****************************************************************************** 2007src1054 in P-1 Fri Aug 03 2007 at 14:20:17 Sir2004 starts on: 2007src1 Used commands & directives: %data Cell 9.750 10.228 14.053 95.766 107.841 96.617 Space P -1 Content C 66 H 66 N 6 O 6 Reflections 2007src1054.hkl Format (3i4,2f8.0) Fosquare %invariants default %phase default %end Files used in Sir2004: Channel Name 5 instruction input file Sir2004.sir 6 printer output file Sir2004.lst 30 direct access structure file 2007src1.bin 31 direct access scratch file 32 sequential scratch file 34 reflection input file 2007src1054.hkl 41 scattering factors file c:\program files\sir2004\sir2004dir\Sir2004.xen ( Release : 05.98 ) Direct access structure file has been initialized ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Sir2004 : Data routine Release 01.00 2007src1054 in P-1 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Direct cell: a = 9.750 b = 10.228 c = 14.053 alpha = 95.766 beta = 107.841 gamma = 96.617 Cell volume = 1311.40 Crystal family : Triclinic Space group (centrosymmetric) : P -1 Symmetry-operations 1) x , y , z 2) -x , -y , -z Seminvariant condition : g g g P-lattice: (0,0,0) Allowed origin translations: ( 0 , 0 , 0 ) (1/2, 0 , 0 ) ( 0 ,1/2, 0 ) ( 0 , 0 ,1/2) ( 0 ,1/2,1/2) (1/2, 0 ,1/2) (1/2,1/2, 0 ) (1/2,1/2,1/2) Space Group Number = 2 Fourier limits : 0.000 < x < 0.500 0.000 < y < 1.000 0.000 < z < 1.000 Patterson limits : 0.000 < x < 0.500 0.000 < y < 1.000 0.000 < z < 1.000 X-ray scattering factors Unit cell contents and scattering factor constants Atom Symbol Number in cell Atomic number Hydrogen H 66 1 Carbon C 66 6 Nitrogen N 6 7 Oxygen O 6 8 Wave Length = 0.7107 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 0.490 20.659 0.262 7.740 0.197 49.552 0.050 2.202 0.001 C 2.310 20.844 1.020 10.208 1.589 0.569 0.865 51.651 0.216 N 12.213 0.006 3.132 9.893 2.013 28.997 1.166 0.583 -11.529 O 3.049 13.277 2.287 5.701 1.546 0.324 0.867 32.909 0.251 Number of atoms in asymmetric unit = 39.00 Equivalent number of equal atoms in primitive cell = 80 Volume per atom = 16.81 21431 input reflections 2071 Fo(s) negative set to 0.0 6002 independent input reflections 12 13 18 maximum h,k,l values 0.4304 maximum s**2 = (sin(theta)/lambda)**2 0.7622 Angstrom resolution 207 reflections are not in input data Symmetry equivalent reflections merged: Rsym(F) = 7.14% Distribution of reflections Angstrom No. of No. of No. of % of resolution expected observed missing missing up to 10.0 2 0 2 100 10.0 - 8.0 3 0 3 100 8.0 - 6.0 39 37 2 5 6.0 - 5.0 40 40 0 0 5.0 - 4.0 190 190 0 0 4.0 - 3.0 410 410 0 0 3.0 - 2.5 502 502 0 0 2.5 - 2.0 1138 1138 0 0 2.0 - 1.8 891 891 0 0 1.8 - 1.6 1310 1310 