+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL - CRYSTAL STRUCTURE REFINEMENT - MULTI-CPU VERSION + + Copyright(C) George M. Sheldrick 1993-2023 Version 2019/3 + + rudi005 started at 16:12:22 on 29-Apr-2026 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Command line parameters: rudi005 -a50000 -b3000 -c624 -g0 -m0 -t12 -a sets the approximate maximum number of atoms including hydrogens. -b sets the maximum number of full-matrix parameters (not used by CGLS). For example -b9000 allows refinement of 1000 anisotropic atoms or 3000 with BLOC 1. For a 32-bit version, -b times the square root of the number of threads should not exceed about 65500. -c sets the reflection buffer size. This depends on the CPU cache size but will rarely need changing. -g sets the number of reflection groups used for calculating R_complete, This must be greater than 1 but not greater than the total number of reflections for refinement. -m sets the current reflection group number. This may not be less than 1 nor greater than the number set by -g. These command line flags override other ways of defining free-R reflections. The -m value is also used as a seed for the WIGL pseudo-random shifts. -t sets the number of threads, otherwise it is set to the apparent number of CPUs. For optimal performance on hyperthreading systems, -t should be set to a little more than half the number of CPUs; e.g. -t4 or -t5 for an Intel i7 processor. Running 12 threads on 16 processors TITL rudi005_a.res in P2(1)2(1)2(1) REM Old TITL rudi005 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1): R1 0.096, Rweak 0.029, Alpha 0.009 REM 2.105 for 29 systematic absences, Orientation as input REM Flack x = 0.037 ( 0.007 ) from 3453 Parsons' quotients REM Formula found by SHELXT: C35 N2 I5 CELL 1.54178 11.2013 16.6942 22.1759 90 90 90 ZERR 4 0.0003 0.0004 0.0006 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 I In N UNIT 144 208 16 4 4 V = 4146.82 F(000) = 2144.0 Mu = 28.09 mm-1 Cell Wt = 4484.81 Rho = 1.796 SIMU 0.002 0.004 2 N1 > C36 RIGU N1 > C36 L.S. 20 PLAN 5 SIZE 0.065 0.126 0.131 TEMP -173.15 CONF BOND list 4 fmap 2 ACTA MORE -1 BOND $H OMIT -4 -1 -1 OMIT -2 -3 -27 OMIT -1 -8 -25 OMIT 0 1 2 OMIT 0 4 26 OMIT 1 1 1 OMIT 6 0 14 OMIT 8 0 0 OMIT 8 8 19 OMIT 13 1 3 OMIT 13 3 1 WGHT 0.0656 10.4711 FVAR 0.19695 REM REM REM I1 3 0.301727 0.538440 0.499559 11.00000 0.01139 0.01793 = 0.01646 -0.00336 -0.00016 0.00031 I2 3 0.036480 0.619846 0.367444 11.00000 0.01320 0.02349 = 0.03111 0.01364 -0.00171 0.00353 I3 3 -0.082476 0.508296 0.541055 11.00000 0.01826 0.02977 = 0.02892 0.00104 0.01011 -0.00156 I4 3 0.079513 0.360787 0.400660 11.00000 0.03675 0.01800 = 0.01717 -0.00165 -0.00027 -0.00583 In1 4 0.083254 0.507524 0.452830 11.00000 0.01033 0.01401 = 0.01543 0.00224 0.00006 -0.00002 N1 5 0.606386 0.511640 0.348183 11.00000 0.00482 0.01133 = 0.01238 0.00108 0.00195 -0.00103 C1 1 0.735418 0.501434 0.361996 11.00000 0.00627 0.01297 = 0.02077 0.00238 -0.00281 -0.00053 AFIX 137 H1a 2 0.774354 0.472890 0.328763 11.00000 -1.50000 H1b 2 0.744347 0.470531 0.399296 11.00000 -1.50000 H1c 2 0.772578 0.554157 0.367028 11.00000 -1.50000 AFIX 0 C2 1 0.563460 0.586948 0.337633 11.00000 0.00652 0.01207 = 0.01169 0.00038 0.00175 0.00039 C3 1 0.441044 0.595671 0.329277 11.00000 0.00581 0.01341 = 0.01265 0.00034 0.00103 0.00132 AFIX 43 H3 2 0.408822 0.647383 0.321873 11.00000 -1.20000 AFIX 0 C4 1 0.366375 0.530876 0.331565 11.00000 0.00637 0.01489 = 0.01234 -0.00008 0.00131 0.00123 AFIX 43 H4 2 0.282590 0.537986 0.327625 11.00000 -1.20000 AFIX 0 C5 1 0.413494 0.454662 0.339667 11.00000 0.00646 0.01379 = 0.01137 -0.00077 0.00062 -0.00055 AFIX 43 H5 2 0.362099 0.409401 0.340221 11.00000 -1.20000 AFIX 0 C6 1 0.534344 0.444736 0.346876 11.00000 0.00541 0.01191 = 0.01045 -0.00031 0.00159 -0.00039 C7 1 0.703655 0.677204 0.281071 11.00000 0.00847 0.01124 = 0.01241 0.00052 0.00214 0.00053 C8 1 0.773891 0.746459 0.280757 11.00000 0.00700 0.01232 = 0.01103 0.00101 0.00155 0.00034 AFIX 43 H8 2 0.814495 0.760495 0.244660 11.00000 -1.20000 AFIX 0 C9 1 0.787001 0.795797 0.330988 11.00000 0.00618 0.01198 = 0.01043 0.00102 0.00130 0.00033 C10 1 0.727904 0.773638 0.383644 11.00000 0.00678 0.01183 = 0.01115 0.00069 0.00108 0.00129 AFIX 43 H10 2 0.735819 0.806757 0.418250 11.00000 -1.20000 AFIX 0 C11 1 0.657538 0.704865 0.387771 11.00000 0.00760 0.01169 = 0.01142 0.00112 0.00127 0.00015 C12 1 0.645191 0.657181 0.335644 11.00000 0.00687 0.01068 = 0.01170 0.00091 0.00170 0.00027 C13 1 0.689677 0.628987 0.223757 11.00000 0.01384 0.01377 = 0.01403 -0.00026 0.00375 -0.00031 AFIX 13 H13 2 0.631385 0.584963 0.232013 11.00000 -1.20000 AFIX 0 C14 1 0.806432 0.590686 0.204343 11.00000 0.02136 0.02382 = 0.02115 -0.00302 0.00477 0.00505 AFIX 137 H14a 2 0.865625 0.632595 0.196367 11.00000 -1.50000 H14b 2 0.793421 0.559218 0.167620 11.00000 -1.50000 H14c 2 0.835622 0.555518 0.236509 11.00000 -1.50000 AFIX 0 C15 1 0.638255 0.680971 0.172742 11.00000 0.02197 0.02197 = 0.01526 -0.00012 0.00209 -0.00103 AFIX 137 H15a 2 0.560025 0.701764 0.184845 11.00000 -1.50000 H15b 2 0.629531 0.648481 0.136200 11.00000 -1.50000 H15c 2 0.692439 0.725796 0.164670 11.00000 -1.50000 AFIX 0 C16 1 0.859995 0.871831 0.332384 11.00000 0.00871 0.01324 = 0.01125 0.00183 0.00202 -0.00177 AFIX 13 H16 2 0.811670 0.913840 0.353301 11.00000 -1.20000 AFIX 0 C17 1 0.974525 0.858862 0.369034 11.00000 0.01285 0.02019 = 0.01174 0.00312 0.00196 -0.00427 AFIX 137 H17a 2 0.953797 0.840492 0.409680 11.00000 -1.50000 H17b 2 1.018745 0.909390 0.371713 11.00000 -1.50000 H17c 2 1.024199 0.818420 0.349122 11.00000 -1.50000 AFIX 0 C18 1 0.892379 0.903666 0.269657 11.00000 0.01937 0.01873 = 0.01804 0.00580 0.00056 -0.00948 AFIX 137 H18a 2 0.925665 0.957731 0.273362 11.00000 -1.50000 H18b 2 0.820553 0.905375 0.244457 11.00000 -1.50000 H18c 2 0.951626 0.868248 0.251044 11.00000 -1.50000 AFIX 0 C19 1 0.594549 0.685016 0.446728 11.00000 0.00950 0.01663 = 0.01221 0.00175 0.00292 0.00173 AFIX 13 H19 2 0.564103 0.628823 0.443994 11.00000 -1.20000 AFIX 0 C20 1 0.681676 0.689666 0.500340 11.00000 0.00856 0.03097 = 0.01233 0.00344 0.00188 -0.00039 AFIX 137 H20a 2 0.754083 0.659197 0.490897 11.00000 -1.50000 H20b 2 0.643650 0.667018 0.536302 11.00000 -1.50000 H20c 2 0.702735 0.745743 0.507933 11.00000 -1.50000 AFIX 0 C21 1 0.487897 0.740419 0.456679 11.00000 0.01502 0.02476 = 0.01539 0.00280 0.00700 0.00702 AFIX 137 H21a 2 0.513940 0.796301 0.453492 11.00000 -1.50000 H21b 2 0.454384 0.730940 0.496872 11.00000 -1.50000 H21c 2 0.426915 0.729576 0.426060 11.00000 -1.50000 AFIX 0 C22 1 0.587588 0.323792 0.407797 11.00000 0.01187 0.01384 = 0.01274 -0.00036 0.00076 0.00185 C23 1 0.639133 0.247699 0.410536 11.00000 0.01148 0.01401 = 0.01438 0.00041 -0.00091 0.00173 AFIX 43 H23 2 0.637588 0.219177 0.447597 11.00000 -1.20000 AFIX 0 C24 1 0.692936 0.212328 0.360269 11.00000 0.01043 0.01402 = 0.01640 0.00014 -0.00122 0.00191 C25 1 0.692596 0.254039 0.305192 11.00000 0.00890 0.01363 = 0.01442 -0.00075 