+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - MSDOS 32-BIT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-1 + + s92 started at 11:39:54 on 09-Sep-1999 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P-1 CELL 0.71073 8.422 11.734 14.333 104.74 103.07 99.03 ZERR 4.00 0.002 0.002 0.003 0.03 0.03 0.03 LATT 1 SFAC C H N O S UNIT 48 48 16 12 4 V = 1299.29 F(000) = 608.0 Mu = 0.26 mm-1 Cell Wt = 1169.26 Rho = 1.494 OMIT 0 -2 2 OMIT -1 0 1 OMIT 0 0 1 OMIT 2 2 2 ACTA FMAP 2 PLAN 10 L.S. 4 BOND WGHT 0.061900 0.634700 FVAR 0.42068 S1 5 0.26393 0.09512 0.87859 11.00000 0.02080 0.03369 = 0.02825 0.01396 0.00721 0.00562 O1 4 0.33677 0.21412 0.87979 11.00000 0.02673 0.03609 = 0.03543 0.01533 0.00911 -0.00016 O2 4 0.36816 0.01701 0.90584 11.00000 0.02502 0.04608 = 0.03659 0.02104 0.00927 0.01486 O3 4 -0.20323 -0.35524 0.45309 11.00000 0.09480 0.03279 = 0.04746 0.00960 -0.00533 0.02152 N1 3 -0.22715 -0.15958 0.48154 11.00000 0.03325 0.02582 = 0.02918 0.01089 0.00571 0.00684 N2 3 0.15215 0.10809 0.96000 11.00000 0.02288 0.03097 = 0.02552 0.01439 0.00702 0.00693 N3 3 -0.10136 0.12503 0.99189 11.00000 0.02430 0.02930 = 0.02425 0.00867 0.00631 0.00512 N4 3 -0.10542 0.32637 0.92371 11.00000 0.02839 0.02655 = 0.02192 0.00507 0.00269 0.00630 C1 1 -0.39090 -0.31018 0.32401 11.00000 0.03864 0.03551 = 0.03448 0.00505 0.00743 0.00621 C2 1 -0.26680 -0.27933 0.42466 11.00000 0.04369 0.03066 = 0.03479 0.01105 0.01103 0.00718 C3 1 -0.10927 -0.10368 0.57478 11.00000 0.02834 0.02807 = 0.02438 0.00872 0.00860 0.00546 C4 1 -0.06319 0.02290 0.60773 11.00000 0.03051 0.02996 = 0.02838 0.01383 0.00940 0.01089 C5 1 0.05145 0.08450 0.69899 11.00000 0.02845 0.02577 = 0.02801 0.01026 0.00945 0.00497 C6 1 0.12248 0.01994 0.76018 11.00000 0.02356 0.02967 = 0.02708 0.01212 0.00825 0.00691 C7 1 0.07920 -0.10544 0.72828 11.00000 0.03704 0.03121 = 0.03139 0.01477 0.00619 0.01195 C9 1 0.02237 0.16944 0.95779 11.00000 0.02235 0.02511 = 0.01927 0.00601 0.00269 0.00380 C8 1 -0.03484 -0.16736 0.63619 11.00000 0.04290 0.02506 = 0.03423 0.01152 0.00900 0.00895 C10 1 -0.22709 0.18292 0.99167 11.00000 0.02397 0.03122 = 0.02609 0.00800 0.00731 0.00564 C11 1 -0.23092 0.28103 0.95649 11.00000 0.02735 0.03195 = 0.02596 0.00609 0.00593 0.00871 C12 1 0.02151 0.27172 0.92532 11.00000 0.02701 0.02755 = 0.02215 0.00769 0.00648 0.00368 H1A 2 -0.26730 -0.10796 0.45553 11.00000 0.04382 H1B 2 -0.43464 -0.24085 0.30829 11.00000 0.04724 H1C 2 -0.33215 -0.34129 0.27069 11.00000 0.07140 H1D 2 -0.48759 -0.37756 0.31683 11.00000 0.07859 H2A 2 0.13250 0.04447 0.97975 11.00000 0.03885 H4 2 -0.11182 0.06648 0.56333 11.00000 0.03729 H5 2 0.08486 0.17031 0.72172 11.00000 0.02777 H7 2 0.13145 -0.14520 0.77158 11.00000 0.04461 H8 2 -0.05941 -0.25436 0.61431 11.00000 0.02805 H10 2 0.10661 0.30466 0.90500 11.00000 