0 0 1.6 - 1.4 1734 1734 0 0 1.4 - 1.3 1156 1156 0 0 1.3 - 1.2 1491 1489 2 0 1.2 - 1.1 1951 1951 0 0 1.1 - 1.0 2312 2307 5 0 1.0 - 0.9 2949 2942 7 0 0.9 - 0.8 3901 3885 16 0 0.8 - 0.7 1619 1449 170 11 -2.325 -2.070 -1.814 -1.559 -1.303 -1.048 * * * * * * ********************************************************* * * * * 0.028* w * ** * w * * * w * * * w* * * w * * 0.106* w * ** * w * * * w * * * w * * * * w * 0.183* * w ** * * w * * * ********************************** * * w* y = s**2 * * * w * x = ln / sigfsq * 0.261* * w * ( w ) = wilson * * w* * ( * ) = calc * * w * ********************************** * w * * intercept = -0.95481 * * w * * slope = -3.29269 * 0.338* w * * b(iso) = 1.64634 * * w * * u(iso) = 0.02085 * * w * * scale = 2.59817 * * w * * scale*f(obs.)**2 = f(abs.)**2 * * w* ********************************** 0.415* x ** * * * * ********************************************************* * * * * * * ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ *** pseudotranslation section *** 2007src1054 in P-1 *** program searched for pseudo-translational symmetry *** class(es) of reflections probably affected by pseudotranslational effects: condition number of figure (m.f.s.p.) reflections of merit h = 4n 1486 1.429 1.66 14 % h = 2n 2997 1.160 1.38 15 % remarkable deviations (of displacive type) from ideal pseudotranslational symmetry are present: at s**2 = 0.0 m.f.s.p. = 21 % at s**2 = max m.f.s.p. = 7 % = 14 % test = 0.945 *** pseudotranslational symmetry will be neglected in subsequent steps *** ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ *** Final statistics section *** Distribution of with sin(th)/lambda and Resol. (Ang.) sinth/lambda 0.0656 0.1312 0.1968 0.2624 0.3280 Resol. 7.62 3.81 2.54 1.91 1.52 0.0000 0.7340 0.5930 0.8374 0.9298 number 0 44 114 229 386 sinth/lambda 0.3936 0.4592 0.5248 0.5904 0.6560 Resol. 1.27 1.09 0.95 0.85 0.76 0.7477 1.4174 1.1267 0.9245 0.9372 number 556 782 1043 1342 1506 Average values Average Numeric Graphic all data acentric centric hypercentric a. c. h. mod(E) 0.751 0.886 0.798 0.718 * E**2 1.000 1.000 1.000 1.000 E**3 1.939 1.329 1.596 1.916 * E**4 5.059 2.000 3.000 4.500 * E**5 17.371 3.323 6.383 12.260 * E**6 77.325 6.000 15.000 37.500 * mod(E**2-1) 1.097 0.736 0.968 1.145 * (E**2-1)**2 4.059 1.000 2.000 3.500 * (E**2-1)**3 64.149 2.000 8.000 26.000 * (mod(E**2-1))**3 64.929 2.415 8.691 26.903 * n(z) cumulative probability distribution z all data acentric centric hypercentric a. c. h. 0.1 0.260 0.095 0.248 0.368 * 0.2 0.384 0.181 0.345 0.463 * 0.3 0.484 0.259 0.416 0.526 * 0.4 0.552 0.330 0.473 0.574 * 0.5 0.606 0.393 0.520 0.612 * 0.6 0.648 0.451 0.561 0.643 * 0.7 0.680 0.503 0.597 0.670 * 0.8 0.708 0.551 0.629 0.694 * 