0.00155 0.00048 AFIX 43 H25 2 0.728112 0.230030 0.270743 11.00000 -1.20000 AFIX 0 C26 1 0.641466 0.329633 0.299980 11.00000 0.00840 0.01340 = 0.01244 0.00082 0.00194 0.00004 C27 1 0.589832 0.364534 0.351998 11.00000 0.00869 0.01276 = 0.01177 -0.00061 0.00159 0.00026 C28 1 0.530955 0.359186 0.463565 11.00000 0.01723 0.01661 = 0.01349 -0.00011 0.00316 0.00425 AFIX 13 H28 2 0.504224 0.414773 0.453563 11.00000 -1.20000 AFIX 0 C29 1 0.420869 0.310817 0.481720 11.00000 0.02199 0.02401 = 0.01598 0.00136 0.00602 0.00405 AFIX 137 H29a 2 0.362236 0.312154 0.448936 11.00000 -1.50000 H29b 2 0.385632 0.334052 0.518192 11.00000 -1.50000 H29c 2 0.444132 0.255223 0.489677 11.00000 -1.50000 AFIX 0 C30 1 0.618878 0.364586 0.516655 11.00000 0.02622 0.02358 = 0.01654 -0.00453 0.00260 -0.00358 AFIX 137 H30a 2 0.640820 0.310483 0.529741 11.00000 -1.50000 H30b 2 0.581142 0.393238 0.550187 11.00000 -1.50000 H30c 2 0.690712 0.393479 0.503875 11.00000 -1.50000 AFIX 0 C31 1 0.744038 0.129029 0.364804 11.00000 0.01299 0.01647 = 0.01907 0.00059 -0.00145 0.00554 AFIX 13 H31 2 0.742550 0.112858 0.408217 11.00000 -1.20000 AFIX 0 C32 1 0.665930 0.069268 0.329322 11.00000 0.02174 0.01737 = 0.03072 -0.00161 -0.00734 0.00829 AFIX 137 H32a 2 0.661829 0.085795 0.286968 11.00000 -1.50000 H32b 2 0.585329 0.068441 0.346500 11.00000 -1.50000 H32c 2 0.701012 0.015606 0.331959 11.00000 -1.50000 AFIX 0 C33 1 0.872355 0.124744 0.343213 11.00000 0.01276 0.02278 = 0.02543 0.00125 0.00132 0.00913 AFIX 137 H33a 2 0.907113 0.073219 0.355051 11.00000 -1.50000 H33b 2 0.918385 0.168405 0.361437 11.00000 -1.50000 H33c 2 0.874480 0.129841 0.299201 11.00000 -1.50000 AFIX 0 C34 1 0.634290 0.372733 0.239470 11.00000 0.00932 0.01454 = 0.01351 0.00190 0.00416 -0.00042 AFIX 13 H34 2 0.633051 0.431566 0.247924 11.00000 -1.20000 AFIX 0 C35 1 0.518926 0.352201 0.206359 11.00000 0.01444 0.01854 = 0.01426 0.00328 0.00144 -0.00135 AFIX 137 H35a 2 0.519052 0.295243 0.195664 11.00000 -1.50000 H35b 2 0.513072 0.384542 0.169597 11.00000 -1.50000 H35c 2 0.450533 0.363625 0.232541 11.00000 -1.50000 AFIX 0 C36 1 0.741430 0.356197 0.199310 11.00000 0.01598 0.02462 = 0.01678 0.00438 0.00977 0.00467 AFIX 137 H36a 2 0.814859 0.370310 0.220860 11.00000 -1.50000 H36b 2 0.735297 0.388391 0.162486 11.00000 -1.50000 H36c 2 0.743223 0.299229 0.188686 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for rudi005_a.res in P2(1)2(1)2(1) C 0.770 H 0.320 I 1.330 IN 1.440 N 0.700 I1 - In1 I2 - In1 I3 - In1 I4 - In1 In1 - I3 I1 I4 I2 N1 - C2 C6 C1 C1 - N1 C2 - N1 C3 C12 C3 - C4 C2 C4 - C3 C5 C5 - C6 C4 C6 - C5 N1 C27 C7 - C8 C12 C13 C8 - C9 C7 C9 - C10 C8 C16 C10 - C9 C11 C11 - C10 C12 C19 C12 - C11 C7 C2 C13 - C7 C14 C15 C14 - C13 C15 - C13 C16 - C9 C18 C17 C17 - C16 C18 - C16 C19 - C11 C21 C20 C20 - C19 C21 - C19 C22 - C23 C27 C28 C23 - C22 C24 C24 - C23 C25 C31 C25 - C26 C24 C26 - C25 C27 C34 C27 - C22 C26 C6 C28 - C22 C29 C30 C29 - C28 C30 - C28 C31 - C24 C33 C32 C32 - C31 C33 - C31 C34 - C36 C26 C35 C35 - C34 C36 - C34 h k l Fo^2 Sigma Why rejected (first 50 of each listed) 1 0 0 2.30 0.50 systematically absent but >3sig(I) 7 0 0 15.20 3.60 systematically absent but >3sig(I) 7 0 0 9.50 2.60 systematically absent but >3sig(I) 0 1 0 2.00 0.40 systematically absent but >3sig(I) 0 1 0 1.30 0.30 systematically absent but >3sig(I) 0 3 0 1.90 0.50 systematically absent but >3sig(I) 0 0 3 2.20 0.40 systematically absent but >3sig(I) 0 0 9 8.80 2.70 systematically absent but >3sig(I) 62 Systematically absent reflections rejected 32863 Reflections read, of which 75 rejected -13 =< h =< 13, -20 =< k =< 20, -25 =< l =< 27, Max. 2-theta = 149.11 8 Systematic absence violations (I>3sig(I)) before merging 1 Inconsistent equivalents 8254 Unique reflections, of which 0 suppressed R(int) = 0.0521 R(sigma) = 0.0431 Friedel opposites not merged Maximum memory for data reduction = 5924 / 81464 Reflection statistics for all twin components combined (TWST 0 set) Number of data for d > 0.800A (CIF: max) and d > 0.833A (CIF: full) (ignoring systematic absences): Unique reflections found (point group) 8254 7442 Unique reflections possible (point group) 8474 7496 Unique reflections found (Laue group) 4667 4169 Unique reflections possible (Laue group) 4714 4189 Unique Friedel pairs found 3587 3273 Unique Friedel pairs possible 3760 3307 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 = 104 / 7099 / 595525 wR2 = 0.1003 before cycle 1 for 8254 data and 392 / 392 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint -0.0143 0.0040 SIMU U22 C19 C20 Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 0 0 0 0 0 291 234 0 0 rms sigma 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0379 0.0028 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0021 0.0032 0.0000 0.0000 GooF = S = 1.041; Restrained GooF = 1.020 for 525 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0656 * P )^2 + 10.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19689 0.00034 -0.180 OSF Mean shift/esd = 0.012 Maximum = -0.180 for OSF Max. shift = 0.002 A for H30A Max. dU = 0.000 for C15 Least-squares cycle 2 Maximum vector length = 623 Memory required = 104 / 7099 / 595525 wR2 = 0.1002 before cycle 2 for 8254 data and 392 / 392 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint -0.0143 0.0040 SIMU U22 C19 C20 Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 0 0 0 0 0 291 234 0 0 rms sigma 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0379 0.0028 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0021 0.0032 0.0000 0.0000 GooF = S = 1.040; Restrained GooF = 1.020 for 525 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0656 * P )^2 + 10.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19687 0.00034 -0.045 OSF Mean shift/esd = 0.004 Maximum = -0.045 for OSF Max. shift = 0.002 A for H30A Max. dU = 0.000 for C15 Least-squares cycle 3 Maximum vector length = 623 Memory required = 104 / 7099 / 595525 wR2 = 0.1003 before cycle 3 for 8254 data and 392 / 392 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint -0.0143 0.0040 SIMU U22 C19 C20 Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 0 0 0 0 0 291 234 0 0 rms sigma 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0379 0.0028 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0021 0.0032 0.0000 0.0000 GooF = S = 1.041; Restrained GooF = 1.020 for 525 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0656 * P )^2 + 10.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19687 0.00034 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.007 for tors H30A Max. shift = 0.001 A for H30A Max. dU = 0.000 for C32 Least-squares cycle 4 Maximum vector length = 623 Memory required = 104 / 7099 / 595525 wR2 = 0.1002 before cycle 4 for 8254 data and 392 / 392 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint -0.0143 0.0040 SIMU U22 C19 C20 Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 0 0 0 0 0 291 234 0 0 rms sigma 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0379 0.0028 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0021 0.0032 0.0000 0.0000 GooF = S = 1.040; Restrained GooF = 1.020 for 525 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0656 * P )^2 + 10.