0.02905 H11 2 -0.32660 0.31716 0.95153 11.00000 0.03634 H12 2 -0.31560 0.14608 1.01390 11.00000 0.03489 S21 5 -0.01003 0.49000 1.23773 11.00000 0.02250 0.02437 = 0.02644 0.00851 0.00485 0.00537 O21 4 -0.13032 0.55189 1.19901 11.00000 0.02526 0.03359 = 0.03426 0.01372 0.00514 0.01156 O22 4 -0.06565 0.37478 1.25090 11.00000 0.02909 0.02532 = 0.03473 0.01173 0.00545 0.00286 O23 4 0.42281 1.00179 1.60367 11.00000 0.05803 0.02655 = 0.03725 0.01045 0.01067 0.01100 N21 3 0.45051 0.81869 1.62250 11.00000 0.03462 0.02489 = 0.02621 0.00682 0.00225 0.00688 N22 3 0.10095 0.47312 1.15754 11.00000 0.02478 0.02751 = 0.02488 0.01025 0.00538 0.00804 N23 3 0.34110 0.45576 1.11051 11.00000 0.02651 0.03355 = 0.02589 0.00405 0.00502 0.00566 N24 3 0.41931 0.30670 1.22971 11.00000 0.03216 0.03797 = 0.03973 0.01045 0.00206 0.01499 C21 1 0.61879 0.99945 1.75201 11.00000 0.04047 0.04243 = 0.02743 0.00352 0.00690 -0.00176 C22 1 0.48805 0.94154 1.65302 11.00000 0.03238 0.02776 = 0.02786 0.00688 0.01104 0.00431 C23 1 0.33991 0.74270 1.53063 11.00000 0.02713 0.02464 = 0.02517 0.00603 0.00535 0.00806 C24 1 0.26071 0.62706 1.52597 11.00000 0.04389 0.02800 = 0.02799 0.01196 0.00446 0.00673 C25 1 0.15534 0.54915 1.43735 11.00000 0.03827 0.02395 = 0.02945 0.00995 0.00596 0.00357 C26 1 0.12719 0.58559 1.35195 11.00000 0.02328 0.02443 = 0.02383 0.00648 0.00648 0.00757 C27 1 0.20656 0.70034 1.35529 11.00000 0.03292 0.02636 = 0.02494 0.01128 0.00628 0.00697 C28 1 0.31365 0.77803 1.44398 11.00000 0.03146 0.02442 = 0.03056 0.00893 0.00738 0.00370 C29 1 0.24309 0.42451 1.16585 11.00000 0.02349 0.02454 = 0.02203 0.00112 0.00106 0.00426 C210 1 0.47699 0.41046 1.11553 11.00000 0.02682 0.04451 = 0.03390 0.00552 0.00821 0.00888 C211 1 0.51713 0.33798 1.17452 11.00000 0.02809 0.04566 = 0.03858 0.00473 0.00329 0.01493 C212 1 0.28134 0.34982 1.22489 11.00000 0.02952 0.03399 = 0.03364 0.01180 0.00725 0.01064 H21A 2 0.48894 0.78280 1.66768 11.00000 0.04125 H22A 2 0.10508 0.53198 1.12789 11.00000 0.05248 H24 2 0.27201 0.60184 1.58209 11.00000 0.04520 H25 2 0.10182 0.47387 1.43430 11.00000 0.04075 H27 2 0.18762 0.72027 1.29509 11.00000 0.02380 H28 2 0.37219 0.85680 1.44517 11.00000 0.03365 H210 2 0.54300 0.43628 1.07976 11.00000 0.05758 H211 2 0.61540 0.31071 1.18273 11.00000 0.04864 H212 2 0.21354 0.32852 1.26180 11.00000 0.04158 H21B 2 0.61219 0.97186 1.78961 11.00000 0.08110 HKLF 4 Covalent radii and connectivity table for s92 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 S1 - O1 O2 N2 C6 O1 - S1 O2 - S1 O3 - C2 N1 - C2 C3 N2 - C9 S1 N3 - C9 C10 N4 - C12 C11 C1 - C2 C2 - O3 N1 C1 C3 - N1 C8 C4 C4 - C5 C3 C5 - C4 C6 C6 - C7 C5 S1 C7 - C8 C6 C9 - N3 C12 N2 C8 - C7 C3 C10 - N3 C11 C11 - N4 C10 C12 - N4 C9 S21 - O21 O22 N22 C26 O21 - S21 O22 - S21 O23 - C22 N21 - C22 C23 N22 - C29 S21 N23 - C210 C29 N24 - C212 C211 C21 - C22 C22 - O23 N21 C21 C23 - C28 C24 N21 C24 - C25 C23 C25 - C24 C26 C26 - C25 C27 S21 C27 - C28 C26 C28 - C27 C23 C29 - N23 C212 N22 C210 - N23 C211 C211 - N24 C210 C212 - N24 C29 16226 Reflections read, of which 10 rejected -10 =< h =< 10, -13 =< k =< 13, -17 =< l =< 17, Max. 2-theta = 50.03 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 0 1 0 1.02 0.07 6 0.52 0 -2 1 82.09 1.63 5 9.87 0 -1 1 10.76 0.12 3 5.89 1 1 1 797.97 15.05 3 231.14 2 0 2 350.71 8.21 4 49.35 -7 -8 6 6.73 1.78 2 11.70 -7 -7 9 0.57 1.37 3 7.62 7 Inconsistent equivalents 4550 Unique reflections, of which 0 suppressed R(int) = 0.0490 R(sigma) = 0.0441 Friedel opposites merged Maximum memory for data reduction = 2913 / 45789 ** Cell contents from UNIT instruction and atom list do not agree ** Unit-cell contents from UNIT instruction and atom list resp. C 48.00 48.00 H 48.00 44.00 N 16.00 16.00 O 12.00 12.00 S 4.00 4.00 Least-squares cycle 1 Maximum vector length = 511 Memory required = 3962 / 584818 wR2 = 0.1162 before cycle 1 for 4550 data and 449 / 449 parameters GooF = S = 1.036; Restrained GooF = 1.036 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0619 * P )^2 + 0.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.42067 0.00086 -0.007 OSF Mean shift/esd = 0.004 Maximum = -0.084 for z S1 Max. shift = 0.000 A for C11 Max. dU = 0.000 for H21B Least-squares cycle 2 Maximum vector length = 511 Memory required = 3962 / 584818 wR2 = 0.1162 before cycle 2 for 4550 data and 449 / 449 parameters GooF = S = 1.036; Restrained GooF = 1.036 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0619 * P )^2 + 0.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.42068 0.00086 0.003 OSF Mean shift/esd = 0.001 Maximum = -0.029 for z S1 Max. shift = 0.000 A for C11 Max. dU = 0.000 for H21B Least-squares cycle 3 Maximum vector length = 511 Memory required = 3962 / 584818 wR2 = 0.1162 before cycle 3 for 4550 data and 449 / 449 parameters GooF = S = 1.036; Restrained GooF = 1.036 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0619 * P )^2 + 0.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.42068 0.00086 0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z S1 Max. shift = 0.000 A for H25 Max. dU = 0.000 for H21B Least-squares cycle 4 Maximum vector length = 511 Memory required = 3962 / 584818 wR2 = 0.1162 before cycle 4 for 4550 data and 449 / 449 parameters GooF = S = 1.036; Restrained GooF = 1.036 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0619 * P )^2 + 0.