****************************************************************************** 2007src0237r in P2(1)/c Thu Jun 21 2007 at 11:40:03 Sir2004 starts on: 2007src0 Used commands & directives: %data Cell 10.723 10.240 20.153 90.000 92.712 90.000 Space P 1 21/c 1 Content C 84 H 144 N 8 O 8 Si 8 Reflections 2007src0237r.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 2007src0.bin 31 direct access scratch file 32 sequential scratch file 34 reflection input file 2007src0237r.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 2007src0237r in P2(1)/c ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Direct cell: a = 10.723 b = 10.240 c = 20.153 alpha = 90.000 beta = 92.712 gamma = 90.000 Cell volume = 2210.39 Crystal family : Monoclinic Space group (centrosymmetric) : P 1 21/c 1 Symmetry-operations 1) x , y , z 2) -x , y+1/2, -z+1/2 3) -x , -y , -z 4) x , -y+1/2, z+1/2 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 = 14 Fourier limits : 0.000 < x < 1.000 0.000 < y < 0.250 0.000 < z < 1.000 Patterson limits : 0.000 < x < 0.500 0.000 < y < 0.500 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 144 1 Carbon C 84 6 Nitrogen N 8 7 Oxygen O 8 8 Silicon Si 8 14 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 Si 6.292 2.439 3.035 32.334 1.989 0.678 1.541 81.694 1.141 Number of atoms in asymmetric unit = 27.00 Equivalent number of equal atoms in primitive cell = 81 Volume per atom = 20.47 Syst. absent : 0 3 0 Fobs = 1.910 Sigma(Fobs) = 1.440 Syst. absent : 0 3 0 Fobs = 1.280 Sigma(Fobs) = 2.140 Syst. absent : 0 -3 0 Fobs = 0.000 Sigma(Fobs) = 2.650 Syst. absent : 0 -3 0 Fobs = 0.000 Sigma(Fobs) = 1.470 Syst. absent : 0 3 0 Fobs = 1.390 Sigma(Fobs) = 1.850 Syst. absent : 0 -3 0 Fobs = 0.000 Sigma(Fobs) = 2.240 Syst. absent : 0 5 0 Fobs = 0.000 Sigma(Fobs) = 2.710 Syst. absent : 0 -5 0 Fobs = 5.930 Sigma(Fobs) = 3.100 Syst. absent : 0 5 0 Fobs = 0.630 Sigma(Fobs) = 2.050 Syst. absent : 0 -5 0 Fobs = 2.200 Sigma(Fobs) = 2.750 .... and so on Space Group Determination Routine Crystal System determination by geometrical analysis of the cell: MONOCLINIC Unique axis b Total number of independent reflections : 40002 Total number of reflections considered: 40002 Total number of reflections greater than 3s: 40002 < fo >Total : 735.7687 < fo/sfo >Total : 27.06232 SYSTEMATIC ABSENCE EXCEPTIONS Note: Symbol # means not equal Refl. Total Condition N.Refl. N.