.6082 1.00000 0.05 0.21 1.34 H9 1.54 H7 1.88 C8 2.23 C10 Q20 1 0.3454 0.5072 0.4080 1.00000 0.05 0.20 0.65 H1 1.10 C2 1.83 C1 2.26 H7 Shortest distances between peaks (including symmetry equivalents) 13 14 0.70 11 15 0.88 9 19 1.20 5 11 1.22 10 14 1.23 8 13 1.31 2 18 1.33 7 12 1.34 10 11 1.35 4 16 1.36 3 4 1.39 6 7 1.43 10 13 1.49 8 14 1.58 7 15 1.60 1 17 1.71 5 15 1.73 10 12 1.74 8 16 1.75 2 9 1.76 1 20 1.78 6 15 1.83 17 20 1.96 5 10 1.98 14 20 1.98 10 15 2.01 8 20 2.11 8 9 2.15 4 9 2.15 13 18 2.15 13 20 2.17 5 7 2.20 7 11 2.22 1 17 2.23 2 19 2.24 12 15 2.26 11 14 2.26 5 12 2.27 9 16 2.27 14 18 2.32 1 12 2.36 6 12 2.37 3 16 2.38 12 13 2.41 14 16 2.42 10 18 2.42 11 11 2.45 1 13 2.45 4 19 2.45 4 19 2.47 16 17 2.47 12 19 2.47 2 16 2.48 1 7 2.50 2 14 2.53 2 13 2.53 20 20 2.53 1 14 2.53 1 10 2.54 11 12 2.54 2 4 2.55 7 10 2.56 13 16 2.60 12 14 2.60 11 12 2.62 3 12 2.63 2 8 2.65 4 8 2.65 17 17 2.68 3 19 2.68 14 15 2.70 6 15 2.70 10 20 2.70 6 11 2.71 6 16 2.72 8 10 2.73 16 19 2.73 9 18 2.74 2 8 2.74 11 13 2.75 7 11 2.78 8 18 2.82 6 6 2.85 7 17 2.86 8 18 2.86 11 15 2.86 3 19 2.89 3 13 2.89 3 18 2.91 16 20 2.92 6 14 2.93 1 1 2.94 16 19 2.99 10 11 3.00 Time profile in seconds ----------------------- 0.21: 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. 0.67: Read intensity data, sort/merge etc. 0.02: Set up constraints 0.13: OSF, H-atoms from difference map 0.53: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.45: Structure factors, sum l.s. matrics 0.31: 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 0.10: Other dependent quantities, CIF, tables 0.12: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.04: 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. +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + lobo002 finished at 11:49:36 Total elapsed time: 3.62 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++