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.42068 0.00086 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z S21 Max. shift = 0.000 A for H21B Max. dU = 0.000 for H22A No correlation matrix elements larger than 0.500 s92 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S1 0.26393 0.09512 0.87859 1.00000 0.02080 0.03369 0.02825 0.01396 0.00721 0.00562 0.02669 0.00128 0.00007 0.00005 0.00004 0.00000 0.00030 0.00032 0.00033 0.00025 0.00024 0.00023 0.00017 O1 0.33677 0.21412 0.87979 1.00000 0.02673 0.03609 0.03543 0.01533 0.00911 -0.00016 0.03265 0.00361 0.00019 0.00014 0.00012 0.00000 0.00085 0.00088 0.00096 0.00076 0.00073 0.00070 0.00039 O2 0.36816 0.01701 0.90584 1.00000 0.02502 0.04608 0.03659 0.02104 0.00927 0.01486 0.03332 0.00384 0.00019 0.00015 0.00012 0.00000 0.00083 0.00096 0.00096 0.00079 0.00073 0.00074 0.00039 O3 -0.20323 -0.35524 0.45309 1.00000 0.09480 0.03279 0.04746 0.00960 -0.00533 0.02152 0.06232 0.00461 0.00030 0.00016 0.00015 0.00000 0.00170 0.00101 0.00124 0.00092 0.00115 0.00106 0.00063 N1 -0.22715 -0.15958 0.48154 1.00000 0.03325 0.02582 0.02918 0.01089 0.00571 0.00684 0.02941 0.00440 0.00025 0.00017 0.00015 0.00000 0.00110 0.00099 0.00109 0.00087 0.00088 0.00084 0.00044 N2 0.15215 0.10809 0.96000 1.00000 0.02288 0.03097 0.02552 0.01439 0.00702 0.00693 0.02518 0.00426 0.00022 0.00017 0.00014 0.00000 0.00097 0.00101 0.00103 0.00086 0.00081 0.00080 0.00042 N3 -0.10136 0.12503 0.99189 1.00000 0.02430 0.02930 0.02425 0.00867 0.00631 0.00512 0.02602 0.00413 0.00022 0.00016 0.00014 0.00000 0.00098 0.00096 0.00101 0.00081 0.00080 0.00079 0.00042 N4 -0.10542 0.32637 0.92371 1.00000 0.02839 0.02655 0.02192 0.00507 0.00269 0.00630 0.02679 0.00407 0.00023 0.00016 0.00013 0.00000 0.00103 0.00095 0.00099 0.00079 0.00080 0.00080 0.00042 C1 -0.39090 -0.31018 0.32401 1.00000 0.03864 0.03551 0.03448 0.00505 0.00743 0.00621 0.03801 0.00599 0.00035 0.00025 0.00020 0.00000 0.00150 0.00139 0.00148 0.00117 0.00121 0.00120 0.00060 C2 -0.26680 -0.27933 0.42466 1.00000 0.04369 0.03066 0.03479 0.01105 0.01103 0.00718 0.03628 0.00573 0.00032 0.00021 0.00019 0.00000 0.00150 0.00126 0.00141 0.00111 0.00118 0.00113 0.00058 C3 -0.10927 -0.10368 0.57478 1.00000 0.02834 0.02807 0.02438 0.00872 0.00860 0.00546 0.02667 0.00510 0.00028 0.00019 0.00017 0.00000 0.00120 0.00114 0.00119 0.00096 0.00098 0.00094 0.00049 C4 -0.06319 0.02290 0.60773 1.00000 0.03050 0.02996 0.02838 0.01383 0.00940 0.01089 0.02797 0.00537 0.00029 0.00020 0.00017 0.00000 0.00124 0.00118 0.00125 0.00102 0.00101 0.00098 0.00050 C5 0.05145 0.08450 0.69899 1.00000 0.02845 0.02577 0.02801 0.01026 0.00945 0.00497 0.02686 0.00535 0.00028 0.00021 0.00017 0.00000 0.00121 0.00116 0.00124 0.00098 0.00099 0.00095 0.00049 C6 0.12248 0.01994 0.76018 1.00000 0.02356 0.02967 0.02708 0.01212 0.00825 0.00691 0.02577 0.00509 0.00027 0.00019 0.00017 0.00000 0.00113 0.00114 0.00122 0.00098 0.00096 0.00092 0.00048 C7 0.07920 -0.10544 0.72828 1.00000 0.03704 0.03121 0.03139 0.01477 0.00619 0.01195 0.03226 0.00563 0.00031 0.00021 0.00018 0.00000 0.00136 0.00124 