****************************************************************************** Test in Pna2(1) Thu Jun 28 2007 at 17:17:40 Sir2004 starts on: test Used commands & directives: %data Cell 15.408 12.992 9.380 90.000 90.000 90.000 Space P n a 21 Content C 76 H 112 N 4 O 8 S 4 Cl 4 Reflections test.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 test.bin 31 direct access scratch file 32 sequential scratch file 34 reflection input file test.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 Test in Pna2(1) ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Direct cell: a = 15.408 b = 12.992 c = 9.380 alpha = 90.000 beta = 90.000 gamma = 90.000 Cell volume = 1877.70 Crystal family : Orthorhombic Space group (noncentrosymmetric) : P n a 21 Symmetry-operations 1) x , y , z 2) -x , -y , z+1/2 3) -x+1/2, y+1/2, z+1/2 4) x+1/2, -y+1/2, z Seminvariant condition : g g 0 P-lattice: (0,0,0) Allowed origin translations: ( 0 , 0 , z ) ( 0 ,1/2, z ) (1/2, 0 , z ) (1/2,1/2, z ) Space Group Number = 33 Fourier limits : 0.000 < x < 0.500 0.000 < y < 0.500 0.000 < z < 1.000 Patterson limits : 0.000 < x < 0.500 0.000 < y < 0.500 0.000 < z < 0.500 X-ray scattering factors Unit cell contents and scattering factor constants Atom Symbol Number in cell Atomic number Hydrogen H 112 1 Carbon C 76 6 Nitrogen N 4 7 Oxygen O 8 8 Sulphur S 4 16 Chlorine Cl 4 17 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 S 6.905 1.468 5.203 22.215 1.438 0.254 1.586 56.172 0.867 Cl 11.460 0.010 7.196 1.166 6.256 18.519 1.646 47.778 -9.557 Number of atoms in asymmetric unit = 24.00 Equivalent number of equal atoms in primitive cell = 56 Volume per atom = 19.56 Syst. absent : 0 0 3 Fobs = 0.000 Sigma(Fobs) = 0.230 Syst. absent : 0 0 -3 Fobs = 0.000 Sigma(Fobs) = 0.210 Syst. absent : 0 0 5 Fobs = 0.590 Sigma(Fobs) = 0.230 Syst. absent : 0 0 -5 Fobs = 0.500 Sigma(Fobs) = 0.440 Syst. absent : 0 0 -7 Fobs = 1.960 Sigma(Fobs) = 0.950 Syst. absent : 0 0 7 Fobs = 1.500 Sigma(Fobs) = 0.480 Syst. absent : 0 0 -9 Fobs = 0.130 Sigma(Fobs) = 0.430 Syst. absent : 0 0 -11 Fobs = 0.000 Sigma(Fobs) = 0.490 Syst. absent : 0 1 -2 Fobs = 2.140 Sigma(Fobs) = 0.320 Syst. absent : 0 1 2 Fobs = 2.190 Sigma(Fobs) = 0.370 .... and so on Space Group Determination Routine Crystal System determination by geometrical analysis of the cell: ORTHORHOMBIC Total number of independent reflections : 11136 Total number of reflections considered: 11136 Total number of reflections greater than 3s: 11136 < fo >Total : 79.17677 < fo/sfo >Total : 18.02231 SYSTEMATIC ABSENCE EXCEPTIONS Note: Symbol # means not equal Refl. Total Condition N.Refl. N.