****************************************************************************** test structure: loganin 30/ 9/1998 at 2:17:18 SIR97(1.02) runs on: loganin Used commands & directives: %data cell 8.187 14.277 15.693 90 90 90 space p 21 21 21 cont c 68 h 104 o 40 refl loganin.hkl %normal default %invariants default %phase default %fourier default %menu default %end Files used in sir: Channel Name 5 instruction input file loganin.sir 6 printer output file loganin.out 30 direct access structure file loganin.bin 31 direct access scratch file 32 sequential scratch file 34 reflection input file loganin.hkl 41 scattering factors file C:\SIR97\SirWare.xen ( Release : 12.96 ) 35 fourier peaks file loganin.ins 36 peaks file to be plotted loganin.plt 33 sequential scratch file Direct access structure file has been initialized 1++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ SIR97 : Data routine Release 97.01 test structure: loganin ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Direct cell a = 8.187 b = 14.277 c = 15.693 alpha = 90.000 beta = 90.000 gamma = 90.000 Crystal family : orthorhombic Space group (noncentrosymmetric) : P 21 21 21 Symmetry-operations 1) x , y , z 2) -x+1/2, -y , z+1/2 3) x+1/2, -y+1/2, -z 4) -x , y+1/2, -z+1/2 Seminvariant condition : g g g Space Group Number = 19 X-ray scattering factors Unit cell contents and scattering factor constants Atom Symbol Number in cell Atomic number Hydrogen H 104 1 Carbon C 68 6 Oxygen O 40 8 f = sum ( a(i) * exp(-b(i)*s2) ) i=1,4 + c a(1) b(1) a(2) b(2) a(3) b(3) a(4) b(4) c H .490 20.659 .262 7.740 .197 49.552 .050 2.202 .001 C 2.310 20.844 1.020 10.207 1.589 .569 .865 51.651 .216 O 3.048 13.277 2.287 5.701 1.546 .324 .867 32.909 .251 Number of atoms in asymmetric unit = 27.00 Equivalent number of equal atoms in primitive cell = 107 Cell volume = 1834.29 Volume per atom = 16.98 3498 input reflections 2428 independent input reflections 10 18 20 maximum h,k,l values .4500 maximum s**2 = (sin(theta)/lambda)**2 .7453 Angstrom resolution 15928 maximum super-index ( must be less then 200000 ) 194 reflections are not in input data Symmetry equivalent reflections merged: Rsym(F) = 2.03% 1++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ SIR97 : Normalization routine Release 97.01 test structure: loganin ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ -2.374 -1.949 -1.524 -1.100 -.675 -.250 * * * * * * ********************************************************* * * * * .034* *w ** * x * * w* * * w * * * w * * .114* w * ** * w * * * x * * * w * * * w * .194* * w ** * * w * * * w ********************************** * * w * y = s**2 * * x * x = ln / sigfsq * .274* w * * ( w ) = wilson * * w * * ( * ) = calc * * w * ********************************** * w * * intercept = -.08737 * * w * * slope = -5.27746 * .354* w * * b(iso) = 2.63873 * * w* * u(iso) = .03342 * * x * scale = 1.09130 * * *w * scale*f(obs.)**2 = f(abs.)**2 * * * w ********************************** .433* * w ** * * * * ********************************************************* * * * * * * ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ *** pseudotranslation section *** test structure: loganin *** program searched for pseudo-translational symmetry *** *** no pseudo-translational symmetry has been found *** ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ *** Final statistics section *** Distribution of with sin(theta)/lambda sinth/lambda .0671 .1342 .2013 .2683 .3354 .8075 1.3774 .7325 1.0309 .8330 number 1 67 178 347 546 sinth/lambda .4025 .4696 .5367 .6038 .6709 .8559 1.3843 .9797 .8409 1.0593 number 857 1192 1541 1953 