0.9 0.731 0.593 0.657 0.715 * 1.0 0.749 0.632 0.683 0.733 * 1.2 0.783 0.699 0.727 0.765 * 1.4 0.811 0.753 0.763 0.791 * 1.6 0.831 0.798 0.794 0.813 * 1.8 0.845 0.835 0.820 0.832 * 2.0 0.858 0.865 0.843 0.848 * 2.2 0.871 0.889 0.862 0.863 * 2.4 0.882 0.909 0.879 0.875 * 2.6 0.893 0.926 0.893 0.886 * 2.8 0.903 0.939 0.906 0.896 * 3.0 0.911 0.950 0.917 0.905 * 3.2 0.919 0.959 0.926 0.913 * 3.4 0.926 0.967 0.935 0.920 * 3.6 0.933 0.973 0.942 0.926 * 3.8 0.937 0.978 0.949 0.932 * 4.0 0.941 0.982 0.954 0.938 * Distribution of E - number of E's .gt. limit E 0.6 0.7 0.8 0.9 1.0 1.1 1.2 1.3 1.4 1.5 number 2829 2393 2026 1736 1507 1294 1105 972 865 760 E 1.6 1.7 1.8 1.9 2.0 2.1 2.2 2.3 2.4 2.5 number 652 554 475 402 354 292 254 215 181 155 Number and percentage Number and percentage of F's > param * sigma(F) of F's > limit number percentage param number percentage limit 5388 90% 0.50 600 10% 12.18 4939 82% 1.00 1200 20% 8.04 4616 77% 1.50 1800 30% 5.95 4436 74% 2.00 2400 40% 4.57 4252 71% 2.50 3000 50% 3.64 4060 68% 3.00 3600 60% 2.95 3828 64% 3.50 4200 70% 2.39 3611 60% 4.00 4800 80% 1.82 3449 57% 4.50 5400 90% 0.84 3302 55% 5.00 6000 100% 0.00 376 largest E-values > 1.953 to phase. ( 10 printed ) code h k l E fo/sig. code h k l E fo/sig. 1 0 6 0 7.653 >6 2 0 9 0 6.084 >6 3 4 -2 8 4.642 >6 4 4 1 8 4.492 >6 5 4 -5 8 4.464 >6 6 5 3 -13 4.397 >6 7 5 6 -13 4.260 >6 8 8 1 -1 4.212 >6 9 0 12 0 4.168 >6 10 5 0 -13 4.122 >6 . . . . . . . . . 125 smallest E-values for psi0 and negative quartets ( 10 printed ) code h k l E fo/sig. code h k l E fo/sig. 5993 1 -11 -5 0.000 0.00 5994 3 12 -2 0.000 0.00 5995 1 -9 13 0.000 0.00 5996 11 -6 -5 0.000 0.00 5997 4 11 -7 0.000 0.00 5998 8 8 0 0.000 0.00 5999 8 0 8 0.000 0.00 6000 3 -11 9 0.000 0.00 6001 3 -9 9 0.000 0.00 6002 0 12 5 0.000 0.00 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Sir2004 : Invariants routine Release 01.00 2007src1054 in P-1 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ 3752 strong triplets found among 376 strongest reflections (E-min = 1.953) strengthned by 70 free vectors using P-10 formula Used 10 triplets per reflection. Gmin = 0.15 Triplets statistic distribution of g - number of |g|'s .gt. limit g 0.0 0.2 0.3 0.4 0.5 0.6 0.8 1.0 1.2 1.6 no. 3752 3733 3719 3713 3704 3699 3681 3658 3638 3601 g 2.0 2.5 3.0 3.5 4.0 5.0 6.0 7.0 9.0 10.0 no. 3559 3511 3456 3398 3351 3209 3057 2872 2481 2256 645 Psi-zero triplets found among 376 strongest reflections and the 125 weakest reflections Quartets statistic 578 negative quartets found ( 578 stored ) among 645 psi-zero relationships distribution of g - number of |g|'s .gt. limit g 0.0 0.2 0.3 0.4 0.5 0.6 0.8 1.0 1.2 1.6 no. 578 533 516 497 476 462 425 391 364 309 g 2.0 2.5 