(>3s) Sym. Op. Type Number 0 0 l 15 l#2n 8 8 0.6 0.4 _ _ 21 l#4n 11 11 91.5 1.6 ______ 0 k 0 21 k#2n 11 11 0.6 0.3 _ 21 _ k#4n 17 17 29.3 1.6 ______ h 0 0 34 h#2n 21 21 1.3 0.7 21 _ _ h#4n 27 27 4.1 1.4 ______ 0 k l 402 k#2n 204 204 72.2 2.4 ______ l#2n 200 200 73.4 2.3 ______ k#2n,l#2n 300 300 49.2 1.7 ______ k+l#2n 196 196 0.6 0.3 n _ _ k#2n,l#2n,k+l#4n 350 350 59.4 2.1 ______ h 0 l 538 h#2n 255 255 1.3 0.8 _ a _ l#2n 277 277 61.5 2.3 ______ h#2n,l#2n 409 409 42.0 1.8 ______ h+l#2n 286 286 59.4 2.2 ______ h#2n,l#2n,h+l#4n 472 472 44.6 2.0 ______ h k 0 780 h#2n 396 396 59.3 3.3 ______ k#2n 390 390 75.4 3.2 ______ h#2n,k#2n 589 589 64.5 3.2 ______ h+k#2n 392 392 59.1 3.2 ______ h#2n,k#2n,h+k#4n 684 684 71.5 3.3 ______ h k l 11136 h+k#2n 5595 5595 33.4 2.9 ______ k+l#2n 5585 5585 40.0 3.0 ______ h+l#2n 5548 5548 39.1 3.0 ______ h+k+l#2n 5600 5600 36.9 2.9 ______ (h+k,k+l,h+l)#2n 8364 8364 37.5 3.0 ______ Extinction Group Fig.Mer P n _ _ 0.135 P _ 21 21 0.066 P _ 21 _ 0.043 P 21 21 21 0.025 P _ _ 21 0.023 P n c _ 0.018 P 21 21 _ 0.017 P n a _ 0.016 P _ _ _ 0.015 P n _ b 0.015 P b _ _ 0.013 P 21 _ 21 0.009 P c _ _ 0.007 P n n _ 0.007 P 21 _ _ 0.006 P n _ n 0.006 P n _ a 0.006 P _ _ b 0.005 P _ c _ 0.003 P b c _ 0.003 Systematically absent reflections analisys Number and percentage of F's > param * sigma(F) Number percentage param 337 75% 0.00 296 66% 0.50 248 55% 1.00 201 45% 1.50 152 34% 2.00 115 25% 2.50 84 19% 3.00 59 13% 3.50 47 10% 4.00 38 8% 4.50 29 6% 5.00 11136 input reflections 215 Fo(s) negative set to 0.0 2550 independent input reflections 451 systematically absent reflections rejected 20 17 12 maximum h,k,l values 0.4569 maximum s**2 = (sin(theta)/lambda)**2 0.7397 Angstrom resolution 25 reflections are not in input data Symmetry equivalent reflections merged: Rsym(F) = 3.63% Distribution of reflections Angstrom No. of No. of No. of % of resolution expected observed missing missing up to 10.0 0 0 0 0 10.0 - 8.0 1 0 1 100 8.0 - 6.0 14 12 2 14 6.0 - 5.0 25 25 0 0 5.0 - 4.0 50 49 1 2 4.0 - 3.0 147 144 3 2 3.0 - 2.5 205 205 0 0 2.5 - 2.0 458 458 0 0 2.0 - 1.8 387 387 0 0 1.8 - 1.6 527 527 0 0 1.6 - 1.4 973 973 0 0 1.4 - 1.3 619 619 0 0 1.3 - 1.2 738 738 0 0 1.2 - 1.1 960 960 0 0 1.1 - 1.0 1199 1198 1 0 1.0 - 0.9 1383 1381 2 0 0.9 - 0.8 1785 1784 1 0 0.8 - 0.7 1239 1225 14 1 -4.270 -3.992 -3.714 -3.435 -3.157 -2.879 * * * * * * ********************************************************* * * * * 0.036* w * ** * w * * * w * * * w* * * w * * 0.117* w* ** * x * * * w * * * w * * * w * 0.198* * w ** * * w * * x ********************************** * w * * y = s**2 * * w * * x = ln / sigfsq * 0.279* w * * ( w ) = wilson * * w * * ( * ) = calc * * w * ********************************** * w * * intercept = -2.75608 * * w* * slope = -3.42689 * 0.361* w* * b(iso) = 1.71344 * * x * u(iso) = 0.02170 * * *w * scale = 15.73810 * * *w * scale*f(obs.)