1864 Average values Average Numeric Graphic all data acentric centric hypercentric a. c. h. mod(E) .865 .886 .798 .718 * E**2 1.000 1.000 1.000 1.000 E**3 1.419 1.329 1.596 1.916 * E**4 2.364 2.000 3.000 4.500 * E**5 4.497 3.323 6.383 12.260 * E**6 9.593 6.000 15.000 37.500 * mod(E**2-1) .805 .736 .968 1.145 * (E**2-1)**2 1.364 1.000 2.000 3.500 * (E**2-1)**3 4.501 2.000 8.000 26.000 * (mod(E**2-1))**3 4.974 2.415 8.691 26.903 * n(z) cumulative probability distribution z all data acentric centric hypercentric a. c. h. .1 .115 .095 .248 .368 * .2 .213 .181 .345 .463 * .3 .296 .259 .416 .526 * .4 .372 .330 .473 .574 * .5 .437 .393 .520 .612 * .6 .495 .451 .561 .643 * .7 .546 .503 .597 .670 * .8 .589 .551 .629 .694 * .9 .627 .593 .657 .715 * 1.0 .658 .632 .683 .733 * 1.2 .718 .699 .727 .765 * 1.4 .763 .753 .763 .791 * 1.6 .811 .798 .794 .813 * 1.8 .838 .835 .820 .832 * 2.0 .863 .865 .843 .848 * 2.2 .883 .889 .862 .863 * 2.4 .901 .909 .879 .875 * 2.6 .913 .926 .893 .886 * 2.8 .928 .939 .906 .896 * 3.0 .935 .950 .917 .905 * 3.2 .946 .959 .926 .913 * 3.4 .953 .967 .935 .920 * 3.6 .962 .973 .942 .926 * 3.8 .966 .978 .949 .932 * 4.0 .972 .982 .954 .938 * Distribution of E - number of E's .gt. limit E .6 .7 .8 .9 1.0 1.1 1.2 1.3 1.4 1.5 number 1570 1364 1164 982 831 679 553 437 353 282 E 1.6 1.7 1.8 1.9 2.0 2.1 2.2 2.3 2.4 2.5 number 230 182 137 103 78 60 46 34 23 16 Number and percentage Number and percentage of F's > param * sigma(F) of F's > limit number percentage param number percentage limit 2399 99% .50 242 10% 24.58 2329 96% 1.00 484 20% 15.74 2298 95% 1.50 726 30% 11.82 2279 94% 2.00 968 40% 9.50 2253 93% 2.50 1210 50% 7.72 2225 92% 3.00 1452 60% 6.24 2202 91% 3.50 1694 70% 5.05 2176 90% 4.00 1936 80% 3.78 2151 89% 4.50 2178 90% 2.52 2127 88% 5.00 2420 100% .74 272 largest E-values to phase. ( 10 printed ) code h k l E fo/sig. code h k l E fo/sig. 1 0 11 7 3.758 >6 2 0 13 2 3.627 >6 3 1 14 0 3.446 >6 4 8 10 5 2.946 >6 5 0 10 7 2.898 >6 6 0 1 4 2.819 >6 7 6 6 3 2.812 >6 8 3 5 15 2.704 >6 9 0 4 6 2.677 >6 10 6 5 2 2.675 >6 . . . . . . . . . . . . 296 smallest E-values for psi0 and negative quartets ( 10 printed ) code h k l E fo/sig. code h k l E fo/sig. 2419 2 7 10 .058 .50 2420 3 7 8 .052 .54 2421 6 0 6 .050 .50 2422 1 2 12 .045 .55 2423 1 2 0 .043 >6 2424 1 0 8 .039 2.58 2425 0 3 10 .034 .55 2426 0 5 8 .029 .46 2427 1 3 0 .029 5.37 2428 0 7 3 .020 .50 1++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ SIR97 : Invariants routine Release 97.01 test structure: loganin ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Triplets statistic distribution of g - number of g's .gt. limit g .0 .2 .4 .6 .8 1.0 1.2 1.4 1.6 2.0 2.5 3.0 no. 3589 3234 3168 3127 2733 2377 2010 1705 1389 921 537 307 4138 strong triplets found among 272 strongest reflections (E-min = 1.518) strengthned by 56 free vectors using P-10 formula 8000 Psi-zero triplets found among 272 strongest reflections and the 296 weakest reflections 5521 negative quartets found among 8000 psi-zero relationships Negative quartets statistic distribution of g - number of g's .gt. limit g .0 .2 .4 .6 .8 1.0 1.2 1.4 1.6 2.0 2.5 3.0 no. 4000 2235 535 140 47 25 14 9 7 4 3 3 number of relationships calculated stored positive estimated triplets 3085 3085 negative estimated triplets 149 149 enantiomorph sensitive triplets 355 355 psi-zero triplets 8000 8000 negative estimated quartets 3374 3374 enantiomorph sensitive quartets 500 500 1++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ SIR97 : Phase routine Release 97.01 test structure: loganin ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ *** converge / diverge section *** Origin fixing reflexion(s) phase assigned code h k l E restriction phase 37 3 0 13 2.29 90,270 90 14 0 2 3 2.58 0,180 360 90 0 11 6 1.97 90,270 90 Selected symbols phase code h k l E restriction 77 4 0 1 2.04 90,270 53 3 6 11 2.14 any 2 0 13 2 3.63 90,270 22 0 2 4 2.43 0,180 38 8 0 0 2.29 0,180 Enantiomorph fixing reflexion code h k l E 30 6 7 0 2.36 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ *** tangent formula section *** the total number of permutations is 64 the maximum number of sets stored will be 10 a set with cfom greater than .950 has been found. the multisolution procedure has been stopped. +++++++++++++ Figures of merit ++++++++++++ mabs alcomb pscomb R(x,y) cphase cfom min 1.347 1.000 1.000 .788 1.000 1.000 max 1.347 1.000 1.000 .788 1.000 1.000 set (trial) mabs alcomb pscomb R(x,y) cphase cfom nund 1 ( 1) 1.347 1.000 1.000 .788 1.000 1.000 0 1++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Fourier / Least-Squares Routine Release 97.01 test structure: loganin ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ *** fast fourier transform section *** +--------------------------------------------------------------------------+ I Space group symbol P 21 21 21 I I I I Unit cell parameters 8.187 14.277 15.693 I I 90.000 90.000 90.000 I I I I Number of grid points along X, Y, Z 25 45 48 I I I I Maximum h, k, l value 10 18 20 I I I I Number of independent reflections input 1571 I I I I Number of reflections in one hemisphere 5632 I I I I Grid spacing (in angstrom) approximately .333 I I I I Scale .594 I +--------------------------------------------------------------------------+ I A number of atoms has to be found such that I I the sum of site occupancies ( occ. ) is equal to 27.000 I +--------------------------------------------------------------------------+ I 1570 ( 65% of total ) reflections used with Fo > 3.07 I I In step B scale factor, atomic coordinates and isotropic I I thermal factors are refined via diagonal matrix. I +--------------------------------------------------------------------------+ 29 1 8 0 1 14 0 2 8 0 2 9 0 3 6 0 4 26 0 5 12 0 5 14 0 6 8 0 6 13 0 7 25 0 9 10 0 9 26 0 10 13 0 10 18 0 11 14 0 11 16 0 11 24 0 12 17 0 13 20 0 15 17 0 15 21 0 16 17 0 16 23 0 21 27 0 22 24 0 23 25 0 24 25 0 15 19 0 ------------ Set no. 1 -------------------- Best R-Factor = 14.13% Step A: 18.10% 17.90% 16.26% 16.12% 16.11% 15.93% Step B: 15.46% 14.13% 19.97% ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ *** Final interpretation *** test structure: loganin Assumed atomic parameters and limits for interatomic bonds and angles (interspecies and intraspecies) distances angles atomic user type radius minimum maximum minimum maximum number conditions O .730 1.11 1.91 85.00 145.00 8.000 C .770 1.15 1.95 85.00 145.00 6.000 Tentative of peak labelling in terms of atomic species group peaks possible species range of number included chemical species assigned bond angles 1 8 O O 85. - 145. 2 19 C C 85. - 145. range of bond distances used to build fragments group group 1 group 2 1 ( 1.1 - 1.9 ) ( 1.1 - 1.9 ) 2 ( 1.2 - 1.9 ) ------------------------------------------------------------------------------ interpeak distances up to 2.40 1) 2( 1) 2.27 3( 1) 2.32 5( 1) 2.37 7( 1) 2.38 11( 1) 1.38 17( 1) 1.46 2) 1( 1) 2.27 11( 1) 1.44 13( 1) 1.46 24( 1) 2.39 3) 1( 1) 2.32 12( 1) 1.38 16( 1) 2.37 17( 1) 1.41 4) 5( 1) 1.44 18( 1) 2.39 5) 1( 1) 2.37 4( 1) 1.44 11( 1) 1.56 18( 1) 1.51 21( 1) 2.38 6) 26( 1) 1.40 7) 1( 1) 2.38 14( 1) 1.59 17( 1) 1.55 25( 1) 1.53 26( 1) 2.37 8) 10( 1) 1.42 13( 1) 1.56 18( 