3.0 3.5 4.0 5.0 6.0 7.0 9.0 10.0 no. 273 220 180 152 133 87 51 34 15 15 number of relationships calculated stored positive estimated triplets 3602 3602 negative estimated triplets 143 143 psi-zero triplets 645 645 negative estimated quartets 276 276 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Sir2004 : Phase routine Release 01.00 2007src1054 in P-1 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Number of Pos. Est. Triplets = 3602 with G > 0.16 Number of Neg. Est. Triplets = 117 with |G| > 0.60 Number of Neg. Est. Quartets = 254 with |G| > 0.20 Number of refl. to phase = 376 Number of random phases = 125 Number of reflexions in LSQ = 4199 ( 70% of total, F's > 2.391 ) Number of atoms to locate = 39.00 Number of atoms used in LSQ = 47.00 Observations / Parameters = 22.34 Resolution & grid step (Ang) = 0.76 0.33 Fourier map grid points = 30 32 48 Threshold on R % = 25.00 Total number of trials = 300 Solve strategy: small-size structure ( 6-80 atoms in a.u. ) ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Space Group: P -1 Cell: 9.75 10.23 14.05 0.50 0.00 0.00 Cheshire cell: 4.88 5.11 7.03 Transf. Matrix 0.00 0.50 0.00 Grid: 0.07 0.07 0.05 0.00 0.00 0.50 Grid points: 15 16 22 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Number of blocks to be used: 3 Block Trials to explore Procedure 1 100 10 Tangent 2 100 20 Tangent 3 100 30 Tangent Summary for Block # 1/ 3 from trial 1 to trial 100 +++++++++++++ Figures of merit ++++++++++++ Set (Trial) eFom undetermined Set (Trial) eFom undetermined 1 ( 69) 3.313 17 2 ( 81) 3.291 23 3 ( 93) 3.272 20 4 ( 99) 3.259 4 5 ( 79) 3.254 8 6 ( 47) 3.219 16 7 ( 27) 3.171 32 8 ( 15) 3.155 23 9 ( 30) 3.146 33 10 ( 46) 3.113 18 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Extending phases for Block # 1 Set 1 Trial 69 eFom = 3.313 UnDet 5% Trial 69 End of DSR - Final FOM = 3.776 R% = 45.58 44.62 44.53 46.59 48.25 50.58 42.61 38.94 37.80 37.86 RELAX procedure ends. Translation applied: 0.0000 0.0000 0.0000 Final FOM = 3.564 RELAX fault. Set 2 Trial 81 eFom = 3.291 UnDet 6% Trial 81 End of DSR - Final FOM = 3.150 R% = 46.87 47.76 49.05 49.62 50.19 51.05 40.38 39.23 38.20 38.02 37.55 37.49 36.51 37.22 RELAX procedure ends. Translation applied: 0.4103 0.3259 0.1186 Final FOM = 4.165 improved by RELAX. R% = 43.60 43.46 38.15 37.79 37.61 37.55 27.36 26.40 25.82 25.65 25.59 25.57 25.53 25.47 25.43 25.38 25.38 25.39 Set 3 Trial 93 eFom = 3.272 UnDet 5% Trial 93 End of DSR - Final FOM = 2.951 R% = 48.62 46.85 46.14 48.60 49.82 50.84 41.98 39.90 40.47 RELAX procedure ends. Translation applied: 0.0684 0.1630 0.3321 Final FOM = 4.147 improved by RELAX. R% = 41.54 43.25 39.59 40.54 42.19 39.75 27.57 26.88 26.27 25.98 25.73 25.66 