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19687 0.00034 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.002 for tors H30A Max. shift = 0.000 A for H30A Max. dU = 0.000 for C14 Least-squares cycle 5 Maximum vector length = 623 Memory required = 104 / 7099 / 595525 wR2 = 0.1003 before cycle 5 for 8254 data and 392 / 392 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint -0.0143 0.0040 SIMU U22 C19 C20 Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 0 0 0 0 0 291 234 0 0 rms sigma 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0379 0.0028 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0021 0.0032 0.0000 0.0000 GooF = S = 1.040; Restrained GooF = 1.020 for 525 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0656 * P )^2 + 10.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19687 0.00034 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for tors H30A Max. shift = 0.000 A for H30C Max. dU = 0.000 for C36 Least-squares cycle 6 Maximum vector length = 623 Memory required = 104 / 7099 / 595525 wR2 = 0.1002 before cycle 6 for 8254 data and 392 / 392 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint -0.0143 0.0040 SIMU U22 C19 C20 Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 0 0 0 0 0 291 234 0 0 rms sigma 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0379 0.0028 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0021 0.0032 0.0000 0.0000 GooF = S = 1.040; Restrained GooF = 1.020 for 525 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0656 * P )^2 + 10.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19687 0.00034 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y In1 Max. shift = 0.000 A for H30A Max. dU = 0.000 for C32 Least-squares cycle 7 Maximum vector length = 623 Memory required = 104 / 7099 / 595525 wR2 = 0.1002 before cycle 7 for 8254 data and 392 / 392 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint -0.0143 0.0040 SIMU U22 C19 C20 Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 0 0 0 0 0 291 234 0 0 rms sigma 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0379 0.0028 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0021 0.0032 0.0000 0.0000 GooF = S = 1.040; Restrained GooF = 1.020 for 525 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0656 * P )^2 + 10.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19687 0.00034 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y In1 Max. shift = 0.000 A for H30C Max. dU = 0.000 for C32 Least-squares cycle 8 Maximum vector length = 623 Memory required = 104 / 7099 / 595525 wR2 = 0.1003 before cycle 8 for 8254 data and 392 / 392 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint -0.0143 0.0040 SIMU U22 C19 C20 Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 0 0 0 0 0 291 234 0 0 rms sigma 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0379 0.0028 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0021 0.0032 0.0000 0.0000 GooF = S = 1.041; Restrained GooF = 1.020 for 525 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0656 * P )^2 + 10.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19687 0.00034 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y In1 Max. shift = 0.000 A for H29C Max. dU = 0.000 for C32 Least-squares cycle 9 Maximum vector length = 623 Memory required = 104 / 7099 / 595525 wR2 = 0.1002 before cycle 9 for 8254 data and 392 / 392 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint -0.0143 0.0040 SIMU U22 C19 C20 Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 0 0 0 0 0 291 234 0 0 rms sigma 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0379 0.0028 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0021 0.0032 0.0000 0.0000 GooF = S = 1.040; Restrained GooF = 1.020 for 525 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0656 * P )^2 + 10.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19687 0.00034 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y In1 Max. shift = 0.000 A for H32A Max. dU = 0.000 for C32 Least-squares cycle 10 Maximum vector length = 623 Memory required = 104 / 7099 / 595525 wR2 = 0.1002 before cycle 10 for 8254 data and 392 / 392 parameters Disagreeable restraints before cycle 10 Observed Target Error Sigma Restraint -0.0143 0.0040 SIMU U22 C19 C20 Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 0 0 0 0 0 291 234 0 0 rms sigma 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0379 0.0028 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0021 0.0032 0.0000 0.0000 GooF = S = 1.040; Restrained GooF = 1.020 for 525 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0656 * P )^2 + 10.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19687 0.00034 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y In1 Max. shift = 0.000 A for H20A Max. dU = 0.000 for C32 Least-squares cycle 11 Maximum vector length = 623 Memory required = 104 / 7099 / 595525 wR2 = 0.1003 before cycle 11 for 8254 data and 392 / 392 parameters Disagreeable restraints before cycle 11 Observed Target Error Sigma Restraint -0.0143 0.0040 SIMU U22 C19 C20 Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 0 0 0 0 0 291 234 0 0 rms sigma 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0379 0.0028 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0021 0.0032 0.0000 0.0000 GooF = S = 1.040; Restrained GooF = 1.020 for 525 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0656 * P )^2 + 10.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19687 0.00034 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y In1 Max. shift = 0.000 A for H32B Max. dU = 0.000 for C32 Least-squares cycle 12 Maximum vector length = 623 Memory required = 104 / 7099 / 595525 wR2 = 0.1002 before cycle 12 for 8254 data and 392 / 392 parameters Disagreeable restraints before cycle 12 Observed Target Error Sigma Restraint -0.0143 0.0040 SIMU U22 C19 C20 Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 0 0 0 0 0 291 234 0 0 rms sigma 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0379 0.0028 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0021 0.0032 0.0000 0.0000 GooF = S = 1.040; Restrained GooF = 1.020 for 525 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0656 * P )^2 + 10.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19687 0.00034 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y In1 Max. shift = 0.000 A for H32C Max. dU = 0.000 for C32 Least-squares cycle 13 Maximum vector length = 623 Memory required = 104 / 7099 / 595525 wR2 = 0.1002 before cycle 13 for 8254 data and 392 / 392 parameters Disagreeable restraints before cycle 13 Observed Target Error Sigma Restraint -0.0143 0.0040 SIMU U22 C19 C20 Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 0 0 0 0 0 291 234 0 0 rms sigma 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0379 0.0028 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0021 0.0032 0.0000 0.0000 GooF = S = 1.040; Restrained GooF = 1.020 for 525 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0656 * P )^2 + 10.