(>3s) Sym. Op. Type Number 0 0 l 109 l#2n 52 52 3.0 0.3 ______ 0 k 0 46 k#2n 24 24 3.3 0.3 _ 21 _ h 0 0 59 h#2n 27 27 1339.8 6.2 ______ 0 k l 2370 k#2n 1170 1170 486.3 4.7 ______ l#2n 1185 1185 583.6 5.0 ______ k#2n,l#2n 1774 1774 503.0 4.8 ______ k+l#2n 1193 1193 439.4 4.7 ______ h 0 l 2389 h#2n 1222 1222 356.1 2.9 ______ l#2n 1155 1155 1.2 0.2 _ c _ h#2n,l#2n 1793 1793 243.1 2.0 ______ h+l#2n 1209 1209 359.9 2.9 ______ h k 0 1315 h#2n 663 663 455.6 5.3 ______ k#2n 653 653 383.8 5.0 ______ h#2n,k#2n 988 988 399.2 5.0 ______ h+k#2n 660 660 357.6 4.8 ______ h k l 40002 h+k#2n 19968 19968 367.9 4.5 ______ k+l#2n 19913 19913 309.0 4.3 ______ h+l#2n 19959 19959 373.5 4.5 ______ h+k+l#2n 20080 20080 336.3 4.5 ______ Extinction Group Fig.Mer P 1 21/c 1 0.522 P 1 c 1 0.219 P 1 21 1 0.112 P 1 21/n 1 0.063 P 1 21/a 1 0.063 A 1 _ 1 0.058 P 1 _ 1 0.047 P 1 a 1 0.027 P 1 n 1 0.027 C 1 _ 1 0.007 C 1 c 1 0.007 A 1 n 1 0.007 I 1 _ 1 0.007 I 1 a 1 0.007 Systematically absent reflections analisys Number and percentage of F's > param * sigma(F) Number percentage param 599 51% 0.00 410 35% 0.50 234 20% 1.00 111 9% 1.50 47 4% 2.00 28 2% 2.50 12 1% 3.00 7 1% 3.50 3 0% 4.00 1 0% 4.50 1 0% 5.00 40002 input reflections 1680 Fo(s) negative set to 0.0 5049 independent input reflections 1179 systematically absent reflections rejected 13 13 26 maximum h,k,l values 0.4219 maximum s**2 = (sin(theta)/lambda)**2 0.7698 Angstrom resolution 21 reflections are not in input data Symmetry equivalent reflections merged: Rsym(F) = 2.68% 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 1 0 1 100 8.0 - 6.0 22 17 5 23 6.0 - 5.0 43 42 1 2 5.0 - 4.0 202 199 3 1 4.0 - 3.0 624 622 2 0 3.0 - 2.5 811 810 1 0 2.5 - 2.0 2163 2163 0 0 2.0 - 1.8 1514 1514 0 0 1.8 - 1.6 2495 2495 0 0 1.6 - 1.4 3299 3299 0 0 1.4 - 1.3 2122 2122 0 0 1.3 - 1.2 2751 2751 0 0 1.2 - 1.1 3618 3618 0 0 1.1 - 1.0 4300 4300 0 0 1.0 - 0.9 5323 5323 0 0 0.9 - 0.8 7068 7068 0 0 0.8 - 0.7 2486 2480 6 0 -1.758 -1.517 -1.276 -1.036 -0.795 -0.554 * * * * * * ********************************************************* * * * * 0.029* w * ** * w * * * w * * * w * * * w * * 0.105* w* ** * * w * * * w * * * w * * * w * 0.182* * w ** * *w * * w* ********************************** * w* * y = s**2 * * x * x = ln / sigfsq * 0.258* *w * ( w ) = wilson * * * w * ( * ) = calc * * * w ********************************** * w* * intercept = -0.46359 * * w * * slope = -3.14898 * 0.334* w * * b(iso) = 1.57449 * * w * * u(iso) = 0.01994 * * w * * scale = 1.58978 * * x * scale*f(obs.)**2 = f(abs.)