1) 1.55 9) 24( 1) 1.44 10) 8( 1) 1.42 11) 1( 1) 1.38 2( 1) 1.44 5( 1) 1.56 17( 1) 2.35 12) 3( 1) 1.38 16( 1) 1.31 17( 1) 2.39 13) 2( 1) 1.46 8( 1) 1.56 24( 1) 1.52 14) 7( 1) 1.59 16( 1) 1.52 23( 1) 1.57 15) 16( 1) 1.51 20( 1) 1.18 22( 1) 1.30 27( 1) 2.30 16) 3( 1) 2.37 12( 1) 1.31 14( 1) 1.52 15( 1) 1.51 20( 1) 2.37 22( 1) 2.34 17) 1( 1) 1.46 3( 1) 1.41 7( 1) 1.55 11( 1) 2.35 12( 1) 2.39 18) 4( 1) 2.39 5( 1) 1.51 8( 1) 1.55 21( 1) 1.39 19) 25( 1) 1.55 20) 15( 1) 1.18 16( 1) 2.37 22( 1) 2.20 21) 5( 1) 2.38 18( 1) 1.39 22) 15( 1) 1.30 16( 1) 2.34 20( 1) 2.20 27( 1) 1.43 23) 14( 1) 1.57 26( 1) 1.57 24) 2( 1) 2.39 9( 1) 1.44 13( 1) 1.52 25) 7( 1) 1.53 19( 1) 1.55 26( 1) 1.55 26) 6( 1) 1.40 7( 1) 2.37 23( 1) 1.57 25( 1) 1.55 27) 15( 1) 2.30 22( 1) 1.43 accepted distances in this interpretation 1) 11( 1) 1.38 17( 1) 1.46 2) 11( 1) 1.44 13( 1) 1.46 3) 12( 1) 1.38 17( 1) 1.41 4) 5( 1) 1.44 5) 4( 1) 1.44 11( 1) 1.56 18( 1) 1.51 6) 26( 1) 1.40 7) 14( 1) 1.59 17( 1) 1.55 25( 1) 1.53 8) 10( 1) 1.42 13( 1) 1.56 18( 1) 1.55 9) 24( 1) 1.44 10) 8( 1) 1.42 11) 1( 1) 1.38 2( 1) 1.44 5( 1) 1.56 12) 3( 1) 1.38 16( 1) 1.31 13) 2( 1) 1.46 8( 1) 1.56 24( 1) 1.52 14) 7( 1) 1.59 16( 1) 1.52 23( 1) 1.57 15) 16( 1) 1.51 20( 1) 1.18 22( 1) 1.30 16) 12( 1) 1.31 14( 1) 1.52 15( 1) 1.51 17) 1( 1) 1.46 3( 1) 1.41 7( 1) 1.55 18) 5( 1) 1.51 8( 1) 1.55 21( 1) 1.39 19) 25( 1) 1.55 20) 15( 1) 1.18 21) 18( 1) 1.39 22) 15( 1) 1.30 27( 1) 1.43 23) 14( 1) 1.57 26( 1) 1.57 24) 9( 1) 1.44 13( 1) 1.52 25) 7( 1) 1.53 19( 1) 1.55 26( 1) 1.55 26) 6( 1) 1.40 23( 1) 1.57 25( 1) 1.55 27) 22( 1) 1.43 bond angles in this interpretation ( 11( 1) - 1 - 17( 1)) 112.0 ( 11( 1) - 2 - 13( 1)) 112.1 ( 12( 1) - 3 - 17( 1)) 117.8 ( 4( 1) - 5 - 11( 1)) 107.6 ( 4( 1) - 5 - 18( 1)) 108.1 ( 11( 1) - 5 - 18( 1)) 109.2 ( 14( 1) - 7 - 17( 1)) 111.4 ( 14( 1) - 7 - 25( 1)) 104.5 ( 17( 1) - 7 - 25( 1)) 111.8 ( 10( 1) - 8 - 13( 1)) 110.5 ( 10( 1) - 8 - 18( 1)) 110.2 ( 13( 1) - 8 - 18( 1)) 110.4 ( 1( 1) - 11 - 2( 1)) 107.4 ( 1( 1) - 11 - 5( 1)) 107.7 ( 2( 1) - 11 - 5( 1)) 107.7 ( 3( 1) - 12 - 16( 1)) 123.5 ( 2( 1) - 13 - 8( 1)) 107.2 ( 2( 1) - 13 - 24( 1)) 106.6 ( 8( 1) - 13 - 24( 1)) 110.4 ( 7( 1) - 14 - 16( 1)) 111.0 ( 7( 1) - 14 - 23( 1)) 103.4 ( 16( 1) - 14 - 23( 1)) 110.9 ( 16( 1) - 15 - 20( 1)) 122.3 ( 16( 1) - 15 - 22( 1)) 112.6 ( 20( 1) - 15 - 22( 1)) 125.0 ( 12( 1) - 16 - 14( 1)) 124.1 ( 12( 1) - 16 - 15( 1)) 120.1 ( 14( 1) - 16 - 15( 1)) 115.7 ( 1( 1) - 17 - 3( 1)) 108.4 ( 1( 1) - 17 - 7( 1)) 104.8 ( 3( 1) - 17 - 7( 1)) 113.1 ( 5( 1) - 18 - 8( 1)) 109.5 ( 5( 1) - 18 - 21( 1)) 110.2 ( 8( 1) - 18 - 21( 1)) 110.5 ( 15( 1) - 22 - 27( 1)) 114.9 ( 14( 1) - 23 - 26( 1)) 105.9 ( 9( 1) - 24 - 13( 1)) 109.0 ( 7( 1) - 25 - 19( 1)) 113.1 ( 7( 1) - 25 - 26( 1)) 100.3 ( 19( 1) - 25 - 26( 1)) 112.8 ( 6( 1) - 26 - 23( 1)) 111.4 ( 6( 1) - 26 - 25( 1)) 109.5 ( 23( 1) - 26 - 25( 1)) 102.2 ------------------------------------------------------------------------------ ------------------------------------------------------------------------------ fragment n. 1 ,fused rings could be found around peaks 7 11 14 17 --------------------- overall plot of the structure ------------------------- ------------ projection on l.s.q. plane ---- scale : 2.03 cms/a ------------ 27 * * 22 * * 21 20 * 4 * *15 * * * * * 18 * 5 * * 16 * *12 * * 10 * * * * * * 8 * 11 14 3 * * * * 1 * * * * * * 23 * * * 13 * 17 * * * * 2 * 7 * * * * * 24 26 * * * 25 * * * * 6 * 9 19 ---------------------------------------------------------------------------- fragment number 1 , 27 peaks included peak 1 2 3 4 5 6 7 8 9 10 11 12 13 linked to 11 11 12 5 4 26 14 10 24 8 1 