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19687 0.00034 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y In1 Max. shift = 0.000 A for H33A Max. dU = 0.000 for C32 Least-squares cycle 14 Maximum vector length = 623 Memory required = 104 / 7099 / 595525 wR2 = 0.1002 before cycle 14 for 8254 data and 392 / 392 parameters Disagreeable restraints before cycle 14 Observed Target Error Sigma Restraint -0.0143 0.0040 SIMU U22 C19 C20 Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 0 0 0 0 0 291 234 0 0 rms sigma 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0379 0.0028 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0021 0.0032 0.0000 0.0000 GooF = S = 1.040; Restrained GooF = 1.020 for 525 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0656 * P )^2 + 10.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19687 0.00034 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y In1 Max. shift = 0.000 A for H30B Max. dU = 0.000 for C30 Least-squares cycle 15 Maximum vector length = 623 Memory required = 104 / 7099 / 595525 wR2 = 0.1002 before cycle 15 for 8254 data and 392 / 392 parameters Disagreeable restraints before cycle 15 Observed Target Error Sigma Restraint -0.0143 0.0040 SIMU U22 C19 C20 Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 0 0 0 0 0 291 234 0 0 rms sigma 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0379 0.0028 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0021 0.0032 0.0000 0.0000 GooF = S = 1.040; Restrained GooF = 1.020 for 525 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0656 * P )^2 + 10.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19687 0.00034 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y In1 Max. shift = 0.000 A for H32C Max. dU = 0.000 for C32 Least-squares cycle 16 Maximum vector length = 623 Memory required = 104 / 7099 / 595525 wR2 = 0.1002 before cycle 16 for 8254 data and 392 / 392 parameters Disagreeable restraints before cycle 16 Observed Target Error Sigma Restraint -0.0143 0.0040 SIMU U22 C19 C20 Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 0 0 0 0 0 291 234 0 0 rms sigma 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0379 0.0028 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0021 0.0032 0.0000 0.0000 GooF = S = 1.040; Restrained GooF = 1.020 for 525 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0656 * P )^2 + 10.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19687 0.00034 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y In1 Max. shift = 0.000 A for H20C Max. dU = 0.000 for C32 Least-squares cycle 17 Maximum vector length = 623 Memory required = 104 / 7099 / 595525 wR2 = 0.1002 before cycle 17 for 8254 data and 392 / 392 parameters Disagreeable restraints before cycle 17 Observed Target Error Sigma Restraint -0.0143 0.0040 SIMU U22 C19 C20 Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 0 0 0 0 0 291 234 0 0 rms sigma 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0379 0.0028 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0021 0.0032 0.0000 0.0000 GooF = S = 1.040; Restrained GooF = 1.020 for 525 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0656 * P )^2 + 10.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19687 0.00034 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y In1 Max. shift = 0.000 A for H30C Max. dU = 0.000 for C32 Least-squares cycle 18 Maximum vector length = 623 Memory required = 104 / 7099 / 595525 wR2 = 0.1003 before cycle 18 for 8254 data and 392 / 392 parameters Disagreeable restraints before cycle 18 Observed Target Error Sigma Restraint -0.0143 0.0040 SIMU U22 C19 C20 Summary of restraints applied in cycle 18 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 0 0 0 0 0 291 234 0 0 rms sigma 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0379 0.0028 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0021 0.0032 0.0000 0.0000 GooF = S = 1.041; Restrained GooF = 1.020 for 525 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0656 * P )^2 + 10.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19687 0.00034 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U22 C20 Max. shift = 0.000 A for H20A Max. dU = 0.000 for C32 Least-squares cycle 19 Maximum vector length = 623 Memory required = 104 / 7099 / 595525 wR2 = 0.1002 before cycle 19 for 8254 data and 392 / 392 parameters Disagreeable restraints before cycle 19 Observed Target Error Sigma Restraint -0.0143 0.0040 SIMU U22 C19 C20 Summary of restraints applied in cycle 19 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 0 0 0 0 0 291 234 0 0 rms sigma 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0379 0.0028 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0021 0.0032 0.0000 0.0000 GooF = S = 1.040; Restrained GooF = 1.020 for 525 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0656 * P )^2 + 10.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19687 0.00034 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y In1 Max. shift = 0.000 A for H18C Max. dU = 0.000 for C32 Least-squares cycle 20 Maximum vector length = 623 Memory required = 104 / 7099 / 595525 wR2 = 0.1002 before cycle 20 for 8254 data and 392 / 392 parameters Disagreeable restraints before cycle 20 Observed Target Error Sigma Restraint -0.0143 0.0040 SIMU U22 C19 C20 Summary of restraints applied in cycle 20 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 0 0 0 0 0 291 234 0 0 rms sigma 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0379 0.0028 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0021 0.0032 0.0000 0.0000 GooF = S = 1.040; Restrained GooF = 1.020 for 525 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0656 * P )^2 + 10.