25.62 25.60 25.58 25.55 25.53 25.52 25.54 Set 4 Trial 99 eFom = 3.259 UnDet 1% Trial 99 End of DSR - Final FOM = 5.333 R% = 44.35 45.26 34.56 23.56 22.63 24.17 17.26 16.98 16.92 16.87 16.85 16.84 16.84 16.83 16.83 16.82 16.81 16.82 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ *** Final interpretation *** 2007src1054 in P-1 Assumed atomic parameters and limits for interatomic bonds and angles (interspecies and intraspecies) distances angles atomic type radius minimum maximum minimum maximum number O 0.730 0.88 1.80 80.00 155.00 8 N 0.750 0.89 1.82 80.00 155.00 7 C 0.770 0.90 1.85 80.00 155.00 6 Tentative of peak labelling in terms of atomic species group peaks possible species range of number included chemical species assigned bond angles 1 3 O O 80. - 155. 2 3 N N 80. - 155. 3 41 C C 80. - 155. range of bond distances used to build fragments group group 1 group 2 group 3 1 (0.88-1.75) (0.89-1.78) (0.90-1.80) 2 (0.90-1.80) (0.91-1.82) 3 (0.92-1.85) ------------------------------------------------------------------------------ interpeak distances up to 2.40 1) 7( 1) 1.22 2) 11( 1) 1.24 3) 19( 1) 1.21 4) 7( 1) 1.36 12( 1) 1.39 5) 7( 1) 1.51 9( 1) 1.48 10( 1) 1.33 6) 11( 1) 1.35 17( 1) 1.39 7) 1( 1) 1.22 4( 1) 1.36 5( 1) 1.51 8) 19( 1) 1.38 21( 1) 1.41 9) 5( 1) 1.48 12( 1) 1.41 13( 1) 1.40 10) 5( 1) 1.33 23( 1) 1.52 35( 1) 1.52 11) 2( 1) 1.24 6( 1) 1.35 16( 1) 1.52 12) 4( 1) 1.39 9( 1) 1.41 14( 1) 1.38 13) 9( 1) 1.40 28( 1) 1.41 14) 12( 1) 1.38 25( 1) 1.40 15) 22( 1) 1.35 26( 1) 1.50 39( 1) 1.53 16) 11( 1) 1.52 18( 1) 1.47 29( 1) 1.36 17) 6( 1) 1.39 18( 1) 1.40 30( 1) 1.40 18) 16( 1) 1.47 17( 1) 1.40 32( 1) 1.40 19) 3( 1) 1.21 8( 1) 1.38 22( 1) 1.52 20) 29( 1) 1.50 21) 8( 1) 1.41 24( 1) 1.41 27( 1) 1.37 22) 15( 1) 1.35 19( 1) 1.52 24( 1) 1.48 23) 10( 1) 1.52 42( 1) 1.17 24) 21( 1) 1.41 22( 1) 1.48 36( 1) 1.39 25) 14( 1) 1.40 28( 1) 1.40 26) 15( 1) 1.50 44( 1) 1.73 27) 21( 1) 1.37 31( 1) 1.40 28) 13( 1) 1.41 25( 1) 1.40 29) 16( 1) 1.36 20( 1) 1.50 38( 1) 1.51 30) 17( 1) 1.40 37( 1) 1.40 31) 27( 1) 1.40 33( 1) 1.39 32) 18( 1) 1.40 34( 1) 1.41 33) 31( 1) 1.39 36( 1) 1.41 40( 1) 1.05 34) 32( 1) 1.41 37( 1) 1.38 43( 1) 1.38 35) 10( 1) 1.52 36) 24( 1) 1.39 33( 1) 1.41 37) 30( 1) 1.40 34( 1) 1.38 38) 29( 1) 1.51 39) 15( 1) 1.53 47( 1) 1.12 40) 33( 1) 1.05 42) 23( 1) 1.17 43) 34( 1) 1.38 45( 1) 1.84 46( 1) 1.76 44) 26( 1) 1.73 45) 43( 1) 1.84 46( -1) 1.04 46( 1) 1.64 46) 43( 1) 1.76 45( -1) 1.04 45( 1) 1.64 46( -1) 1.06 47) 39( 1) 1.12 accepted distances in this interpretation 1) 7( 1) 1.22 2) 11( 1) 1.24 3) 19( 1) 1.21 4) 7( 1) 1.36 12( 1) 1.39 5) 7( 1) 1.51 9( 1) 1.48 10( 1) 1.33 6) 11( 1) 1.35 17( 1) 1.39 7) 1( 1) 1.22 4( 1) 1.36 5( 1) 1.51 8) 19( 1) 1.38 21( 1) 1.41 9) 5( 1) 