3 2 17 13 17 11 17 13 2 16 8 18 25 18 5 24 ring * * * * * * * * * peak 14 15 16 17 18 19 20 21 22 23 24 25 26 linked to 7 16 12 1 5 25 15 18 15 14 9 7 6 16 20 14 3 8 27 26 13 19 23 23 22 15 7 21 26 25 ring * * * * * * * peak 27 linked to 22 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ *** Output section *** test structure: loganin Final residual value = 14.13% Serial Atom Height x y z Occ. B[iso] Frag 1) O 1 835 .037 .528 .994 1.000 2.25 1 2) O 2 771 .265 .466 1.055 1.000 2.37 1 3) O 3 756 .050 .518 .847 1.000 2.44 1 4) O 4 737 -.134 .358 1.014 1.000 2.51 1 5) C 5 675 .010 .381 1.063 1.000 3.86 1 6) O 6 657 -.075 .863 .917 1.000 3.47 1 7) C 7 653 -.006 .669 .917 1.000 3.90 1 8) C 8 649 .267 .314 1.124 1.000 3.82 1 9) O 9 646 .614 .473 1.058 1.000 3.26 1 10) O 10 646 .357 .230 1.138 1.000 2.77 1 11) C 11 645 .119 .445 1.007 1.000 2.08 1 12) C 12 637 -.113 .508 .826 1.000 2.13 1 13) C 13 620 .366 .383 1.068 1.000 2.90 1 14) C 14 615 -.196 .654 .903 1.000 2.38 1 15) C 15 608 -.405 .544 .832 1.000 2.47 1 16) C 16 608 -.228 .565 .852 1.000 2.20 1 17) C 17 604 .089 .575 .917 1.000 2.18 1 18) C 18 586 .100 .291 1.082 1.000 2.65 1 19) C 19 554 .217 .776 .855 1.000 2.60 1 20) O 20 546 -.513 .590 .860 1.000 2.55 1 21) C 21 527 .007 .234 1.134 1.000 1.70 1 22) C 22 524 -.423 .470 .786 1.000 1.71 1 23) C 23 502 -.250 .743 .852 1.000 2.75 1 24) C 24 480 .518 .416 1.115 1.000 3.28 1 25) C 25 476 .046 .732 .843 1.000 2.33 1 26) C 26 470 -.094 .806 .845 1.000 2.63 1 27) C 27 346 -.588 .451 .760 1.000 3.81 1 28) Q 28 131 .129 .656 .920 1.000 29) Q 29 115 -.138 .577 .901 1.000 30) Q 30 111 .428 .408 1.000 1.000 31) Q 31 109 -.230 .825 .834 1.000 32) Q 32 109 -.026 .300 1.060 1.000 1++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Least-Squares Routine Release 97.01 test structure: loganin ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Used directives: FullMatrix Cutoff 3 Damping 1.0 Cycles 3 Iso O(1) O(2) O(3) O(4) C(5) O(6) C(7) C(8) O(9) O(10) C(11) C(12) Iso C(13) C(14) C(15) C(16) C(17) C(18) C(19) O(20) C(21) C(22) Iso C(23) C(24) C(25) C(26) C(27) Structure factor least squares (Vers. 2496) Weighting scheme no. 6 Parameter(s) provided 1 p(1) p(2) p(3) p(4) 1.00000 Cycle(s) requested 3 threshold=n*sig(fo) 3 4 5 6 no. reflections... 2224 2176 2124 2062 no(refl)/param.... 20.40 19.96 19.49 18.92 R(F)% (+)..... 15.886 15.767 15.622 15.439 wR(F**2)% (+)..... 15.228 15.194 15.138 15.069 R(F)% (-)..... 15.885 15.767 15.622 15.438 wR(F**2)% (-)..... 15.228 15.195 15.138 15.069 goodnes of fit.... 2.828 2.854 2.879 2.910 Hamilton test out of range! minimization function = 16919.4900 Structure factor least squares calculation 1 ends minimum (shift/e.s.d.) = .01 maximum (shift/e.s.d.) = 12.95 mean (shift/e.s.d.) = 1.38 sum of the squares of the (shift/e.s.d.) = 551.54 average value of B(equiv) = 2.720 number of refined parameters 109 threshold=n*sig(fo) 3 4 5 6 no. reflections... 2224 2176 2124 2062 no(refl)/param.... 20.40 19.96 19.49 18.92 R(F)% (+)..... 13.458 13.356 13.211 13.068 wR(F**2)% (+)..... 13.005 12.978 12.924 12.877 R(F)% (-)..... 13.458 13.356 13.212 13.069 wR(F**2)% (-)..... 13.005 12.978 12.924 12.877 goodnes of fit.... 2.415 2.438 2.458 2.487 Hamilton test out of range! minimization function = 12340.0400 Structure factor least squares calculation 2 ends minimum (shift/e.s.d.) = .00 maximum (shift/e.s.d.) = 3.72 mean (shift/e.s.d.) = .35 sum of the squares of the (shift/e.s.d.) = 36.84 threshold=n*sig(fo) 3 4 5 6 no. reflections... 2224 2176 2124 2062 no(refl)/param.... 20.40 19.96 19.49 18.92 R(F)% (+)..... 13.352 13.265 13.131 12.993 wR(F**2)% (+)..... 