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19687 0.00034 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y In1 Max. shift = 0.000 A for H29B Max. dU = 0.000 for C32 Largest correlation matrix elements 0.522 U22 C31 / U22 C24 Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.7744 0.4730 0.3287 137 0.980 0.000 C1 N1 H1A H1B 0.7444 0.4705 0.3993 137 0.980 0.000 C1 N1 H1A H1C 0.7725 0.5542 0.3671 137 0.980 0.000 C1 N1 H1A H3 0.4088 0.6474 0.3219 43 0.950 0.000 C3 C4 C2 H4 0.2826 0.5380 0.3276 43 0.950 0.000 C4 C3 C5 H5 0.3621 0.4094 0.3402 43 0.950 0.000 C5 C6 C4 H8 0.8145 0.7605 0.2447 43 0.950 0.000 C8 C9 C7 H10 0.7358 0.8068 0.4183 43 0.950 0.000 C10 C9 C11 H13 0.6314 0.5850 0.2320 13 1.000 0.000 C13 C7 C14 C15 H14A 0.8656 0.6326 0.1963 137 0.980 0.000 C14 C13 H14A H14B 0.7934 0.5592 0.1676 137 0.980 0.000 C14 C13 H14A H14C 0.8357 0.5556 0.2365 137 0.980 0.000 C14 C13 H14A H15A 0.5600 0.7018 0.1848 137 0.980 0.000 C15 C13 H15A H15B 0.6295 0.6485 0.1362 137 0.980 0.000 C15 C13 H15A H15C 0.6924 0.7258 0.1647 137 0.980 0.000 C15 C13 H15A H16 0.8117 0.9138 0.3533 13 1.000 0.000 C16 C9 C18 C17 H17A 0.9538 0.8406 0.4097 137 0.980 0.000 C17 C16 H17A H17B 1.0189 0.9094 0.3716 137 0.980 0.000 C17 C16 H17A H17C 1.0241 0.8183 0.3492 137 0.980 0.000 C17 C16 H17A H18A 0.9257 0.9577 0.2734 137 0.980 0.000 C18 C16 H18A H18B 0.8205 0.9054 0.2445 137 0.980 0.000 C18 C16 H18A H18C 0.9516 0.8682 0.2510 137 0.980 0.000 C18 C16 H18A H19 0.5641 0.6288 0.4440 13 1.000 0.000 C19 C11 C21 C20 H20A 0.7540 0.6591 0.4909 137 0.980 0.000 C20 C19 H20A H20B 0.6436 0.6672 0.5363 137 0.980 0.000 C20 C19 H20A H20C 0.7029 0.7457 0.5078 137 0.980 0.000 C20 C19 H20A H21A 0.5140 0.7963 0.4536 137 0.980 0.000 C21 C19 H21A H21B 0.4542 0.7308 0.4968 137 0.980 0.000 C21 C19 H21A H21C 0.4270 0.7297 0.4260 137 0.980 0.000 C21 C19 H21A H23 0.6376 0.2192 0.4476 43 0.950 0.000 C23 C22 C24 H25 0.7282 0.2300 0.2707 43 0.950 0.000 C25 C26 C24 H28 0.5042 0.4148 0.4536 13 1.000 0.000 C28 C22 C29 C30 H29A 0.3622 0.3122 0.4489 137 0.980 0.000 C29 C28 H29A H29B 0.3856 0.3340 0.5182 137 0.980 0.000 C29 C28 H29A H29C 0.4441 0.2552 0.4896 137 0.980 0.000 C29 C28 H29A H30A 0.6412 0.3105 0.5296 137 0.980 0.000 C30 C28 H30A H30B 0.5810 0.3930 0.5503 137 0.980 0.000 C30 C28 H30A H30C 0.6906 0.3937 0.5039 137 0.980 0.000 C30 C28 H30A H31 0.7426 0.1129 0.4082 13 1.000 0.000 C31 C24 C33 C32 H32A 0.6620 0.0857 0.2870 137 0.980 0.000 C32 C31 H32A H32B 0.5852 0.0686 0.3464 137 0.980 0.000 C32 C31 H32A H32C 0.7008 0.0156 0.3321 137 0.980 0.000 C32 C31 H32A H33A 0.9070 0.0732 0.3550 137 0.980 0.000 C33 C31 H33A H33B 0.9184 0.1684 0.3615 137 0.980 0.000 C33 C31 H33A H33C 0.8745 0.1299 0.2992 137 0.980 0.000 C33 C31 H33A H34 0.6330 0.4316 0.2479 13 1.000 0.000 C34 C36 C26 C35 H35A 0.5191 0.2953 0.1956 137 0.980 0.000 C35 C34 H35A H35B 0.5130 0.3846 0.1696 137 0.980 0.000 C35 C34 H35A H35C 0.4505 0.3635 0.2326 137 0.980 0.000 C35 C34 H35A H36A 0.8149 0.3703 0.2208 137 0.980 0.000 C36 C34 H36A H36B 0.7353 0.3884 0.1625 137 0.980 0.000 C36 C34 H36A H36C 0.7432 0.2992 0.1887 137 0.980 0.000 C36 C34 H36A rudi005_a.res in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq I1 0.30173 0.53844 0.49956 1.00000 0.01137 0.01792 0.01644 -0.00335 -0.00016 0.00031 0.01524 0.00084 0.00004 0.00003 0.00002 0.00000 0.00023 0.00024 0.00025 0.00020 0.00020 0.00018 0.00013 I2 0.03648 0.61985 0.36744 1.00000 0.01318 0.02347 0.03109 0.01363 -0.00171 0.00354 0.02258 0.00105 0.00005 0.00003 0.00003 0.00000 0.00025 0.00027 0.00032 0.00023 0.00022 0.00021 0.00015 I3 -0.08248 0.50830 0.54106 1.00000 0.01822 0.02975 0.02891 0.00104 0.01010 -0.00155 0.02563 0.00109 0.00005 0.00004 0.00003 0.00000 0.00029 0.00030 0.00031 0.00024 0.00023 0.00024 0.00015 I4 0.07951 0.36079 0.40066 1.00000 0.03673 0.01798 0.01716 -0.00165 -0.00027 -0.00583 0.02395 0.00097 0.00006 0.00003 0.00002 0.00000 0.00034 0.00026 0.00027 0.00020 0.00024 0.00024 0.00015 In1 0.08325 0.50752 0.45283 1.00000 0.01030 0.01399 0.01541 0.00225 0.00006 -0.00002 0.01323 0.00092 0.00005 0.00003 0.00002 0.00000 0.00026 0.00024 0.00026 0.00020 0.00020 0.00020 0.00013 N1 0.60639 0.51164 0.34819 1.00000 0.00481 0.01129 0.01238 0.00105 0.00194 -0.00101 0.00949 0.01093 0.00056 0.00038 0.00028 0.00000 0.00180 0.00174 0.00184 0.00159 0.00159 0.00159 0.00087 C1 0.73542 0.50144 0.36200 1.00000 0.00630 0.01290 0.02069 0.00232 -0.00277 -0.00050 0.01329 0.01365 0.00066 0.00047 0.00037 0.00000 0.00292 0.00290 0.00334 0.00281 0.00258 0.00246 0.00137 H1A 0.77439 0.47299 0.32873 1.00000 0.01994 0.00000 0.00000 H1B 0.74436 0.47045 0.39926 1.00000 0.01994 0.00000 0.00000 H1C 0.77254 0.55417 0.36711 1.00000 0.01994 0.00000 0.00000 C2 0.56348 0.58695 0.33762 1.00000 0.00648 0.01203 0.01169 0.00038 0.00174 0.00039 0.01007 0.01326 0.00067 0.00045 0.00035 0.00000 0.00179 0.00171 0.00178 0.00159 0.00157 0.00156 0.00087 C3 0.44104 0.59568 0.32928 1.00000 0.00581 0.01337 0.01268 0.00033 0.00106 0.00131 0.01062 0.01316 0.00066 0.00045 0.00034 0.00000 0.00204 0.00200 0.00209 0.00183 0.00177 0.00176 0.00100 H3 0.40881 0.64740 0.32190 1.00000 0.01274 0.00000 0.00000 C4 0.36635 0.53087 0.33156 1.00000 0.00635 0.01485 0.01239 -0.00008 0.00129 0.00125 0.01120 0.01343 0.00068 0.00046 0.00034 0.00000 0.00202 0.00207 0.00213 0.00188 0.00183 0.00185 0.00100 H4 0.28257 0.53798 0.32762 1.00000 0.01344 0.00000 0.00000 C5 0.41347 0.45465 0.33966 1.00000 0.00641 0.01377 0.01143 -0.00076 0.00059 -0.00053 0.01054 0.01318 0.00070 0.00045 0.00033 0.00000 0.00197 0.00199 0.00203 0.00183 0.00183 0.00185 0.00096 H5 0.36208 0.40938 0.34021 1.00000 0.01264 0.00000 0.00000 C6 0.53435 0.44474 0.34687 1.00000 0.00538 0.01190 0.01050 -0.00031 0.00156 -0.00038 0.00926 0.01314 0.00069 0.00044 0.00034 0.00000 0.00172 0.00171 0.00177 0.00158 0.00158 0.00161 0.00085 C7 0.70364 0.67721 0.28107 1.00000 0.00849 0.01125 0.01239 0.00055 0.00214 0.00052 0.01071 0.01362 0.00071 0.00044 0.00034 0.00000 0.00180 0.00177 0.00186 0.00166 0.00167 0.00166 0.00089 C8 0.77389 0.74645 0.28075 1.00000 0.00701 0.01230 0.01102 0.00104 0.00156 0.00033 0.01011 0.01320 0.00066 0.00044 0.00036 0.00000 0.00196 0.00196 0.00203 0.00182 0.00180 0.00180 0.00097 H8 0.81450 0.76047 0.24466 1.00000 0.01213 0.00000 0.00000 C9 0.78700 0.79579 0.33098 1.00000 0.00618 0.01195 0.01043 0.00101 0.00128 0.00031 0.00952 0.01324 0.00068 0.00045 0.00034 0.00000 0.00181 0.00181 0.00189 0.00166 0.00165 0.00167 0.00089 C10 0.72789 0.77364 0.38365 1.00000 0.00678 0.01178 0.01115 0.00071 0.00109 0.00124 0.00990 0.01321 0.00065 0.00044 0.00035 0.00000 0.00198 0.00197 0.00205 0.00179 0.00178 0.00177 0.00099 H10 0.73579 0.80677 0.41825 1.00000 0.01189 0.00000 0.00000 C11 0.65755 0.70486 0.38777 1.00000 0.00758 0.01168 0.01142 0.00113 0.00127 0.00013 0.01023 0.01344 0.00068 0.00046 0.00035 0.00000 0.00179 0.00178 0.00185 0.00165 0.00163 0.00163 0.00090 C12 0.64520 0.65718 0.33565 1.00000 0.00686 0.01069 0.01171 0.00091 0.00168 0.00024 0.00975 0.01340 0.00068 0.00045 0.00035 0.00000 0.00173 0.00170 0.00177 0.00159 0.00159 0.00158 0.00087 C13 0.68966 0.62899 0.22376 1.00000 0.01378 0.01376 0.01402 -0.00024 0.00376 -0.00029 0.01385 0.01412 0.00074 0.00047 0.00036 0.00000 0.00226 0.00217 0.00225 0.00203 0.00203 0.00204 0.00108 H13 0.63137 0.58497 0.23201 1.00000 0.01663 0.00000 0.00000 C14 0.80643 0.59069 0.20434 1.00000 0.02122 0.02380 0.02115 -0.00300 0.00479 0.00507 0.02206 0.01670 0.00087 0.00056 0.00041 0.00000 0.00356 0.00346 0.00351 0.00298 0.00310 0.00302 0.00160 H14A 0.86560 0.63261 0.19632 1.00000 0.03309 0.00000 0.00000 H14B 0.79340 0.55918 0.16764 1.00000 0.03309 0.00000 0.00000 H14C 0.83567 0.55557 0.23652 1.00000 0.03309 0.00000 0.00000 C15 0.63826 0.68097 0.17275 1.00000 0.02184 0.02189 0.01525 -0.00014 0.00202 -0.00101 0.01966 0.01579 0.00084 0.00053 0.00039 0.00000 0.00356 0.00340 0.00334 0.00291 0.00295 0.00299 0.00156 H15A 0.56003 0.70176 0.18485 1.00000 0.02949 0.00000 0.00000 H15B 0.62955 0.64849 0.13621 1.00000 0.02949 