**2 = f(abs.)**2 * * *w ********************************** 0.442* *w ** * * * * ********************************************************* * * * * * * ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ *** pseudotranslation section *** Test in Pna2(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 = 2n 4642 1.366 2.16 36 % h+2k+2l = 4n 2394 1.657 2.15 22 % *** pseudotranslational symmetry will be neglected in subsequent steps *** ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ *** Final statistics section *** Distribution of with sin(th)/lambda and Resol. (Ang.) sinth/lambda 0.0676 0.1352 0.2028 0.2704 0.3380 Resol. 7.40 3.70 2.47 1.85 1.48 0.0000 1.0759 0.8629 0.9686 0.9351 number 0 59 161 321 571 sinth/lambda 0.4056 0.4732 0.5408 0.6084 0.6760 Resol. 1.23 1.06 0.92 0.82 0.74 1.0088 1.1912 0.9319 0.9316 1.0333 number 848 1163 1595 2049 2511 Average values Average Numeric Graphic all data acentric centric hypercentric a. c. h. mod(E) 0.851 0.886 0.798 0.718 * E**2 1.000 1.000 1.000 1.000 E**3 1.492 1.329 1.596 1.916 * E**4 2.667 2.000 3.000 4.500 * E**5 5.477 3.323 6.383 12.260 * E**6 12.500 6.000 15.000 37.500 * mod(E**2-1) 0.855 0.736 0.968 1.145 * (E**2-1)**2 1.667 1.000 2.000 3.500 * (E**2-1)**3 6.499 2.000 8.000 26.000 * (mod(E**2-1))**3 7.009 2.415 8.691 26.903 * n(z) cumulative probability distribution z all data acentric centric hypercentric a. c. h. 0.1 0.113 0.095 0.248 0.368 * 0.2 0.234 0.181 0.345 0.463 * 0.3 0.329 0.259 0.416 0.526 * 0.4 0.407 0.330 0.473 0.574 * 0.5 0.469 0.393 0.520 0.612 * 0.6 0.527 0.451 0.561 0.643 * 0.7 0.576 0.503 0.597 0.670 * 0.8 0.613 0.551 0.629 0.694 * 0.9 0.649 0.593 0.657 0.715 * 1.0 0.676 0.632 0.683 0.733 * 1.2 0.730 0.699 0.727 0.765 * 1.4 0.782 0.753 0.763 0.791 * 1.6 0.816 0.798 0.794 0.813 * 1.8 0.844 0.835 0.820 0.832 * 2.0 0.866 0.865 0.843 0.848 * 2.2 0.884 0.889 0.862 0.863 * 2.4 0.899 0.909 0.879 0.875 * 2.6 0.912 0.926 0.893 0.886 * 2.8 0.922 0.939 0.906 0.896 * 3.0 0.929 0.950 0.917 0.905 * 3.2 0.937 0.959 0.926 0.913 * 3.4 0.945 0.967 0.935 0.920 * 3.6 0.951 0.973 0.942 0.926 * 3.8 0.958 0.978 0.949 0.932 * 4.0 0.964 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 1587 1377 1157 987 841 698 554 455 375 305 E 1.6 1.7 1.8 1.9 2.0 2.1 2.2 2.3 2.4 2.5 number 243 202 165 133 100 79 64 45 35 32 Number and percentage Number and percentage of F's > param * sigma(F) of F's > limit number percentage param number percentage