12.885 12.861 12.811 12.764 R(F)% (-)..... 13.352 13.264 13.131 12.993 wR(F**2)% (-)..... 12.885 12.861 12.811 12.764 goodnes of fit.... 2.393 2.416 2.437 2.465 Hamilton test out of range! minimization function = 12113.4900 Structure factor least squares calculation 3 ends minimum (shift/e.s.d.) = .00 maximum (shift/e.s.d.) = .41 mean (shift/e.s.d.) = .07 sum of the squares of the (shift/e.s.d.) = 1.22 threshold=n*sig(fo) 3 4 5 6 no. reflections... 2224 2176 2124 2062 no(refl)/param.... 20.40 19.96 19.49 18.92 R(F)% (+)..... 13.348 13.261 13.127 12.987 wR(F**2)% (+)..... 12.880 12.856 12.806 12.758 R(F)% (-)..... 13.348 13.260 13.127 12.987 wR(F**2)% (-)..... 12.880 12.857 12.807 12.759 goodnes of fit.... 2.392 2.415 2.436 2.464 Hamilton test out of range! minimization function = 12104.5100 Structure factor least squares calculation 4 ends ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ 1++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Least-Squares Routine Release 97.01 test structure: loganin ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Used directives: FullMatrix Cutoff 3 Damping 1.0 Cycles 3 Aniso O(1) O(2) O(3) O(4) C(5) O(6) C(7) C(8) O(9) O(10) C(11) C(12) Aniso C(13) C(14) C(15) C(16) C(17) C(18) C(19) O(20) C(21) C(22) Aniso C(23) C(24) C(25) C(26) C(27) Structure factor least squares (Vers. 2496) Weighting scheme no. 6 Parameter(s) provided 1 p(1) p(2) p(3) p(4) 1.00000 Cycle(s) requested 3 threshold=n*sig(fo) 3 4 5 6 no. reflections... 2224 2176 2124 2062 no(refl)/param.... 9.11 8.92 8.70 8.45 R(F)% (+)..... 13.348 13.261 13.127 12.987 wR(F**2)% (+)..... 12.880 12.856 12.806 12.758 R(F)% (-)..... 13.348 13.260 13.127 12.987 wR(F**2)% (-)..... 12.880 12.857 12.807 12.759 goodnes of fit.... 2.473 2.498 2.522 2.554 Hamilton test out of range! minimization function = 12104.5100 Structure factor least squares calculation 1 ends minimum (shift/e.s.d.) = .01 maximum (shift/e.s.d.) = 7.91 mean (shift/e.s.d.) = 1.05 sum of the squares of the (shift/e.s.d.) = 642.33 average value of B(equiv) = 2.817 number of refined parameters 244 threshold=n*sig(fo) 3 4 5 6 no. reflections... 2224 2176 2124 2062 no(refl)/param.... 9.11 8.92 8.70 8.45 R(F)% (+)..... 9.890 9.810 9.674 9.531 wR(F**2)% (+)..... 10.240 10.217 10.165 10.117 R(F)% (-)..... 9.893 9.813 9.677 9.534 wR(F**2)% (-)..... 10.240 10.218 10.165 10.118 goodnes of fit.... 1.966 1.985 2.002 2.025 Hamilton test out of range! minimization function = 7650.4510 Structure factor least squares calculation 2 ends minimum (shift/e.s.d.) = .00 maximum (shift/e.s.d.) = 2.60 mean (shift/e.s.d.) = .32 sum of the squares of the (shift/e.s.d.) = 51.65 threshold=n*sig(fo) 3 4 5 6 no. reflections... 2224 2176 2124 2062 no(refl)/param.... 9.11 8.92 8.70 8.45 R(F)% (+)..... 9.447 9.373 9.252 9.121 wR(F**2)% (+)..... 10.054 10.035 9.991 9.949 R(F)% (-)..... 9.449 9.375 9.254 9.123 wR(F**2)% (-)..... 10.055 10.035 9.991 9.949 goodnes of fit.... 1.930 1.950 1.967 1.991 Hamilton test out of range! minimization function = 7375.6950 Structure factor least squares calculation 3 ends minimum (shift/e.s.d.) = .00 maximum (shift/e.s.d.) = .50 mean (shift/e.s.d.) = .10 sum of the squares of the (shift/e.s.d.) = 4.68 threshold=n*sig(fo) 3 4 5 6 no. reflections... 2224 2176 2124 2062 no(refl)/param.... 9.11 8.92 8.70 8.45 R(F)% (+)..... 9.452 9.378 9.262 9.135 wR(F**2)% (+)..... 10.041 10.023 9.981 9.941 R(F)% (-)..... 9.453 9.380 9.264 9.137 wR(F**2)% (-)..... 