0.00135 0.00109 0.00109 0.00106 0.00054 C9 0.02237 0.16944 0.95779 1.00000 0.02235 0.02511 0.01927 0.00601 0.00269 0.00380 0.02309 0.00471 0.00026 0.00019 0.00016 0.00000 0.00111 0.00106 0.00109 0.00089 0.00088 0.00088 0.00046 C8 -0.03484 -0.16736 0.63619 1.00000 0.04290 0.02506 0.03423 0.01152 0.00900 0.00895 0.03372 0.00582 0.00032 0.00022 0.00019 0.00000 0.00147 0.00121 0.00139 0.00106 0.00115 0.00105 0.00056 C10 -0.22709 0.18292 0.99167 1.00000 0.02397 0.03122 0.02609 0.00800 0.00731 0.00564 0.02724 0.00518 0.00028 0.00020 0.00017 0.00000 0.00118 0.00119 0.00122 0.00099 0.00097 0.00098 0.00050 C11 -0.23092 0.28103 0.95649 1.00000 0.02735 0.03195 0.02596 0.00609 0.00593 0.00871 0.02896 0.00520 0.00029 0.00021 0.00017 0.00000 0.00124 0.00121 0.00124 0.00099 0.00100 0.00101 0.00051 C12 0.02151 0.27172 0.92532 1.00000 0.02701 0.02755 0.02215 0.00769 0.00648 0.00368 0.02589 0.00509 0.00029 0.00020 0.00017 0.00000 0.00122 0.00114 0.00117 0.00095 0.00097 0.00096 0.00049 H1A -0.26730 -0.10796 0.45553 1.00000 0.04382 0.06157 0.00340 0.00248 0.00206 0.00000 0.00785 H1B -0.43464 -0.24085 0.30829 1.00000 0.04724 0.06146 0.00337 0.00257 0.00203 0.00000 0.00763 H1C -0.33215 -0.34129 0.27069 1.00000 0.07140 0.07495 0.00417 0.00289 0.00256 0.00000 0.00995 H1D -0.48759 -0.37756 0.31683 1.00000 0.07859 0.08190 0.00446 0.00321 0.00255 0.00000 0.01075 H2A 0.13250 0.04447 0.97975 1.00000 0.03885 0.05942 0.00324 0.00241 0.00197 0.00000 0.00733 H4 -0.11182 0.06648 0.56333 1.00000 0.03729 0.05805 0.00315 0.00222 0.00196 0.00000 0.00672 H5 0.08486 0.17031 0.72172 1.00000 0.02777 0.05484 0.00287 0.00218 0.00175 0.00000 0.00601 H7 0.13145 -0.14520 0.77158 1.00000 0.04461 0.06163 0.00339 0.00238 0.00209 0.00000 0.00741 H8 -0.05941 -0.25436 0.61431 1.00000 0.02805 0.05432 0.00285 0.00217 0.00175 0.00000 0.00605 H10 0.10661 0.30466 0.90500 1.00000 0.02905 0.05494 0.00308 0.00209 0.00182 0.00000 0.00627 H11 -0.32660 0.31716 0.95153 1.00000 0.03634 0.05666 0.00320 0.00221 0.00186 0.00000 0.00679 H12 -0.31560 0.14608 1.01390 1.00000 0.03489 0.05650 0.00317 0.00215 0.00189 0.00000 0.00665 S21 -0.01003 0.49000 1.23773 1.00000 0.02250 0.02437 0.02644 0.00851 0.00485 0.00537 0.02460 0.00122 0.00007 0.00005 0.00004 0.00000 0.00030 0.00029 0.00031 0.00023 0.00023 0.00022 0.00016 O21 -0.13032 0.55189 1.19901 1.00000 0.02526 0.03359 0.03426 0.01372 0.00514 0.01156 0.03032 0.00359 0.00019 0.00014 0.00012 0.00000 0.00083 0.00085 0.00093 0.00073 0.00071 0.00068 0.00037 O22 -0.06565 0.37478 1.25090 1.00000 0.02909 0.02532 0.03473 0.01173 0.00545 0.00286 0.03017 0.00349 0.00019 0.00013 0.00012 0.00000 0.00086 0.00079 0.00093 0.00070 0.00072 0.00066 0.00037 O23 0.42281 1.00179 1.60367 1.00000 0.05803 0.02655 0.03725 0.01045 0.01067 0.01100 0.04073 0.00397 0.00023 0.00014 0.00013 0.00000 