0.00000 0.00000 H15C 0.69245 0.72580 0.16468 1.00000 0.02949 0.00000 0.00000 C16 0.85999 0.87182 0.33238 1.00000 0.00868 0.01323 0.01126 0.00182 0.00198 -0.00177 0.01105 0.01330 0.00068 0.00046 0.00034 0.00000 0.00217 0.00220 0.00226 0.00199 0.00197 0.00199 0.00106 H16 0.81166 0.91383 0.35330 1.00000 0.01327 0.00000 0.00000 C17 0.97455 0.85886 0.36903 1.00000 0.01275 0.02012 0.01177 0.00310 0.00191 -0.00426 0.01488 0.01425 0.00072 0.00050 0.00036 0.00000 0.00306 0.00322 0.00312 0.00283 0.00273 0.00277 0.00140 H17A 0.95383 0.84063 0.40971 1.00000 0.02232 0.00000 0.00000 H17B 1.01886 0.90937 0.37162 1.00000 0.02232 0.00000 0.00000 H17C 1.02414 0.81833 0.34917 1.00000 0.02232 0.00000 0.00000 C18 0.89237 0.90367 0.26965 1.00000 0.01937 0.01872 0.01799 0.00575 0.00055 -0.00945 0.01869 0.01510 0.00082 0.00051 0.00039 0.00000 0.00351 0.00329 0.00332 0.00281 0.00284 0.00284 0.00154 H18A 0.92573 0.95771 0.27336 1.00000 0.02804 0.00000 0.00000 H18B 0.82053 0.90543 0.24446 1.00000 0.02804 0.00000 0.00000 H18C 0.95155 0.86822 0.25101 1.00000 0.02804 0.00000 0.00000 C19 0.59455 0.68500 0.44673 1.00000 0.00947 0.01659 0.01220 0.00173 0.00294 0.00172 0.01275 0.01407 0.00072 0.00047 0.00034 0.00000 0.00219 0.00219 0.00223 0.00197 0.00200 0.00201 0.00107 H19 0.56410 0.62881 0.44400 1.00000 0.01531 0.00000 0.00000 C20 0.68168 0.68967 0.50033 1.00000 0.00858 0.03092 0.01230 0.00341 0.00190 -0.00036 0.01726 0.01480 0.00070 0.00054 0.00037 0.00000 0.00302 0.00355 0.00315 0.00298 0.00274 0.00282 0.00146 H20A 0.75400 0.65909 0.49093 1.00000 0.02590 0.00000 0.00000 H20B 0.64359 0.66715 0.53632 1.00000 0.02590 0.00000 0.00000 H20C 0.70289 0.74574 0.50785 1.00000 0.02590 0.00000 0.00000 C21 0.48790 0.74044 0.45668 1.00000 0.01489 0.02469 0.01542 0.00278 0.00696 0.00700 0.01833 0.01623 0.00075 0.00053 0.00040 0.00000 0.00326 0.00340 0.00335 0.00301 0.00277 0.00286 0.00152 H21A 0.51402 0.79632 0.45363 1.00000 0.02750 0.00000 0.00000 H21B 0.45422 0.73085 0.49682 1.00000 0.02750 0.00000 0.00000 H21C 0.42703 0.72973 0.42598 1.00000 0.02750 0.00000 0.00000 C22 0.58760 0.32379 0.40779 1.00000 0.01183 0.01385 0.01272 -0.00036 0.00079 0.00185 0.01280 0.01386 0.00074 0.00046 0.00035 0.00000 0.00185 0.00184 0.00188 0.00167 0.00171 0.00172 0.00091 C23 0.63915 0.24771 0.41054 1.00000 0.01146 0.01403 0.01435 0.00041 -0.00088 0.00173 0.01328 0.01378 0.00070 0.00047 0.00036 0.00000 0.00204 0.00207 0.00210 0.00185 0.00187 0.00187 0.00101 H23 0.63763 0.21920 0.44760 1.00000 0.01593 0.00000 0.00000 C24 0.69294 0.21232 0.36026 1.00000 0.01040 0.01402 0.01638 0.00015 -0.00121 0.00191 0.01360 0.01404 0.00074 0.00046 0.00037 0.00000 0.00190 0.00192 0.00196 0.00172 0.00174 0.00171 0.00094 C25 0.69262 0.25404 0.30519 1.00000 0.00885 0.01363 0.01442 -0.00072 0.00156 0.00047 0.01230 0.01368 0.00071 0.00046 0.00036 0.00000 0.00204 0.00203 0.00207 0.00184 0.00183 0.00187 0.00099 H25 0.72816 0.23004 0.27075 1.00000 0.01476 0.00000 0.00000 C26 0.64147 0.32963 0.29998 1.00000 0.00836 0.01339 0.01246 0.00082 0.00196 0.00004 0.01141 0.01365 0.00070 0.00046 0.00035 0.00000 0.00183 0.00184 0.00188 0.00167 0.00165 0.00167 0.00091 C27 0.58982 0.36453 0.35200 1.00000 0.00865 0.01275 0.01177 -0.00061 0.00158 0.00027 0.01106 0.01322 0.00071 0.00044 0.00034 0.00000 0.00173 0.00174 0.00177 0.00159 0.00160 0.00165 0.00087 C28 0.53093 0.35919 0.46356 1.00000 0.01720 0.01660 0.01349 -0.00009 0.00318 0.00420 0.01576 0.01488 0.00078 0.00049 0.00036 0.00000 0.00228 0.00222 0.00228 0.00203 0.00210 0.00213 0.00110 H28 0.50420 0.41477 0.45355 1.00000 0.01892 0.00000 0.00000 C29 0.42083 0.31081 0.48172 1.00000 0.02196 0.02393 0.01599 0.00136 0.00606 0.00400 0.02063 0.01641 0.00085 0.00052 0.00039 0.00000 0.00342 0.00341 0.00334 0.00285 0.00295 0.00312 0.00154 H29A 0.36218 0.31218 0.44894 1.00000 0.03094 0.00000 0.00000 H29B 0.38563 0.33402 0.51821 1.00000 0.03094 0.00000 0.00000 H29C 0.44409 0.25521 0.48965 1.00000 0.03094 0.00000 0.00000 C30 0.61890 0.36460 0.51665 1.00000 0.02617 0.02354 0.01653 -0.00448 0.00258 -0.00352 0.02208 0.01529 0.00084 0.00056 0.00039 0.00000 0.00357 0.00347 0.00335 0.00294 0.00291 0.00313 0.00161 H30A 0.64115 0.31050 0.52961 1.00000 0.03312 0.00000 0.00000 H30B 0.58104 0.39302 0.55025 1.00000 0.03312 0.00000 0.00000 H30C 0.69056 0.39372 0.50392 1.00000 0.03312 0.00000 0.00000 C31 0.74405 0.12904 0.36480 1.00000 0.01301 0.01645 0.01908 0.00056 -0.00149 0.00552 0.01618 0.01456 0.00073 0.00049 0.00039 0.00000 0.00229 0.00228 0.00239 0.00210 0.00209 0.00205 0.00112 H31 0.74257 0.11287 0.40822 1.00000 0.01941 0.00000 0.00000 C32 0.66589 0.06926 0.32933 1.00000 0.02170 0.01734 0.03067 -0.00162 -0.00736 0.00823 0.02323 0.01600 0.00087 0.00052 0.00044 0.00000 0.00357 0.00326 0.00386 0.00309 0.00316 0.00292 0.00166 H32A 0.66197 0.08570 0.28695 1.00000 0.03485 0.00000 0.00000 H32B 0.58524 0.06857 0.34644 1.00000 0.03485 0.00000 0.00000 H32C 0.70084 0.01557 0.33207 1.00000 0.03485 0.00000 0.00000 C33 0.87233 0.12474 0.34321 1.00000 0.01281 0.02272 0.02545 0.00121 0.00125 0.00910 0.02033 0.01652 0.00076 0.00055 0.00042 0.00000 0.00320 0.00348 0.00363 0.00316 0.00291 0.00289 0.00158 H33A 0.90705 0.07318 0.35500 1.00000 0.03049 0.00000 0.00000 H33B 0.91840 0.16835 0.36149 1.00000 0.03049 0.00000 0.00000 H33C 0.87447 0.12993 0.29921 1.00000 0.03049 0.00000 0.00000 C34 0.63428 0.37273 0.23947 1.00000 0.00931 0.01453 0.01349 0.00189 0.00415 -0.00041 0.01244 0.01401 0.00069 0.00048 0.00035 0.00000 0.00221 0.00223 0.00224 0.00199 0.00197 0.00200 0.00108 H34 0.63304 0.43156 0.24792 1.00000 0.01493 0.00000 0.00000 C35 0.51892 0.35219 0.20636 1.00000 0.01445 0.01853 0.01425 0.00327 0.00145 -0.00134 0.01574 0.01458 0.00075 0.00050 0.00038 0.00000 0.00314 0.00323 0.00322 0.00280 0.00270 0.00281 0.00145 H35A 0.51912 0.29525 0.19559 1.00000 0.02362 0.00000 0.00000 H35B 0.51298 0.38461 0.16964 1.00000 0.02362 0.00000 0.00000 H35C 0.45053 0.36350 0.23257 1.00000 0.02362 0.00000 0.00000 C36 0.74142 0.35619 0.19931 1.00000 0.01599 0.02461 0.01680 0.00446 0.00979 0.00463 0.01913 0.01654 0.00077 0.00054 0.00039 0.00000 0.00326 0.00346 0.00335 0.00294 0.00282 0.00298 0.00155 H36A 0.81485 0.37032 0.22085 1.00000 0.02870 0.00000 0.00000 H36B 0.73527 0.38837 0.16248 1.00000 0.02870 0.00000 0.00000 H36C 0.74323 0.29922 0.18869 1.00000 0.02870 0.00000 0.00000 Final Structure Factor Calculation for rudi005_a.res in P2(1)2(1)2(1) Total number of l.s. parameters = 392 Maximum vector length = 623 Memory required = 104 / 6707 / 29281 wR2 = 0.1002 before cycle 21 for 8254 data and 0 / 392 parameters Disagreeable restraints before cycle 21 Observed Target Error Sigma Restraint -0.0143 0.0040 SIMU U22 C19 C20 Summary of restraints applied in cycle 21 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 0 0 0 0 0 291 234 0 0 rms sigma 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0379 0.0028 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0021 0.0032 0.0000 0.0000 GooF = S = 1.040; Restrained GooF = 1.020 for 525 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0656 * P )^2 + 10.