10.042 10.023 9.981 9.942 goodnes of fit.... 1.928 1.947 1.965 1.990 Hamilton test out of range! minimization function = 7356.5850 Structure factor least squares calculation 4 ends ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ ------------------------------------------------------------------------------ Generation Procedure of Hydrogen Atom(s) Atom c ( 5) 1 H-atom(s) bonded to a sp3 atom h 1.00000 -.01956 .41331 1.11499 2.56969 Atom c ( 7) 1 H-atom(s) bonded to a sp3 atom h 2.00000 .02012 .69757 .97109 2.32898 Atom c ( 8) 1 H-atom(s) bonded to a sp3 atom h 3.00000 .24982 .34498 1.17765 2.40100 Atom c ( 11) 1 H-atom(s) bonded to a sp3 atom h 4.00000 .14379 .41141 .95692 2.08896 Atom c ( 12) 1 H-atom(s) bonded to a sp2 atom h 5.00000 -.14349 .45310 .79162 2.70265 Atom c ( 13) 1 H-atom(s) bonded to a sp3 atom h 6.00000 .39062 .35274 1.01596 2.40845 Atom c ( 14) 1 H-atom(s) bonded to a sp3 atom h 7.00000 -.25225 .64723 .95730 2.45592 Atom c ( 17) 1 H-atom(s) bonded to a sp3 atom h 8.00000 .20148 .58893 .91707 2.27893 Atom c ( 18) 1 H-atom(s) bonded to a sp3 atom h 9.00000 .12203 .25679 1.03061 2.89521 Atom c ( 19) 3 H-atom(s) bonded to a sp3 atom h 10.00000 .24198 .81601 .80606 3.29464 h 11.00000 .22236 .81365 .90540 3.29464 h 12.00000 .29814 .72760 .85754 3.29464 Atom c ( 21) 2 H-atom(s) bonded to a sp2 atom h 13.00000 .04704 .17436 1.15463 2.20540 h 14.00000 -.09868 .25549 1.15505 2.20540 Atom c ( 22) 1 H-atom(s) bonded to a sp2 atom h 15.00000 -.33242 .43108 .76659 2.15896 Atom c ( 23) 2 H-atom(s) bonded to a sp3 atom h 16.00000 -.28945 .72531 .79683 3.34116 h 17.00000 -.33474 .77643 .88205 3.34116 Atom c ( 24) 2 H-atom(s) bonded to a sp3 atom h 18.00000 .58119 .36262 1.13152 3.46816 h 19.00000 .49011 .45284 1.16296 3.46816 Atom c ( 25) 1 H-atom(s) bonded to a sp3 atom h 20.00000 .05604 .70108 .79068 2.45244 Atom c ( 26) 1 H-atom(s) bonded to a sp3 atom h 21.00000 -.09580 .84432 .79522 3.03645 Atom c ( 27) 3 H-atom(s) bonded to a sp3 atom h 22.00000 -.59233 .39253 .72608 4.14318 h 23.00000 -.65423 .43811 .81103 4.14318 h 24.00000 -.63487 .49954 .72883 4.14318 ------------------------------------------------------------------------------ ------------------------------------------------------------------------------ Generation Procedure of Hydrogen Atom(s) Atom c ( 5) 1 H-atom(s) bonded to a sp3 atom h 1.00000 -.01956 .41331 1.11499 2.56969 Atom c ( 7) 1 H-atom(s) bonded to a sp3 atom h 2.00000 .02012 .69757 .97109 2.32898 Atom c ( 8) 1 H-atom(s) bonded to a sp3 atom h 3.00000 .24982 .34498 1.17765 2.40100 Atom c ( 11) 1 H-atom(s) bonded to a sp3 atom h 4.00000 .14379 .41141 .95692 2.08896 Atom c ( 12) 1 H-atom(s) bonded to a sp2 atom h 5.00000 -.14349 .45310 .79162 2.70265 Atom c ( 13) 1 H-atom(s) bonded to a sp3 atom h 6.00000 .39062 .35274 1.01596 2.40845 Atom c ( 14) 1 H-atom(s) bonded to a sp3 atom h 7.00000 -.25225 .64723 .95730 2.45592 Atom c ( 17) 1 H-atom(s) bonded to a sp3 atom h 8.00000 .20148 .58893 .91707 2.27893 Atom c ( 18) 1 H-atom(s) bonded to a sp3 atom h 9.00000 .12203 .25679 1.03061 2.89521 Atom c ( 19) 3 H-atom(s) bonded to a sp3 atom h 10.00000 .24198 .81601 .80606 3.29464 h 11.00000 .22236 .81365 .90540 3.29464 h 12.00000 .29814 .72760 .85754 3.29464 Atom c ( 21) 2 H-atom(s) bonded to a sp2 atom h 13.00000 .04704 .17436 1.15463 2.20540 h 14.00000 -.09868 .25549 1.15505 2.20540 Atom c ( 22) 1 H-atom(s) bonded to a sp2 atom h 15.00000 -.33242 .43108 .76659 2.15896 Atom c ( 23) 2 H-atom(s) bonded to a sp3 atom h 16.00000 -.28945 .72531 .79683 3.34116 h 17.00000 -.33474 .77643 .88205 3.34116 Atom c ( 24) 2 H-atom(s) bonded to a sp3 atom h 18.00000 .58119 .36262 1.13152 3.46816 h 19.00000 .49011 .45284 1.16296 3.46816 Atom c ( 25) 1 H-atom(s) bonded