**2 * * * w ********************************** 0.411* * w ** * * * * ********************************************************* * * * * * * ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ *** pseudotranslation section *** 2007src0237r in P2(1)/c *** program searched for pseudo-translational symmetry *** *** no pseudo-translational symmetry has been found *** ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ *** Final statistics section *** Distribution of with sin(th)/lambda and Resol. (Ang.) sinth/lambda 0.0650 0.1299 0.1949 0.2598 0.3248 Resol. 7.70 3.85 2.57 1.92 1.54 0.0000 1.1378 0.8304 0.9862 0.9140 number 0 49 168 361 592 sinth/lambda 0.3897 0.4547 0.5196 0.5846 0.6496 Resol. 1.28 1.10 0.96 0.86 0.77 1.0881 1.0723 0.9734 1.0049 0.9783 number 889 1265 1667 2149 2677 Average values Average Numeric Graphic all data acentric centric hypercentric a. c. h. mod(E) 0.807 0.886 0.798 0.718 * E**2 1.000 1.000 1.000 1.000 E**3 1.565 1.329 1.596 1.916 * E**4 2.844 2.000 3.000 4.500 * E**5 5.762 3.323 6.383 12.260 * E**6 12.709 6.000 15.000 37.500 * mod(E**2-1) 0.962 0.736 0.968 1.145 * (E**2-1)**2 1.844 1.000 2.000 3.500 * (E**2-1)**3 6.177 2.000 8.000 26.000 * (mod(E**2-1))**3 6.854 2.415 8.691 26.903 * n(z) cumulative probability distribution z all data acentric centric hypercentric a. c. h. 0.1 0.238 0.095 0.248 0.368 * 0.2 0.346 0.181 0.345 0.463 * 0.3 0.420 0.259 0.416 0.526 * 0.4 0.469 0.330 0.473 0.574 * 0.5 0.517 0.393 0.520 0.612 * 0.6 0.561 0.451 0.561 0.643 * 0.7 0.599 0.503 0.597 0.670 * 0.8 0.629 0.551 0.629 0.694 * 0.9 0.656 0.593 0.657 0.715 * 1.0 0.680 0.632 0.683 0.733 * 1.2 0.721 0.699 0.727 0.765 * 1.4 0.756 0.753 0.763 0.791 * 1.6 0.786 0.798 0.794 0.813 * 1.8 0.812 0.835 0.820 0.832 * 2.0 0.837 0.865 0.843 0.848 * 2.2 0.856 0.889 0.862 0.863 * 2.4 0.873 0.909 0.879 0.875 * 2.6 0.888 0.926 0.893 0.886 * 2.8 0.903 0.939 0.906 0.896 * 3.0 0.916 0.950 0.917 0.905 * 3.2 0.927 0.959 0.926 0.913 * 3.4 0.935 0.967 0.935 0.920 * 3.6 0.943 0.973 0.942 0.926 * 3.8 0.950 0.978 0.949 0.932 * 4.0 0.956 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 2770 2456 2140 1847 1611 1393 1195 1006 843 708 E 1.6 1.7 1.8 1.9 2.0 2.1 2.2 2.3 2.4 2.5 number 584 457 358 283 222 171 130 92 73 50 Number and percentage Number and percentage of F's > param * sigma(F) of F's > limit number percentage param number percentage limit 4943 98% 0.50 504 10% 26.84 4784 95% 1.00 1008 20% 19.11 4648 92% 1.50 1512 30% 14.87 4574 91% 2.00 2016 40% 11.68 4520 90% 2.50 2520 50% 9.14 4460 88% 3.00 3024 60% 7.08 4381 87% 3.50 3528 70% 5.24 4328 86% 4.00 4032 80% 3.52 4266 84% 4.50 4536 90% 2.06 4219 84% 5.00 5040 100% 0.00 272 largest E-values > 1.915 to phase. ( 10 printed ) code h k l E fo/sig. code h k l E fo/sig. 1 1 6 -10 3.461 >6 2 8 3 18 3.383 >6 3 7 6 -16 3.367 >6 4 4 8 -13 3.318 >6 5 4 2 10 3.217 >6 6 6 8 2 3.180 >6 7 6 9 -14 3.065 >6 8 9 6 -14 2.990 >6 9 6 7 -1 2.960 >6 10 2 11 -1 2.953 >6 . . . . . . . . . 