limit 2538 100% 0.50 255 10% 8.52 2521 99% 1.00 510 20% 5.82 2502 98% 1.50 765 30% 4.66 2473 97% 2.00 1020 40% 3.75 2435 95% 2.50 1275 50% 3.11 2404 94% 3.00 1530 60% 2.49 2375 93% 3.50 1785 70% 2.02 2336 92% 4.00 2040 80% 1.66 2289 90% 4.50 2295 90% 1.21 2254 88% 5.00 2550 100% 0.00 258 largest E-values > 1.573 to phase. ( 10 printed ) code h k l E fo/sig. code h k l E fo/sig. 1 18 4 3 3.585 >6 2 18 7 0 3.386 >6 3 10 13 0 3.282 >6 4 10 9 0 3.273 >6 5 8 2 0 3.079 >6 6 0 15 3 3.043 >6 7 10 6 3 3.008 >6 8 16 10 1 2.957 >6 9 0 15 5 2.953 >6 10 18 4 5 2.926 >6 . . . . . . . . . 86 smallest E-values for psi0 and negative quartets ( 10 printed ) code h k l E fo/sig. code h k l E fo/sig. 2541 5 11 9 0.000 0.00 2542 17 6 5 0.000 0.00 2543 2 7 11 0.000 0.00 2544 5 1 11 0.000 0.00 2545 1 8 8 0.000 0.00 2546 15 1 4 0.000 0.00 2547 16 0 6 0.000 0.00 2548 18 6 0 0.000 0.00 2549 11 11 0 0.000 0.00 2550 0 0 12 0.000 0.00 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Sir2004 : Invariants routine Release 01.00 Test in Pna2(1) ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ 5200 strong triplets found among 258 strongest reflections (E-min = 1.573) strengthned by 44 free vectors using P-10 formula Used 19 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 1.4 no. 5200 5171 5157 5142 5125 5114 5083 5057 5033 5002 g 1.6 2.0 2.5 3.0 3.5 4.0 6.0 8.0 10.0 15.0 no. 4968 4917 4852 4760 4682 4591 4192 3727 3226 1927 2017 Psi-zero triplets found among 258 strongest reflections and the 86 weakest reflections Quartets statistic 6189 negative quartets found ( 4000 stored ) among 2017 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 1.4 no. 4000 3540 3220 2823 2453 2122 1490 1091 812 613 g 1.6 2.0 2.5 3.0 3.5 4.0 6.0 8.0 10.0 15.0 no. 481 295 167 93 66 41 10 3 1 0 number of relationships calculated stored positive estimated triplets 4924 4924 negative estimated triplets 249 249 psi-zero triplets 2017 2017 negative estimated quartets 3226 3226 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Sir2004 : Phase routine Release 01.00 Test in Pna2(1) ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Number of Pos. Est. Triplets = 4924 with G > 0.15 Number of Neg. Est. Triplets = 222 with |G| > 0.60 Number of Neg. Est. Quartets = 1000 with |G| > 0.20 Number of refl. to phase = 258 Number of random phases = 64 Number of reflexions in LSQ = 1785 ( 70% of total, F's > 2.021 ) Number of atoms to locate = 24.00 Number of atoms used in LSQ = 29.00 Observations / Parameters = 15.39 Resolution & grid step (Ang) = 0.74 0.33 Fourier map grid points = 48 40 30 Threshold on R % = 25.00 Total number of trials = 300 Solve