1.48 12( 1) 1.41 13( 1) 1.40 10) 5( 1) 1.33 23( 1) 1.52 35( 1) 1.52 11) 2( 1) 1.24 6( 1) 1.35 16( 1) 1.52 12) 4( 1) 1.39 9( 1) 1.41 14( 1) 1.38 13) 9( 1) 1.40 28( 1) 1.41 14) 12( 1) 1.38 25( 1) 1.40 15) 22( 1) 1.35 26( 1) 1.50 39( 1) 1.53 16) 11( 1) 1.52 18( 1) 1.47 29( 1) 1.36 17) 6( 1) 1.39 18( 1) 1.40 30( 1) 1.40 18) 16( 1) 1.47 17( 1) 1.40 32( 1) 1.40 19) 3( 1) 1.21 8( 1) 1.38 22( 1) 1.52 20) 29( 1) 1.50 21) 8( 1) 1.41 24( 1) 1.41 27( 1) 1.37 22) 15( 1) 1.35 19( 1) 1.52 24( 1) 1.48 23) 10( 1) 1.52 42( 1) 1.17 24) 21( 1) 1.41 22( 1) 1.48 36( 1) 1.39 25) 14( 1) 1.40 28( 1) 1.40 26) 15( 1) 1.50 44( 1) 1.73 27) 21( 1) 1.37 31( 1) 1.40 28) 13( 1) 1.41 25( 1) 1.40 29) 16( 1) 1.36 20( 1) 1.50 38( 1) 1.51 30) 17( 1) 1.40 37( 1) 1.40 31) 27( 1) 1.40 33( 1) 1.39 32) 18( 1) 1.40 34( 1) 1.41 33) 31( 1) 1.39 36( 1) 1.41 40( 1) 1.05 34) 32( 1) 1.41 37( 1) 1.38 43( 1) 1.38 35) 10( 1) 1.52 36) 24( 1) 1.39 33( 1) 1.41 37) 30( 1) 1.40 34( 1) 1.38 38) 29( 1) 1.51 39) 15( 1) 1.53 47( 1) 1.12 40) 33( 1) 1.05 42) 23( 1) 1.17 43) 34( 1) 1.38 45( 1) 1.84 46( 1) 1.76 44) 26( 1) 1.73 45) 43( 1) 1.84 46( -1) 1.04 46( 1) 1.64 46) 43( 1) 1.76 45( -1) 1.04 45( 1) 1.64 46( -1) 1.06 47) 39( 1) 1.12 bond angles in this interpretation ( 7( 1) - 4 - 12( 1)) 112.0 ( 7( 1) - 5 - 9( 1)) 104.5 ( 7( 1) - 5 - 10( 1)) 126.1 ( 9( 1) - 5 - 10( 1)) 129.4 ( 11( 1) - 6 - 17( 1)) 112.0 ( 1( 1) - 7 - 4( 1)) 124.7 ( 1( 1) - 7 - 5( 1)) 128.4 ( 4( 1) - 7 - 5( 1)) 106.8 ( 19( 1) - 8 - 21( 1)) 112.3 ( 5( 1) - 9 - 12( 1)) 107.4 ( 5( 1) - 9 - 13( 1)) 134.5 ( 12( 1) - 9 - 13( 1)) 118.1 ( 5( 1) - 10 - 23( 1)) 123.5 ( 5( 1) - 10 - 35( 1)) 122.3 ( 23( 1) - 10 - 35( 1)) 114.2 ( 2( 1) - 11 - 6( 1)) 124.6 ( 2( 1) - 11 - 16( 1)) 128.9 ( 6( 1) - 11 - 16( 1)) 106.5 ( 4( 1) - 12 - 9( 1)) 109.2 ( 4( 1) - 12 - 14( 1)) 127.3 ( 9( 1) - 12 - 14( 1)) 123.5 ( 9( 1) - 13 - 28( 1)) 119.0 ( 12( 1) - 14 - 25( 1)) 117.8 ( 22( 1) - 15 - 26( 1)) 124.4 ( 22( 1) - 15 - 39( 1)) 121.4 ( 26( 1) - 15 - 39( 1)) 114.2 ( 11( 1) - 16 - 18( 1)) 104.8 ( 11( 1) - 16 - 29( 1)) 124.3 ( 18( 1) - 16 - 29( 1)) 130.8 ( 6( 1) - 17 - 18( 1)) 109.8 ( 6( 1) - 17 - 30( 1)) 127.3 ( 18( 1) - 17 - 30( 1)) 122.9 ( 16( 1) - 18 - 17( 1)) 106.9 ( 16( 1) - 18 - 32( 1)) 134.0 ( 17( 1) - 18 - 32( 1)) 119.1 ( 3( 1) - 19 - 8( 1)) 124.0 ( 3( 1) - 19 - 22( 1)) 130.8 ( 8( 1) - 19 - 22( 1)) 105.2 ( 8( 1) - 21 - 24( 1)) 109.4 ( 8( 1) - 21 - 27( 1)) 127.5 ( 24( 1) - 21 - 27( 1)) 123.1 ( 15( 1) - 22 - 19( 1)) 123.7 ( 15( 1) - 22 - 24( 1)) 129.8 ( 19( 1) - 22 - 24( 1)) 106.4 ( 10( 1) - 23 - 42( 1)) 106.9 ( 21( 1) - 24 - 22( 1)) 106.6 ( 21( 1) - 24 - 36( 1)) 118.7 ( 22( 1) - 24 - 36( 1)) 134.7 ( 14( 1) - 25 - 28( 1)) 120.3 ( 15( 1) - 26 - 44( 1)) 72.6 ( 21( 1) - 27 - 31( 1)) 117.9 ( 13( 1) - 