1000 smallest E-values for psi0 and negative quartets ( 10 printed ) code h k l E fo/sig. code h k l E fo/sig. 5040 10 5 -15 0.000 0.00 5041 5 8 -18 0.000 0.00 5042 9 9 1 0.000 0.00 5043 10 2 -16 0.000 0.00 5044 12 1 8 0.000 0.00 5045 5 10 -6 0.000 0.00 5046 13 0 6 0.000 0.00 5047 5 9 -2 0.000 0.00 5048 1 0 -22 0.000 0.00 5049 11 8 -4 0.000 0.00 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Sir2004 : Invariants routine Release 01.00 2007src0237r in P2(1)/c ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ 2129 strong triplets found among 272 strongest reflections (E-min = 1.915) strengthned by 50 free vectors using P-10 formula Used 8 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. 2129 2124 2118 2114 2108 2106 2100 2082 2062 2026 g 2.0 2.5 3.0 3.5 4.0 5.0 6.0 7.0 9.0 10.0 no. 1963 1852 1690 1510 1300 868 532 288 76 32 8000 Psi-zero triplets found among 272 strongest reflections and the 1000 weakest reflections Quartets statistic 3079 negative quartets found ( 3079 stored ) among 8000 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. 3079 2689 2427 2155 1846 1572 1125 778 530 255 g 2.0 2.5 3.0 3.5 4.0 5.0 6.0 7.0 9.0 10.0 no. 123 60 36 18 10 3 1 0 0 0 number of relationships calculated stored positive estimated triplets 2089 2089 negative estimated triplets 35 35 psi-zero triplets 8000 8000 negative estimated quartets 2581 2581 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Sir2004 : Phase routine Release 01.00 2007src0237r in P2(1)/c ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Number of Pos. Est. Triplets = 2089 with G > 0.20 Number of Neg. Est. Triplets = 32 with |G| > 0.60 Number of Neg. Est. Quartets = 1000 with |G| > 0.20 Number of refl. to phase = 272 Number of random phases = 90 Number of reflexions in LSQ = 3527 ( 70% of total, F's > 5.238 ) Number of atoms to locate = 27.00 Number of atoms used in LSQ = 32.00 Observations / Parameters = 27.55 Resolution & grid step (Ang) = 0.77 0.33 Fourier map grid points = 32 32 60 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 21/c 1 Cell: 10.72 10.24 20.15 0.50 0.00 0.00 Cheshire cell: 5.36 5.12 10.08 Transf. Matrix 0.00 0.50 0.00 Grid: 0.06 0.07 0.03 0.00 0.00 0.50 Grid points: 17 16 31 