to a sp3 atom h 20.00000 .05604 .70108 .79068 2.45244 Atom c ( 26) 1 H-atom(s) bonded to a sp3 atom h 21.00000 -.09580 .84432 .79522 3.03645 Atom c ( 27) 3 H-atom(s) bonded to a sp3 atom h 22.00000 -.59233 .39253 .72608 4.14318 h 23.00000 -.65423 .43811 .81103 4.14318 h 24.00000 -.63487 .49954 .72883 4.14318 ------------------------------------------------------------------------------ 1++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Least-Squares Routine Release 97.01 test structure: loganin ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Used directives: FullMatrix Fix H(1) H(2) H(3) H(4) H(5) H(6) H(7) H(8) H(9) H(10) 11/B[iso] Fix H(11) H(12) H(13) H(14) H(15) H(16) H(17) H(18) H(19) 11/B[iso] Fix H(20) H(21) H(22) H(23) H(24) 11/B[iso] Ride C H Cutoff 3 Damping 1.0 Cycles 3 Iso H(1) H(2) H(3) H(4) H(5) H(6) H(7) H(8) H(9) H(10) H(11) H(12) Iso H(13) H(14) H(15) H(16) H(17) H(18) H(19) H(20) H(21) H(22) Iso H(23) H(24) Structure factor least squares (Vers. 2496) Weighting scheme no. 6 Parameter(s) provided 1 p(1) p(2) p(3) p(4) 1.00000 Cycle(s) requested 3 threshold=n*sig(fo) 3 4 5 6 no. reflections... 2224 2176 2124 2062 no(refl)/param.... 9.11 8.92 8.70 8.45 R(F)% (+)..... 8.208 8.122 8.004 7.876 wR(F**2)% (+)..... 8.122 8.094 8.043 7.995 R(F)% (-)..... 8.209 8.123 8.005 7.877 wR(F**2)% (-)..... 8.123 8.094 8.044 7.996 goodnes of fit.... 1.559 1.573 1.584 1.600 Hamilton test out of range! minimization function = 4812.8090 Structure factor least squares calculation 1 ends minimum (shift/e.s.d.) = .01 maximum (shift/e.s.d.) = 3.61 mean (shift/e.s.d.) = .70 sum of the squares of the (shift/e.s.d.) = 209.48 average value of B(equiv) = 2.922 number of refined parameters 244 threshold=n*sig(fo) 3 4 5 6 no. reflections... 2224 2176 2124 2062 no(refl)/param.... 9.11 8.92 8.70 8.45 R(F)% (+)..... 7.640 7.554 7.437 7.312 wR(F**2)% (+)..... 7.674 7.648 7.600 7.554 R(F)% (-)..... 7.643 7.557 7.439 7.315 wR(F**2)% (-)..... 7.675 7.648 7.600 7.555 goodnes of fit.... 1.473 1.486 1.496 1.512 Hamilton test out of range! minimization function = 4297.3720 Structure factor least squares calculation 2 ends minimum (shift/e.s.d.) = .00 maximum (shift/e.s.d.) = .64 mean (shift/e.s.d.) = .11 sum of the squares of the (shift/e.s.d.) = 4.64 threshold=n*sig(fo) 3 4 5 6 no. reflections... 2224 2176 2124 2062 no(refl)/param.... 9.11 8.92 8.70 8.45 R(F)% (+)..... 7.608 7.524 7.410 7.288 wR(F**2)% (+)..... 7.665 7.639 7.594 7.549 R(F)% (-)..... 7.610 7.526 7.412 7.290 wR(F**2)% (-)..... 7.666 7.639 7.595 7.550 goodnes of fit.... 1.471 1.484 1.495 1.511 the ratio of wR factors = 1.0001 the test = 1.0001 at the level .500 we can reject the hypotesis (-) ! minimization function = 4286.8960 Structure factor least squares calculation 3 ends minimum (shift/e.s.d.) = .00 maximum (shift/e.s.d.) = .15 mean (shift/e.s.d.) = .02 sum of the squares of the (shift/e.s.d.) = .16 threshold=n*sig(fo) 3 4 5 6 no. reflections... 2224 2176 2124 2062 no(refl)/param.... 9.11 8.92 8.70 8.45 R(F)% (+)..... 7.605 7.521 7.407 7.285 wR(F**2)% (+)..... 7.665 7.638 7.594 7.549 R(F)% (-)..... 7.607 7.523 7.409 7.287 wR(F**2)% (-)..... 7.666 7.639 7.595 7.550 goodnes of fit.... 1.471 1.484 1.495 1.511 the ratio of wR factors = 1.0001 the test = 1.0001 at the level .500 we can reject the hypotesis (-) ! minimization function = 4286.5570 Structure factor least squares calculation 4 ends ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Final R value using 51 atoms is 7.60% Atoms informations files produced: Format File Name SHELX-93 loganin.ins SCHAKAL loganin.plt At 2:50:12 SIR97 ends ok