28 - 25( 1)) 121.2 ( 16( 1) - 29 - 20( 1)) 124.1 ( 16( 1) - 29 - 38( 1)) 122.3 ( 20( 1) - 29 - 38( 1)) 113.7 ( 17( 1) - 30 - 37( 1)) 117.7 ( 27( 1) - 31 - 33( 1)) 120.4 ( 18( 1) - 32 - 34( 1)) 117.9 ( 31( 1) - 33 - 36( 1)) 121.3 ( 31( 1) - 33 - 40( 1)) 121.2 ( 36( 1) - 33 - 40( 1)) 116.8 ( 32( 1) - 34 - 37( 1)) 122.3 ( 32( 1) - 34 - 43( 1)) 142.9 ( 37( 1) - 34 - 43( 1)) 94.6 ( 24( 1) - 36 - 33( 1)) 118.7 ( 30( 1) - 37 - 34( 1)) 120.1 ( 15( 1) - 39 - 47( 1)) 110.2 ( 34( 1) - 43 - 45( 1)) 72.4 ( 34( 1) - 43 - 46( 1)) 124.6 ( 45( 1) - 43 - 46( 1)) 54.0 ( 43( 1) - 45 - 46( -1)) 79.2 ( 43( 1) - 45 - 46( 1)) 60.5 ( 46( -1) - 45 - 46( 1)) 39.1 ( 46( 1) - 45 - 46( -1)) 39.1 ( 43( 1) - 46 - 45( -1)) 121.7 ( 43( 1) - 46 - 45( 1)) 65.4 ( 43( 1) - 46 - 46( -1)) 82.7 ( 45( -1) - 46 - 45( 1)) 140.9 ( 45( -1) - 46 - 46( -1)) 102.6 ( 45( 1) - 46 - 45( -1)) 140.9 ( 45( 1) - 46 - 46( -1)) 38.3 ------------------------------------------------------------------------------ --------------------- overall plot of the structure ------------------------- ------------ projection on l.s.q. plane ---- scale : 1.94 cms/a ------------ 2 6 * * * * * 11 30 * * * 17 * * * * * 37 * * 16 * 18 * * 20 * * * * * * 29 34 * * * 32 * * 4345 1 * * 4 * * * * * * 38 7 14 * * * 12 * * * * * 25 * * 5 * 9 * * 47 * * * * 23 * *39* * 10 * *42 28 * * * 13 40 41 * * * * 36 * * * 33 15 * 35 * * 44 * * * 26 * * 24 * 22 * * 31 * * * * * 21 * * * 27 19 * * * * * 8 3 --------------------- partial plot for fragment 1 ------------------------- ------------ projection on l.s.q. plane ---- scale : 2.50 cms/a ------------ 1 * 4 * * 7 * * * * 12 * * 14 * * * 5 * * * 23 * * 25 * * * 9 42 * * 10 * * * * * 28 13 * * * 35 ---------------------------------------------------------------------------- fragment number 1 , 13 peaks included peak 1 4 5 7 9 10 12 13 14 23 25 28 35 linked to 7 7 7 1 5 5 4 9 12 10 14 13 10 12 9 4 12 23 9 28 25 42 28 25 10 5 13 35 14 peak 42 linked to 23 --------------------- partial plot for fragment 2 ------------------------- ------------ projection on l.s.q. plane ---- scale : 2.35 cms/a ------------ 6 * 30 * * 2 * * * * * * 17 * 11 * 37 * * * * * 16 * * 18 * 34 * * * * * * 43 32 * * * 46 * * 29 * * 38 ---------------------------------------------------------------------------- fragment number 2 , 13 peaks included peak 2 6 11 16 17 18 20 29 30 32 34 37 38 linked to 11 11 2 11 6 16 29 16 17 18 32 30 29 17 6 18 18 17 20 37 34 37 34 16 29 30 32 38 43 peak 43 46 linked to 34 43 46 --------------------- partial plot for fragment 3 ------------------------- ------------ projection on l.s.q. plane ---- scale : 2.50 cms/a ------------ 3 8 * * * * * * 19 27 * * 21 * * * * * * 31 * * 22 * 24 * * * 26 * * * * 15 33 * * 36 * * * 40 * 39 ** 47 ---------------------------------------------------------------------------- fragment number 3 , 13 peaks included peak 3 8 15 19 21 22 24 26 27 31 33 36 39 linked to 19 19 22 3 8 15 21 15 21 27 31 24 15 21 26 8 24 19 22 31 33 36 33 47 39 22 27 24 36 40 peak 40 47 linked to 33 39 ------------------------------------------------------------------------------ ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ *** Output section *** 2007src1054 in P-1 Final residual value = 16.81% Serial Atom Label Height*10 x y z Occ. B[iso] Frag 1) O O1 134 1.046 -0.001 1.378 1.000 0.82 0 2) O O2 130 1.314 0.311 1.706 1.000 0.91 0 3) N N1 122 0.213 0.314 0.946 1.000 0.98 0 4) O O3 117 0.830 0.007 1.410 1.000 0.98 0 5) C C1 107 0.816 0.004 1.242 1.000 0.98 0 6) C C2 103 1.095 0.315 1.735 1.000 0.98 0 7) C C3 102 0.915 0.002 1.349 1.000 0.68 0 8) N N2 101 0.432 0.318 0.918 1.000 0.98 0 9) N N3 100 0.670 0.008 1.253 1.000 0.98 0 10) C C4 98 0.856 0.001 1.160 1.000 0.82 0 11) C C5 97 1.180 0.313 1.676 1.000 0.81 0 12) C C6 95 0.685 0.009 1.356 1.000 0.73 0 13) C C7 92 0.530 0.007 1.185 1.000 0.97 0 14) C C8 91 0.570 0.010 1.393 1.000 0.94 0 15) C C9 90 0.404 0.350 1.168 1.000 0.76 0 16) C C10 90 1.081 0.316 1.569 1.000 0.72 0 17) C C11 88 0.951 0.319 1.681 1.000 0.86 0 18) C C12 88 0.936 0.321 1.579 1.000 0.69 0 19) C C13 87 0.344 0.325 0.978 1.000 0.74 0 20) C C14 85 1.280 0.303 1.489 1.000 1.29 0 21) C C15 85 0.581 0.334 0.975 1.000 0.75 0 22) C C16 85 0.448 0.343 1.086 1.000 0.62 0 23) C C17 83 1.010 -0.011 1.160 1.000 1.29 0 24) C C18 83 0.597 0.348 1.079 1.000 0.67 0 25) C C19 82 0.431 0.010 1.325 1.000 1.40 0 26) C C20 82 0.248 0.342 1.165 1.000 1.57 0 27) C C21 80 0.697 0.335 0.939 1.000 0.89 0 28) C C22 78 0.411 0.006 1.222 1.000 1.01 0 29) C C23 76 1.127 0.318 1.487 1.000 0.88 0 30) C C24 75 0.833 0.319 1.718 1.000 1.25 0 31) C C25 75 0.837 0.355 1.010 1.000 1.00 0 32) C C26 74 0.798 0.324 1.510 1.000 1.16 0 33) C C27 73 0.857 0.371 1.113 1.000 1.27 0 34) C C28 71 0.679 0.324 1.548 1.000 1.47 0 35) C C29 71 0.750 0.008 1.056 1.000 1.01 0 36) C C30 66 0.737 0.368 1.149 1.000 1.06 0 37) C C31 66 0.696 0.323 1.649 1.000 1.43 0 38) C C32 63 1.028 0.336 1.385 1.000 1.47 0 39) C C33 62 0.514 0.368 1.275 1.000 1.35 0 40) Q Q1 16 0.958 0.369 1.166 1.000 0.97 0 41) Q Q2 16 0.473 0.634 1.272 1.000 0.97 0 42) Q Q3 13 1.006 -0.119 1.120 1.000 0.97 0 43) Q Q4 12 0.533 0.337 1.521 1.000 0.97 0 44) C C34 11 0.281 0.181 1.144 1.000 0.98 0 45) Q Q5 11 0.636 0.501 1.524 1.000 0.97 0 46) Q Q6 11 0.467 0.490 1.523 1.000 0.97 0 47) Q Q7 11 0.586 0.466 1.291 1.000 0.97 0 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Final R value is 16.81% (Block 1, Set 4, # of LSQ Refinement 6)