strategy: small-size structure ( 6-80 atoms in a.u. ) ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Space Group: P n a 21 Cell: 15.41 12.99 9.38 0.50 0.00 0.00 Cheshire cell: 7.70 6.50 0.00 Transf. Matrix 0.00 0.50 0.00 Grid: 0.04 0.05 0.00 0.00 0.00 0.00 Grid points: 24 20 1 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ 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 ( 35) 2.951 48 2 ( 4) 2.838 48 3 ( 51) 2.823 48 4 ( 97) 2.821 48 5 ( 90) 2.821 48 6 ( 37) 2.817 48 7 ( 93) 2.817 48 8 ( 2) 2.816 48 9 ( 12) 2.816 48 10 ( 54) 2.815 48 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Extending phases for Block # 1 Set 1 Trial 35 eFom = 2.951 UnDet 19% Trial 35 End of DSR - Final FOM = 2.631 R% = 76.81 47.62 43.68 39.79 40.35 40.38 34.94 35.37 34.96 34.18 33.93 34.15 RELAX procedure ends. Translation applied: 0.1082 0.4362 0.0000 Final FOM = 1.727 RELAX fault. Set 2 Trial 4 eFom = 2.838 UnDet 19% Trial 4 End of DSR - Final FOM = 3.213 R% = 66.82 52.70 27.52 19.63 20.62 19.79 15.91 15.35 15.07 14.80 14.54 14.30 14.04 13.46 13.25 12.77 12.29 12.54 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ *** Final interpretation *** Test in Pna2(1) Assumed atomic parameters and limits for interatomic bonds and angles (interspecies and intraspecies) distances angles atomic type radius minimum maximum minimum maximum number Cl 0.990 1.03 2.41 80.00 155.00 17 S 1.020 1.05 2.45 80.00 155.00 16 O 0.730 0.88 2.10 80.00 155.00 8 N 0.750 0.89 2.12 80.00 155.00 7 C 0.770 0.90 2.15 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 1 Cl Cl 80. - 155. 2 1 S S 80. - 155. 3 2 O O 80. - 155. 4 1 N N 80. - 155. 5 24 C C 80. - 155. range of bond distances used to build fragments group group 1 group 2 group 3 group 4 1 (1.19-2.38) (1.21-2.41) (1.03-2.06) (1.04-2.09) 2 (1.22-2.45) (1.05-2.10) (1.06-2.12) 3 (0.88-1.75) (0.89-1.78) 4 (0.90-1.80) group group 5 1 (1.06-2.11) 2 (1.07-2.15) 3 (0.90-1.80) 4 (0.91-1.82) 5 (0.92-1.85) ------------------------------------------------------------------------------ interpeak distances up to 2.45 1) 3( 1) 1.63 4( 1) 1.41 5( 1) 1.44 6( 1) 1.76 2) 19( 1) 1.84 3) 1( 1) 1.63 8( 1) 1.46 15( 1) 1.54 4) 1( 1) 1.41 5) 1( 1) 1.44 6) 1( 1) 1.76 11( 1) 1.37 13( 1) 1.43 7) 12( 1) 1.50 8) 3( 1) 1.46 16( 1) 1.52 24( 1) 1.37 9) 19( 1) 1.48 10) 12( 1) 1.35 13( 1) 1.44 11) 6( 1) 1.37 18( 1) 1.42 12) 7( 1) 1.50 10( 1) 1.35 18( 1) 1.43 13) 6( 1) 1.43 10( 1) 1.44 14) 17( 1) 1.57 21( 1) 1.56 25( 2) 1.72 28( 1) 1.13 15) 3( 1) 1.54 23( 1) 1.82 26( 1) 1.62 16) 8( 1) 1.52 20( 1) 1.55 22( 1) 1.60 17) 14( 1) 1.57 20( 1) 1.52 18) 11( 1) 1.42 12( 1) 1.43 19) 2( 1) 1.84 9( 1) 1.48 20) 16( 1) 