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 wR2 = 0.1002, GooF = S = 1.040, Restrained GooF = 1.020 for all data R1 = 0.0374 for 8086 Fo > 4sig(Fo) and 0.0383 for all 8254 data Flack x = 0.013(10) by classical fit to all intensities -0.004(5) from 3390 selected quotients (Parsons' method) Occupancy sum of asymmetric unit = 42.00 for non-hydrogen and 52.00 for H and D atoms Principal mean square atomic displacements U 0.0206 0.0138 0.0114 I1 0.0415 0.0170 0.0093 I2 0.0350 0.0299 0.0119 I3 0.0384 0.0184 0.0150 I4 0.0171 0.0123 0.0103 In1 0.0132 0.0111 0.0041 N1 0.0218 0.0123 0.0058 C1 0.0126 0.0116 0.0059 C2 0.0138 0.0126 0.0055 C3 0.0150 0.0126 0.0059 C4 0.0141 0.0112 0.0063 C5 0.0121 0.0108 0.0049 C6 0.0136 0.0111 0.0075 C7 0.0131 0.0108 0.0065 C8 0.0126 0.0102 0.0058 C9 0.0127 0.0107 0.0063 C10 0.0129 0.0106 0.0072 C11 0.0127 0.0102 0.0063 C12 0.0177 0.0137 0.0101 C13 0.0278 0.0251 0.0133 C14 0.0232 0.0211 0.0147 C15 0.0144 0.0121 0.0067 C16 0.0225 0.0141 0.0081 C17 0.0297 0.0188 0.0075 C18 0.0180 0.0127 0.0076 C19 0.0315 0.0126 0.0077 C20 0.0306 0.0169 0.0075 C21 0.0150 0.0130 0.0104 C22 0.0149 0.0146 0.0104 C23 0.0166 0.0148 0.0094 C24 0.0151 0.0135 0.0084 C25 0.0141 0.0125 0.0076 C26 0.0131 0.0121 0.0079 C27 0.0218 0.0149 0.0106 C28 0.0291 0.0207 0.0121 C29 0.0303 0.0217 0.0143 C30 0.0206 0.0192 0.0087 C31 0.0365 0.0227 0.0104 C32 0.0289 0.0247 0.0074 C33 0.0169 0.0139 0.0065 C34 0.0203 0.0156 0.0113 C35 0.0319 0.0189 0.0066 C36 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 0.049 0.077 0.100 0.123 0.146 0.172 0.204 0.248 0.318 1.000 Number in group 841. 836. 822. 838. 812. 823. 811. 814. 830. 827. GooF 1.097 0.996 1.000 1.064 1.048 0.956 1.143 0.994 1.041 1.052 K 1.178 1.041 1.028 1.018 1.009 1.008 1.004 1.016 1.001 0.976 Resolution(A) 0.80 0.83 0.87 0.91 0.96 1.02 1.10 1.20 1.38 1.74 inf Number in group 846. 833. 828. 798. 826. 837. 807. 826. 823. 830. GooF 1.630 1.101 0.895 0.799 0.796 0.935 1.075 1.031 0.889 0.974 K 0.962 1.008 1.030 1.028 1.030 1.019 1.007 1.015 0.988 0.960 R1 0.088 0.054 0.042 0.035 0.032 0.034 0.037 0.033 0.028 0.029 Recommended weighting scheme: WGHT 0.0650 10.6512 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) -13 1 10 1411.02 3604.67 6.54 0.118 0.80 13 7 1 5205.99 9979.78 6.42 0.196 0.81 -13 7 1 5260.17 9563.14 5.90 0.192 0.81 -12 10 3 1075.87 2936.59 5.49 0.106 0.81 -13 7 2 2290.81 4324.40 5.25 0.129 0.81 -12 9 2 2946.14 5413.77 5.17 0.144 0.83 -12 2 14 8435.93 13901.58 5.12 0.231 0.80 13 3 2 1568.40 3142.93 5.02 0.110 0.85 -13 6 2 6230.26 10267.55 5.02 0.199 0.82 13 1 5 4839.62 8015.99 4.87 0.175 0.84 -8 3 22 2587.51 4439.42 4.78 0.131 0.81 13 0 9 4958.30 8088.26 4.75 0.176 0.81 -13 6 6 5445.93 8780.90 4.72 0.184 0.80 13 1 6 5513.01 8912.68 4.68 0.185 0.84 -13 4 7 771.43 1584.13 4.41 0.078 0.82 -13 4 5 2755.22 4490.86 4.28 0.131 0.83 -10 12 10 7834.78 12070.78 4.23 0.215 0.81 -13 2 4 17746.23 26290.18 4.22 0.318 0.85 -13 1 6 6047.08 9260.06 4.21 0.189 0.84 -2 3 27 23308.26 14676.96 4.19 0.237 0.80 -1 8 25 18659.56 11178.30 4.07 0.207 0.81 -9 1 21 1220.93 2052.04 4.00 0.089 0.80 -13 5 2 2917.76 4585.47 4.00 0.133 0.83 3 2 19 17172.62 23747.56 3.96 0.302 1.10 -13 4 4 5936.14 8833.80 3.92 0.184 0.83 -13 5 6 1560.36 2629.89 3.85 0.100 0.81 3 8 16 17042.25 23168.51 3.82 0.298 1.10 12 9 1 1251.32 2247.53 3.78 0.093 0.83 1 1 2 31287.85 42533.34 3.73 0.404 7.13 -11 5 3 2854.27 4326.95 3.71 0.129 0.97 -12 10 4 10271.20 14959.34 3.67 0.240 0.81 -7 4 23 745.63 1330.20 3.66 0.071 0.81 1 12 12 5143.18 7193.66 3.66 0.166 1.11 -13 4 8 2105.65 3260.29 3.61 0.112 0.81 -13 6 3 823.03 1486.91 3.60 0.076 0.82 8 0 22 14851.69 20783.64 3.59 0.282 0.82 -13 6 5 1073.29 1951.85 3.59 0.087 0.81 10 0 0 27701.05 20668.23 3.59 0.282 1.12 -12 7 10 3061.59 4424.83 3.57 0.130 0.81 12 10 2 12713.11 18271.93 3.56 0.265 0.81 -13 5 3 2517.85 3821.72 3.54 0.121 0.83 -13 3 7 1637.82 2626.13 3.52 0.100 0.82 -12 6 9 849.80 1465.51 3.52 0.075 0.83 4 9 14 17550.58 23360.41 3.52 0.299 1.11 9 13 12 7605.16 10714.62 3.51 0.203 0.80 -13 2 6 2414.65 3666.29 3.50 0.119 0.83 0 2 3 1259.06 1953.22 3.49 0.087 5.53 13 3 3 6176.08 9025.22 3.48 0.186 0.85 -3 2 26 11905.56 8080.77 3.43 0.176 0.83 -13 6 4 683.71 1250.65 3.42 0.069 0.81 Bond lengths and angles I1 - Distance Angles In1 2.7072 (0.0007) I1 I2 - Distance Angles In1 2.7159 (0.0007) I2 I3 - Distance Angles In1 2.6971 (0.0008) I3 I4 - Distance Angles In1 2.7094 (0.0007) I4 In1 - Distance Angles I3 2.6971 (0.0008) I1 2.7072 (0.0007) 110.10 (0.03) I4 2.7094 (0.0007) 107.66 (0.02) 110.47 (0.02) I2 2.7159 (0.0007) 111.69 (0.03) 108.04 (0.02) 108.88 (0.03) In1 I3 I1 I4 N1 - Distance Angles C2 1.3663 (0.0099) C6 1.3780 (0.0098) 122.42 (0.65) C1 1.4872 (0.0094) 118.85 (0.63) 118.73 (0.63) N1 C2 C6 C1 - Distance Angles N1 1.4872 (0.0094) H1A 0.9800 109.47 H1B 0.9800 109.47 109.47 H1C 0.9800 109.47 109.47 109.47 C1 N1 H1A H1B C2 - Distance Angles N1 1.3663 (0.0098) C3 1.3915 (0.0106) 117.77 (0.68) C12 1.4882 (0.0104) 120.91 (0.65) 121.32 (0.68) C2 N1 C3 C3 - Distance Angles C4 1.3686 (0.0108) C2 1.3915 (0.0106) 120.98 (0.72) H3 0.9500 119.51 119.51 C3 C4 C2 C4 - Distance Angles C3 1.3686 (0.0109) C5 1.3893 (0.0105) 119.78 (0.70) H4 0.9500 120.11 120.11 C4 C3 C5 C5 - Distance Angles C6 1.3734 (0.0107) C4 1.3893 (0.0105) 119.99 (0.71) H5 0.9500 120.00 120.00 C5 C6 C4 C6 - Distance Angles C5 1.3734 (0.0106) N1 1.3780 (0.0098) 118.83 (0.69) C27 1.4805 (0.0102) 122.11 (0.69) 119.05 (0.66) C6 C5 N1 C7 - Distance Angles C8 1.3983 (0.0106) C12 1.4162 (0.0106) 117.35 (0.70) C13 1.5124 (0.0108) 119.60 (0.68) 123.01 (0.68) C7 C8 C12 C8 - Distance Angles C9 1.3930 (0.0109) C7 1.3983 (0.0106) 122.97 (0.72) H8 0.9500 118.52 118.52 C8 C9 C7 C9 - Distance Angles C10 1.3925 (0.0105) C8 1.3930 (0.0109) 117.61 (0.70) C16 1.5102 (0.0104) 117.60 (0.67) 124.78 (0.69) C9 C10 C8 C10 - Distance Angles C9 1.3925 (0.0106) C11 1.3956 (0.0106) 122.80 (0.71) H10 0.9500 118.60 118.60 C10 C9 C11 C11 - Distance Angles C10 1.3956 (0.0106) C12 1.4100 (0.0110) 117.78 (0.69) C19 1.5223 (0.0105) 119.81 (0.69) 122.39 (0.68) C11 C10 C12 C12 - Distance Angles C11 1.4100 (0.0110) C7 1.4162 (0.0106) 121.47 (0.69) C2 1.4882 (0.0104) 118.76 (0.67) 119.69 (0.68) C12 C11 C7 C13 - Distance Angles C7 1.5124 (0.0108) C14 1.5182 (0.0118) 111.92 (0.70) C15 1.5375 (0.0117) 110.89 (0.66) 110.59 (0.70) H13 1.0000 107.75 107.75 107.75 C13 C7 C14 C15 C14 - Distance Angles C13 1.5182 (0.0117) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 C13 H14A H14B C15 - Distance Angles C13 1.5375 (0.0117) H15A 0.9800 109.47 H15B 0.9800 109.47 109.47 H15C 0.9800 109.47 109.47 109.47 C15 C13 H15A H15B C16 - Distance Angles C9 1.5102 (0.0104) C18 1.5327 (0.0108) 113.64 (0.65) C17 1.5343 (0.0108) 110.19 (0.63) 109.38 (0.65) H16 1.0000 107.81 107.81 107.81 C16 C9 C18 C17 C17 - Distance Angles C16 1.5343 (0.0108) H17A 0.9800 109.47 H17B 0.9800 109.47 109.47 H17C 0.9800 109.47 109.47 109.47 C17 C16 