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ 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 ( 80) 2.842 2 2 ( 62) 2.841 2 3 ( 52) 2.827 4 4 ( 88) 2.818 4 5 ( 81) 2.515 14 6 ( 63) 2.503 10 7 ( 58) 2.188 13 8 ( 84) 2.185 11 9 ( 73) 2.184 5 10 ( 24) 2.151 23 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Extending phases for Block # 1 Set 1 Trial 80 eFom = 2.842 UnDet 1% Trial 80 End of DSR - Final FOM = 7.589 R% = 30.29 25.93 21.61 13.37 14.62 14.86 8.97 8.32 8.28 8.28 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ *** Final interpretation *** 2007src0237r in P2(1)/c Assumed atomic parameters and limits for interatomic bonds and angles (interspecies and intraspecies) distances angles atomic type radius minimum maximum minimum maximum number Si 1.110 1.10 2.66 80.00 155.00 14 O 0.730 0.88 2.21 80.00 155.00 8 N 0.750 0.89 2.23 80.00 155.00 7 C 0.770 0.90 2.26 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 2 Si Si 80. - 155. 2 1 O O 80. - 155. 3 2 N N 80. - 155. 4 27 C C 80. - 155. range of bond distances used to build fragments group group 1 group 2 group 3 group 4 1 (1.33-2.66) (1.10-2.21) (1.12-2.23) (1.13-2.26) 2 (0.88-1.75) (0.89-1.78) (0.90-1.80) 3 (0.90-1.80) (0.91-1.82) 4 (0.92-1.85) ------------------------------------------------------------------------------ interpeak distances up to 2.63 1) 6( 1) 1.79 13( 1) 1.87 18( 1) 1.86 24( 1) 1.86 29( 1) 2.02 2) 5( 1) 1.81 20( 1) 1.87 21( 1) 1.86 27( 1) 1.86 30( 1) 1.17 3) 9( 1) 1.21 4) 16( 1) 1.21 5) 2( 1) 1.81 9( 1) 1.38 16( 1) 1.41 6) 1( 1) 1.79 15( 1) 1.48 16( 1) 1.37 7) 11( 1) 1.40 12( 1) 1.39 15( 1) 1.53 8) 10( 1) 1.40 19( 1) 1.39 9) 3( 1) 1.21 5( 1) 1.38 15( 1) 1.55 10) 8( 1) 1.40 14( 1) 1.39 11) 7( 1) 1.40 26( 1) 1.40 12) 7( 1) 1.39 25( 1) 1.41 13) 1( 1) 1.87 29( 1) 1.81 14) 10( 1) 1.39 15( 1) 1.53 17( 1) 1.40 15) 6( 1) 1.48 7( 1) 1.53 9( 1) 1.55 14( 1) 1.53 16) 4( 1) 1.21 5( 1) 1.41 6( 1) 1.37 17) 14( 1) 1.40 23( 1) 1.39 18) 1( 1) 1.86 32( 1) 0.95 19) 8( 1) 1.39 23( 1) 1.40 20) 2( 1) 1.87 30( 1) 1.09 21) 2( 1) 1.86 28( 1) 0.98 22) 25( 1) 1.39 26( 1) 1.40 23) 17( 1) 1.39 19( 1) 1.40 24) 1( 1) 1.86 25) 12( 1) 1.41 22( 1) 1.39 26) 11( 1) 1.40 22( 1) 1.40 27) 2( 1) 1.86 28) 21( 1) 0.98 29) 1( 1) 2.02 13( 1) 1.81 30) 2( 1) 1.17 20( 1) 1.09 32) 18( 1) 0.95 accepted distances in this interpretation 1) 6( 1) 1.79 13( 1) 1.87 18( 1) 1.86 24( 1) 1.86 29( 1) 2.02 2) 5( 1) 1.81 20( 1) 1.87 21( 1) 1.86 27( 1) 1.86 30( 1) 1.17 3) 9( 1) 1.21 4) 16( 1) 1.21 5) 2( 1) 1.81 9( 1) 1.38 16( 1) 1.41 6) 1( 1) 1.79 15( 1) 1.48 16( 1) 1.37 7) 11( 