1.55 17( 1) 1.52 21) 14( 1) 1.56 22( 1) 1.48 22) 16( 1) 1.60 21( 1) 1.48 23) 15( 1) 1.82 24( 1) 1.41 24) 8( 1) 1.37 23( 1) 1.41 25) 14( 2) 1.72 27( 2) 1.84 28( 2) 1.77 26) 15( 1) 1.62 29( 1) 1.33 27) 25( 2) 1.84 28( 1) 1.32 28) 14( 1) 1.13 25( 2) 1.77 27( 1) 1.32 29) 26( 1) 1.33 accepted distances in this interpretation 1) 3( 1) 1.63 4( 1) 1.41 5( 1) 1.44 6( 1) 1.76 2) 19( 1) 1.84 3) 1( 1) 1.63 8( 1) 1.46 15( 1) 1.54 4) 1( 1) 1.41 5) 1( 1) 1.44 6) 1( 1) 1.76 11( 1) 1.37 13( 1) 1.43 7) 12( 1) 1.50 8) 3( 1) 1.46 16( 1) 1.52 24( 1) 1.37 9) 19( 1) 1.48 10) 12( 1) 1.35 13( 1) 1.44 11) 6( 1) 1.37 18( 1) 1.42 12) 7( 1) 1.50 10( 1) 1.35 18( 1) 1.43 13) 6( 1) 1.43 10( 1) 1.44 14) 17( 1) 1.57 21( 1) 1.56 25( 2) 1.72 28( 1) 1.13 15) 3( 1) 1.54 23( 1) 1.82 26( 1) 1.62 16) 8( 1) 1.52 20( 1) 1.55 22( 1) 1.60 17) 14( 1) 1.57 20( 1) 1.52 18) 11( 1) 1.42 12( 1) 1.43 19) 2( 1) 1.84 9( 1) 1.48 20) 16( 1) 1.55 17( 1) 1.52 21) 14( 1) 1.56 22( 1) 1.48 22) 16( 1) 1.60 21( 1) 1.48 23) 15( 1) 1.82 24( 1) 1.41 24) 8( 1) 1.37 23( 1) 1.41 25) 14( 2) 1.72 27( 2) 1.84 28( 2) 1.77 26) 15( 1) 1.62 29( 1) 1.33 27) 25( 2) 1.84 28( 1) 1.32 28) 14( 1) 1.13 25( 2) 1.77 27( 1) 1.32 29) 26( 1) 1.33 bond angles in this interpretation ( 3( 1) - 1 - 4( 1)) 107.6 ( 3( 1) - 1 - 5( 1)) 106.0 ( 3( 1) - 1 - 6( 1)) 108.4 ( 4( 1) - 1 - 5( 1)) 119.3 ( 4( 1) - 1 - 6( 1)) 108.0 ( 5( 1) - 1 - 6( 1)) 107.2 ( 1( 1) - 3 - 8( 1)) 121.1 ( 1( 1) - 3 - 15( 1)) 115.4 ( 8( 1) - 3 - 15( 1)) 113.1 ( 1( 1) - 6 - 11( 1)) 120.5 ( 1( 1) - 6 - 13( 1)) 116.2 ( 11( 1) - 6 - 13( 1)) 123.2 ( 3( 1) - 8 - 16( 1)) 111.9 ( 3( 1) - 8 - 24( 1)) 117.7 ( 16( 1) - 8 - 24( 1)) 94.8 ( 12( 1) - 10 - 13( 1)) 124.4 ( 6( 1) - 11 - 18( 1)) 120.0 ( 7( 1) - 12 - 10( 1)) 121.1 ( 7( 1) - 12 - 18( 1)) 119.6 ( 10( 1) - 12 - 18( 1)) 119.3 ( 6( 1) - 13 - 10( 1)) 114.2 ( 17( 1) - 14 - 21( 1)) 111.5 ( 17( 1) - 14 - 25( 2)) 93.1 ( 17( 1) - 14 - 28( 1)) 132.7 ( 21( 1) - 14 - 25( 2)) 69.9 ( 21( 1) - 14 - 28( 1)) 105.8 ( 25( 2) - 14 - 28( 1)) 73.3 ( 3( 1) - 15 - 23( 1)) 88.3 ( 3( 1) - 15 - 26( 1)) 106.0 ( 23( 1) - 15 - 26( 1)) 105.3 ( 8( 1) - 16 - 20( 1)) 114.2 ( 8( 1) - 16 - 22( 1)) 110.4 ( 20( 1) - 16 - 22( 1)) 110.0 ( 14( 1) - 17 - 20( 1)) 111.3 ( 11( 1) - 18 - 12( 1)) 118.8 ( 2( 1) - 19 - 9( 1)) 107.7 ( 16( 1) - 20 - 17( 1)) 110.2 ( 14( 1) - 21 - 22( 1)) 113.3 ( 16( 1) - 22 - 21( 1)) 112.0 ( 15( 1) - 23 - 24( 1)) 116.7 ( 8( 1) - 24 - 23( 1)) 99.3 ( 14( 2) - 25 - 27( 2)) 68.3 ( 14( 2) - 25 - 28( 2)) 37.6 ( 27( 2) - 25 - 28( 2)) 42.8 ( 15( 1) - 26 - 29( 1)) 123.1 ( 25( 2) - 27 - 28( 1)) 65.7 ( 14( 1) - 28 - 25( 2)) 69.0 ( 14( 1) - 28 - 27( 1)) 109.7 ( 25( 2) - 28 - 27( 1)) 71.5 ------------------------------------------------------------------------------ --------------------- overall plot of the structure ------------------------- ------------ projection on l.s.q. plane ---- scale : 2.50 cms/a ------------ 28 * * 27 * * 14 * * * 17 * 21 * * * * 20 25 * 22 * * * 16 29 * 24 * * * * * * 8 * 23 * 26 * * 9**19 * 3 * * * 4 * * * 15 * * * 1 * * * 5 * 2 * 6 * * 11 * * * * 18 13 * * * * 10 * * 12 * * 7 ---------------------------------------------------------------------------- fragment number 1 , 22 peaks included peak 1 3 4 5 6 7 8 10 11 12 13 14 15 linked to 3 1 1 1 1 12 3 12 6 7 6 17 3 4 8 11 16 13 18 10 10 21 23 5 15 13 24 18 28 26 6 peak 16 17 18 20 21 22 23 24 26 27 28 29 linked to 8 14 11 16 14 16 15 8 15 28 14 26 20 20 12 17 22 21 24 23 29 27 22 ---------------------------------------------------------------------------- fragments with less than five peaks peak 2 9 19 linked to 19 19 2 9 fragment 2 2 2 ------------------------------------------------------------------------------ ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ *** Output section *** Test in Pna2(1) Final residual value = 12.29% *** warning *** freely floating origin along z Serial Atom Label Height*10 x y z Occ. B[iso] Frag 1) Cl Cl1 322 0.324 0.248 0.401 1.000 1.41 0 2) S S1 211 0.485 -0.016 0.417 1.000 2.43 0 3) N N1 105 0.430 0.249 0.395 1.000 2.34 0 4) O O1 105 0.299 0.294 0.531 1.000 1.63 0 5) O O2 96 0.296 0.293 0.268 1.000 2.34 0 6) C C1 90 0.289 0.119 0.403 1.000 1.37 0 7) C C2 76 0.215 -0.199 0.391 1.000 1.96 0 8) C C3 76 0.482 0.218 0.519 1.000 1.13 0 9) C C4 69 0.658 0.008 0.422 1.000 2.00 0 10) C C5 68 0.241 -0.031 0.274 1.000 1.89 0 11) C C6 67 0.287 0.064 0.528 1.000 1.97 0 12) C C7 67 0.240 -0.088 0.395 1.000 1.18 0 13) C C8 64 0.268 0.075 0.268 1.000 1.90 0 14) C C9 64 0.602 0.448 0.804 1.000 2.51 0 15) C C10 61 0.471 0.215 0.253 1.000 2.68 0 16) C C11 58 0.497 0.308 0.621 1.000 1.97 0 17) C C12 58 0.558 0.485 0.662 1.000 2.24 0 18) C C13 58 0.263 -0.041 0.527 1.000 1.62 0 19) C C14 58 0.580 0.056 0.483 1.000 1.83 0 20) C C15 55 0.551 0.397 0.556 1.000 1.99 0 21) C C16 54 0.555 0.352 0.868 1.000 2.72 0 22) C C17 52 0.543 0.268 0.764 1.000 2.54 0 23) C C18 49 0.566 0.174 0.352 1.000 3.43 0 24) C C19 38 0.568 0.198 0.498 1.000 4.36 0 25) Q Q1 21 0.484 0.513 0.407 1.000 2.05 0 26) Q Q2 20 0.499 0.320 0.173 1.000 2.05 0 27) Q Q3 20 0.608 0.444 1.017 1.000 2.05 0 28) C C20 17 0.631 0.491 0.898 1.000 2.34 0 29) Q Q4 16 0.541 0.397 0.237 1.000 2.05 0 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ The following Atom(s) has been deleted : C19 Final R value is 12.29% (Block 1, Set 2, # of LSQ Refinement 2)