H17A H17B C18 - Distance Angles C16 1.5327 (0.0108) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 C16 H18A H18B C19 - Distance Angles C11 1.5223 (0.0105) C21 1.5272 (0.0108) 110.78 (0.64) C20 1.5398 (0.0111) 110.99 (0.65) 110.71 (0.68) H19 1.0000 108.08 108.08 108.08 C19 C11 C21 C20 C20 - Distance Angles C19 1.5398 (0.0111) H20A 0.9800 109.47 H20B 0.9800 109.47 109.47 H20C 0.9800 109.47 109.47 109.47 C20 C19 H20A H20B C21 - Distance Angles C19 1.5272 (0.0109) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C21 C19 H21A H21B C22 - Distance Angles C23 1.3965 (0.0108) C27 1.4122 (0.0106) 117.97 (0.71) C28 1.5105 (0.0108) 119.60 (0.71) 122.43 (0.68) C22 C23 C27 C23 - Distance Angles C22 1.3965 (0.0108) C24 1.3982 (0.0113) 121.85 (0.74) H23 0.9500 119.08 119.08 C23 C22 C24 C24 - Distance Angles C23 1.3982 (0.0113) C25 1.4059 (0.0111) 118.83 (0.71) C31 1.5070 (0.0106) 120.02 (0.72) 121.07 (0.73) C24 C23 C25 C25 - Distance Angles C26 1.3906 (0.0108) C24 1.4059 (0.0111) 121.52 (0.73) H25 0.9500 119.24 119.24 C25 C26 C24 C26 - Distance Angles C25 1.3906 (0.0108) C27 1.4159 (0.0106) 118.29 (0.71) C34 1.5247 (0.0108) 121.54 (0.70) 120.08 (0.67) C26 C25 C27 C27 - Distance Angles C22 1.4122 (0.0106) C26 1.4159 (0.0106) 121.52 (0.68) C6 1.4805 (0.0102) 119.70 (0.67) 118.76 (0.66) C27 C22 C26 C28 - Distance Angles C22 1.5105 (0.0108) C29 1.5282 (0.0123) 110.37 (0.69) C30 1.5379 (0.0120) 112.37 (0.70) 110.26 (0.69) H28 1.0000 107.89 107.89 107.89 C28 C22 C29 C30 C29 - Distance Angles C28 1.5282 (0.0123) H29A 0.9800 109.47 H29B 0.9800 109.47 109.47 H29C 0.9800 109.47 109.47 109.47 C29 C28 H29A H29B C30 - Distance Angles C28 1.5379 (0.0120) H30A 0.9800 109.47 H30B 0.9800 109.47 109.47 H30C 0.9800 109.47 109.47 109.47 C30 C28 H30A H30B C31 - Distance Angles C24 1.5070 (0.0106) C33 1.5163 (0.0112) 112.49 (0.72) C32 1.5430 (0.0120) 110.31 (0.67) 110.25 (0.73) H31 1.0000 107.87 107.87 107.87 C31 C24 C33 C32 C32 - Distance Angles C31 1.5430 (0.0120) H32A 0.9800 109.47 H32B 0.9800 109.47 109.47 H32C 0.9800 109.47 109.47 109.47 C32 C31 H32A H32B C33 - Distance Angles C31 1.5163 (0.0112) H33A 0.9800 109.47 H33B 0.9800 109.47 109.47 H33C 0.9800 109.47 109.47 109.47 C33 C31 H33A H33B C34 - Distance Angles C36 1.5198 (0.0105) C26 1.5247 (0.0108) 112.85 (0.67) C35 1.5253 (0.0111) 110.24 (0.67) 111.24 (0.63) H34 1.0000 107.41 107.41 107.41 C34 C36 C26 C35 C35 - Distance Angles C34 1.5253 (0.0111) H35A 0.9800 109.47 H35B 0.9800 109.47 109.47 H35C 0.9800 109.47 109.47 109.47 C35 C34 H35A H35B C36 - Distance Angles C34 1.5198 (0.0104) H36A 0.9800 109.47 H36B 0.9800 109.47 109.47 H36C 0.9800 109.47 109.47 109.47 C36 C34 H36A H36B Selected torsion angles 4.34 ( 1.10) C6 - N1 - C2 - C3 -175.27 ( 0.68) C1 - N1 - C2 - C3 -176.17 ( 0.68) C6 - N1 - C2 - C12 4.22 ( 1.07) C1 - N1 - C2 - C12 -0.07 ( 1.14) N1 - C2 - C3 - C4 -179.55 ( 0.72) C12 - C2 - C3 - C4 -2.86 ( 1.17) C2 - C3 - C4 - C5 1.64 ( 1.15) C3 - C4 - C5 - C6 2.44 ( 1.12) C4 - C5 - C6 - N1 -176.27 ( 0.69) C4 - C5 - C6 - C27 -5.55 ( 1.10) C2 - N1 - C6 - C5 174.06 ( 0.69) C1 - N1 - C6 - C5 173.20 ( 0.69) C2 - N1 - C6 - C27 -7.19 ( 1.01) C1 - N1 - C6 - C27 -0.72 ( 1.13) C12 - C7 - C8 - C9 177.22 ( 0.72) C13 - C7 - C8 - C9 0.77 ( 1.14) C7 - C8 - C9 - C10 -178.82 ( 0.73) C7 - C8 - C9 - C16 0.17 ( 1.13) C8 - C9 - C10 - C11 179.79 ( 0.69) C16 - C9 - C10 - C11 -1.09 ( 1.12) C9 - C10 - C11 - C12 -179.35 ( 0.71) C9 - C10 - C11 - C19 1.12 ( 1.12) C10 - C11 - C12 - C7 179.33 ( 0.70) C19 - C11 - C12 - C7 -175.50 ( 0.67) C10 - C11 - C12 - C2 2.72 ( 1.12) C19 - C11 - C12 - C2 -0.26 ( 1.13) C8 - C7 - C12 - C11 -178.12 ( 0.71) C13 - C7 - C12 - C11 176.33 ( 0.68) C8 - C7 - C12 - C2 -1.54 ( 1.13) C13 - C7 - C12 - C2 -97.42 ( 0.90) N1 - C2 - C12 - C11 82.05 ( 0.97) C3 - C2 - C12 - C11 85.90 ( 0.95) N1 - C2 - C12 - C7 -94.63 ( 0.93) C3 - C2 - C12 - C7 66.43 ( 0.95) C8 - C7 - C13 - C14 -115.75 ( 0.84) C12 - C7 - C13 - C14 -57.57 ( 0.97) C8 - C7 - C13 - C15 120.25 ( 0.82) C12 - C7 - C13 - C15 -163.91 ( 0.71) C10 - C9 - C16 - C18 15.68 ( 1.10) C8 - C9 - C16 - C18 72.94 ( 0.85) C10 - C9 - C16 - C17 -107.47 ( 0.85) C8 - C9 - C16 - C17 73.98 ( 0.93) C10 - C11 - C19 - C21 -104.20 ( 0.86) C12 - C11 - C19 - C21 -49.43 ( 0.96) C10 - C11 - C19 - C20 132.39 ( 0.77) C12 - C11 - C19 - C20 0.71 ( 1.20) C27 - C22 - C23 - C24 -179.87 ( 0.77) C28 - C22 - C23 - C24 -1.38 ( 1.22) C22 - C23 - C24 - C25 -178.09 ( 0.75) C22 - C23 - C24 - C31 0.76 ( 1.20) C23 - C24 - C25 - C26 177.43 ( 0.75) C31 - C24 - C25 - C26 0.48 ( 1.16) C24 - C25 - C26 - C27 -176.19 ( 0.75) C24 - C25 - C26 - C34 0.59 ( 1.19) C23 - C22 - C27 - C26 -178.82 ( 0.75) C28 - C22 - C27 - C26 178.97 ( 0.72) C23 - C22 - C27 - C6 -0.43 ( 1.19) C28 - C22 - C27 - C6 -1.17 ( 1.18) C25 - C26 - C27 - C22 175.55 ( 0.73) C34 - C26 - C27 - C22 -179.57 ( 0.70) C25 - C26 - C27 - C6 -2.85 ( 1.11) C34 - C26 - C27 - C6 -80.55 ( 1.01) C5 - C6 - C27 - C22 100.74 ( 0.88) N1 - C6 - C27 - C22 97.88 ( 0.94) C5 - C6 - C27 - C26 -80.83 ( 0.94) N1 - C6 - C27 - C26 -66.09 ( 0.99) C23 - C22 - C28 - C29 113.30 ( 0.86) C27 - C22 - C28 - C29 57.43 ( 1.03) C23 - C22 - C28 - C30 -123.17 ( 0.85) C27 - C22 - C28 - C30 -127.65 ( 0.85) C23 - C24 - C31 - C33 55.71 ( 1.03) C25 - C24 - C31 - C33 108.80 ( 0.90) C23 - C24 - C31 - C32 -67.84 ( 1.01) C25 - C24 - C31 - C32 -34.84 ( 1.05) C25 - C26 - C34 - C36 148.54 ( 0.76) C27 - C26 - C34 - C36 89.67 ( 0.90) C25 - C26 - C34 - C35 -86.94 ( 0.89) C27 - C26 - C34 - C35 FMAP and GRID set by program FMAP 2 3 26 GRID -1.087 -2 -2 1.087 2 2 R1 = 0.0358 for 4667 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.37 at 0.8196 0.0390 0.0126 [ 1.39 A from I1 ] Deepest hole -1.99 at 0.9784 -0.0014 0.0496 [ 0.71 A from IN1 ] Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including eq.) Q1 1 0.1804 0.5390 0.4874 1.00000 0.05 1.37 1.39 I1 1.43 IN1 3.22 I3 3.37 H10 Q2 1 0.2045 0.5305 0.4716 1.00000 0.05 1.31 1.26 I1 1.47 IN1 3.31 H4 3.33 I2 Q3 1 0.1990 0.5028 0.4361 1.00000 0.05 1.28 1.35 IN1 1.91 I1 2.65 H4 2.83 I4 Q4 1 0.1821 0.5433 0.5064 1.00000 0.05 1.16 1.35 I1 1.73 IN1 3.07 H10 3.12 I3 Q5 1 -0.0787 0.6088 0.3503 1.00000 0.05 1.14 1.36 I2 1.94 H1C 2.76 C1 2.84 H1A Shortest distances between peaks (including symmetry equivalents) 1 4 0.43 1 2 0.46 2 4 0.84 2 3 0.91 1 3 1.30 3 4 1.71 Time profile in seconds ----------------------- 0.02: 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. 0.09: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.08: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.19: Structure factors and derivatives 0.18: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.05: Solve l.s. equations 0.00: Generate HTAB table 0.18: Other dependent quantities, CIF, tables 0.01: Analysis of variance 0.04: Merge reflections for Fourier and .fcf 0.00: 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. +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + rudi005 finished at 16:12:22 Total elapsed time: 0.88 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++