1) 1.40 12( 1) 1.39 15( 1) 1.53 8) 10( 1) 1.40 19( 1) 1.39 9) 3( 1) 1.21 5( 1) 1.38 15( 1) 1.55 10) 8( 1) 1.40 14( 1) 1.39 11) 7( 1) 1.40 26( 1) 1.40 12) 7( 1) 1.39 25( 1) 1.41 13) 1( 1) 1.87 29( 1) 1.81 14) 10( 1) 1.39 15( 1) 1.53 17( 1) 1.40 15) 6( 1) 1.48 7( 1) 1.53 9( 1) 1.55 14( 1) 1.53 16) 4( 1) 1.21 5( 1) 1.41 6( 1) 1.37 17) 14( 1) 1.40 23( 1) 1.39 18) 1( 1) 1.86 32( 1) 0.95 19) 8( 1) 1.39 23( 1) 1.40 20) 2( 1) 1.87 30( 1) 1.09 21) 2( 1) 1.86 28( 1) 0.98 22) 25( 1) 1.39 26( 1) 1.40 23) 17( 1) 1.39 19( 1) 1.40 24) 1( 1) 1.86 25) 12( 1) 1.41 22( 1) 1.39 26) 11( 1) 1.40 22( 1) 1.40 27) 2( 1) 1.86 28) 21( 1) 0.98 29) 1( 1) 2.02 13( 1) 1.81 30) 2( 1) 1.17 20( 1) 1.09 32) 18( 1) 0.95 bond angles in this interpretation ( 6( 1) - 1 - 13( 1)) 109.9 ( 6( 1) - 1 - 18( 1)) 108.9 ( 6( 1) - 1 - 24( 1)) 108.6 ( 6( 1) - 1 - 29( 1)) 77.9 ( 13( 1) - 1 - 18( 1)) 110.8 ( 13( 1) - 1 - 24( 1)) 109.7 ( 13( 1) - 1 - 29( 1)) 55.3 ( 18( 1) - 1 - 24( 1)) 109.1 ( 18( 1) - 1 - 29( 1)) 166.0 ( 24( 1) - 1 - 29( 1)) 79.2 ( 5( 1) - 2 - 20( 1)) 106.8 ( 5( 1) - 2 - 21( 1)) 106.6 ( 5( 1) - 2 - 27( 1)) 108.4 ( 5( 1) - 2 - 30( 1)) 73.7 ( 20( 1) - 2 - 21( 1)) 111.6 ( 20( 1) - 2 - 27( 1)) 111.0 ( 20( 1) - 2 - 30( 1)) 33.0 ( 21( 1) - 2 - 27( 1)) 112.2 ( 21( 1) - 2 - 30( 1)) 122.2 ( 27( 1) - 2 - 30( 1)) 122.6 ( 2( 1) - 5 - 9( 1)) 119.7 ( 2( 1) - 5 - 16( 1)) 130.4 ( 9( 1) - 5 - 16( 1)) 109.7 ( 1( 1) - 6 - 15( 1)) 130.4 ( 1( 1) - 6 - 16( 1)) 118.3 ( 15( 1) - 6 - 16( 1)) 111.0 ( 11( 1) - 7 - 12( 1)) 119.7 ( 11( 1) - 7 - 15( 1)) 118.1 ( 12( 1) - 7 - 15( 1)) 122.2 ( 10( 1) - 8 - 19( 1)) 121.1 ( 3( 1) - 9 - 5( 1)) 125.5 ( 3( 1) - 9 - 15( 1)) 125.9 ( 5( 1) - 9 - 15( 1)) 108.6 ( 8( 1) - 10 - 14( 1)) 119.9 ( 7( 1) - 11 - 26( 1)) 120.5 ( 7( 1) - 12 - 25( 1)) 119.8 ( 1( 1) - 13 - 29( 1)) 66.7 ( 10( 1) - 14 - 15( 1)) 121.9 ( 10( 1) - 14 - 17( 1)) 119.3 ( 15( 1) - 14 - 17( 1)) 118.6 ( 6( 1) - 15 - 7( 1)) 111.4 ( 6( 1) - 15 - 9( 1)) 100.9 ( 6( 1) - 15 - 14( 1)) 113.4 ( 7( 1) - 15 - 9( 1)) 108.2 ( 7( 1) - 15 - 14( 1)) 115.3 ( 9( 1) - 15 - 14( 1)) 106.4 ( 4( 1) - 16 - 5( 1)) 124.6 ( 4( 1) - 16 - 6( 1)) 125.6 ( 5( 1) - 16 - 6( 1)) 109.7 ( 14( 1) - 17 - 23( 1)) 120.3 ( 1( 1) - 18 - 32( 1)) 129.0 ( 8( 1) - 19 - 23( 1)) 118.9 ( 2( 1) - 20 - 30( 1)) 35.6 ( 2( 1) - 21 - 28( 1)) 109.1 ( 25( 1) - 22 - 26( 1)) 119.7 ( 17( 1) - 23 - 19( 1)) 120.4 ( 12( 1) - 25 - 22( 1)) 120.5 ( 11( 1) - 26 - 22( 1)) 119.8 ( 1( 1) - 29 - 13( 1)) 58.1 ( 2( 1) - 30 - 20( 1)) 111.3 ------------------------------------------------------------------------------ --------------------- overall plot of the structure ------------------------- ------------ projection on l.s.q. plane ---- scale : 2.49 cms/a ------------ 32 * 26 * * * 22 18 * * * * * 11 25 * * * * 1 * * * 24 7 * 31* * * 12 21 4 * * * * * * *16 * * 6 * * * * 13 * * 27 * 5 * 15 * * * * * * 2 * *9 * * 3 29 * * 30 14 * ** ** 1017 20 ** ** 23 8 ** ** 19 ---------------------------------------------------------------------------- fragment number 1 , 28 peaks included peak 1 2 3 4 5 6 7 8 9 10 11 12 13 linked to 6 5 9 16 2 1 11 10 3 8 7 7 1 13 20 9 15 12 19 5 14 26 25 18 21 16 16 15 15 24 27 peak 14 15 16 17 18 19 20 21 22 23 24 25 26 linked to 10 6 4 14 1 8 2 2 25 17 1 12 11 15 7 5 23 32 23 28 26 19 22 22 17 9 6 14 peak 27 28 32 linked to 2 21 18 ------------------------------------------------------------------------------ ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ *** Output section *** 2007src0237r in P2(1)/c Final residual value = 8.28% Serial Atom Label Height*10 x y z Occ. B[iso] Frag 1) Si Si1 244 0.617 0.013 0.213 1.000 1.53 1 2) Si Si2 241 0.765 -0.415 0.060 1.000 1.65 1 3) O O1 106 0.903 -0.165 0.029 1.000 2.10 1 4) N N1 102 0.599 -0.266 0.171 1.000 2.01 1 5) N N2 96 0.749 -0.250 0.091 1.000 1.46 1 6) C C1 96 0.692 -0.069 0.148 1.000 2.01 1 7) C C2 83 0.904 0.029 0.142 1.000 1.67 1 8) C C3 76 0.565 0.181 -0.011 1.000 2.05 1 9) C C4 76 0.824 -0.152 0.068 1.000 1.39 1 10) C C5 75 0.610 0.102 0.042 1.000 1.68 1 11) C C6 74 0.970 -0.057 0.184 1.000 2.04 1 12) C C7 73 0.943 0.158 0.137 1.000 2.22 1 13) C C8 73 0.444 0.013 0.197 1.000 2.12 1 14) C C9 73 0.736 0.068 0.048 1.000 1.55 1 15) C C10 71 0.788 -0.022 0.103 1.000 1.47 1 16) C C11 70 0.671 -0.201 0.140 1.000 1.38 1 17) C C12 70 0.815 0.110 -0.001 1.000 2.21 1 18) C C13 68 0.659 -0.070 0.294 1.000 2.66 1 19) C C14 68 0.644 0.224 -0.058 1.000 2.26 1 20) C C15 66 0.741 -0.406 -0.033 1.000 2.42 1 21) C C16 65 0.927 -0.468 0.085 1.000 2.69 1 22) C C17 64 1.115 0.114 0.217 1.000 2.49 1 23) C C18 63 0.770 0.188 -0.053 1.000 2.41 1 24) C C19 62 0.675 0.185 0.218 1.000 2.87 1 25) C C20 57 1.050 0.200 0.175 1.000 2.49 1 26) C C21 56 1.076 -0.015 0.221 1.000 2.50 1 27) C C22 50 0.645 -0.519 0.096 1.000 2.99 1 28) Q Q1 18 0.940 -0.556 0.068 1.000 2.01 1 29) Q Q2 13 0.529 0.090 0.132 1.000 2.01 1 30) C C23 13 0.744 -0.348 0.013 1.000 2.01 1 31) C C24 13 1.088 -0.008 0.094 1.000 2.01 1 32) C C25 13 0.740 -0.089 0.313 1.000 2.01 1 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Final R value is 8.28% (Block 1, Set 1, # of LSQ Refinement 1)