0.00118 0.00084 0.00101 0.00078 0.00088 0.00081 0.00044 N21 0.45051 0.81869 1.62250 1.00000 0.03462 0.02489 0.02621 0.00682 0.00225 0.00688 0.02980 0.00436 0.00025 0.00017 0.00015 0.00000 0.00113 0.00098 0.00106 0.00085 0.00088 0.00084 0.00045 N22 0.10095 0.47312 1.15754 1.00000 0.02478 0.02751 0.02488 0.01025 0.00538 0.00804 0.02529 0.00418 0.00022 0.00017 0.00014 0.00000 0.00100 0.00096 0.00101 0.00083 0.00080 0.00078 0.00041 N23 0.34110 0.45576 1.11051 1.00000 0.02651 0.03355 0.02589 0.00405 0.00502 0.00566 0.03013 0.00425 0.00023 0.00017 0.00014 0.00000 0.00103 0.00103 0.00105 0.00085 0.00085 0.00083 0.00044 N24 0.41931 0.30670 1.22971 1.00000 0.03216 0.03797 0.03973 0.01045 0.00206 0.01499 0.03740 0.00474 0.00025 0.00018 0.00016 0.00000 0.00113 0.00114 0.00125 0.00097 0.00097 0.00092 0.00050 C21 0.61879 0.99945 1.75201 1.00000 0.04047 0.04243 0.02743 0.00352 0.00690 -0.00176 0.03989 0.00610 0.00035 0.00026 0.00021 0.00000 0.00156 0.00150 0.00143 0.00124 0.00119 0.00119 0.00065 C22 0.48805 0.94154 1.65302 1.00000 0.03238 0.02776 0.02786 0.00688 0.01104 0.00431 0.02947 0.00531 0.00029 0.00020 0.00018 0.00000 0.00127 0.00116 0.00126 0.00101 0.00103 0.00099 0.00052 C23 0.33991 0.74270 1.53063 1.00000 0.02713 0.02464 0.02517 0.00603 0.00535 0.00806 0.02601 0.00499 0.00027 0.00019 0.00017 0.00000 0.00119 0.00109 0.00121 0.00094 0.00096 0.00092 0.00049 C24 0.26071 0.62706 1.52597 1.00000 0.04389 0.02800 0.02799 0.01196 0.00446 0.00673 0.03373 0.00560 0.00032 0.00021 0.00019 0.00000 0.00147 0.00120 0.00132 0.00106 0.00112 0.00106 0.00056 C25 0.15534 0.54915 1.43735 1.00000 0.03827 0.02395 0.02945 0.00995 0.00596 0.00357 0.03119 0.00549 0.00031 0.00021 0.00018 0.00000 0.00136 0.00116 0.00132 0.00102 0.00106 0.00102 0.00054 C26 0.12719 0.58559 1.35195 1.00000 0.02328 0.02443 0.02383 0.00648 0.00648 0.00757 0.02376 0.00485 0.00026 0.00019 0.00016 0.00000 0.00112 0.00107 0.00117 0.00092 0.00092 0.00088 0.00047 C27 0.20656 0.70034 1.35529 1.00000 0.03292 0.02636 0.02494 0.01128 0.00628 0.00697 0.02766 0.00523 0.00029 0.00020 0.00018 0.00000 0.00129 0.00113 0.00124 0.00098 0.00101 0.00097 0.00050 C28 0.31365 0.77803 1.44398 1.00000 0.03146 0.02442 0.03056 0.00893 0.00738 0.00370 0.02921 0.00530 0.00029 0.00020 0.00018 0.00000 0.00127 0.00113 0.00131 0.00099 0.00103 0.00097 0.00051 C29 0.24309 0.42451 1.16585 1.00000 0.02349 0.02454 0.02203 0.00112 0.00106 0.00426 0.02555 0.00478 0.00027 0.00019 0.00016 0.00000 0.00114 0.00107 0.00116 0.00090 0.00092 0.00089 0.00048 C210 0.47699 0.41046 1.11553 1.00000 0.02682 0.04451 0.03390 0.00552 0.00821 0.00888 0.03625 0.00577 0.00031 0.00023 0.00020 0.00000 0.00129 0.00146 0.00143 0.00118 0.00112 0.00111 0.00058 C211 0.51713 0.33798 1.17452 1.00000 0.02809 0.04566 0.03858 0.00473 0.00329 0.01493 0.03925 0.00583 0.00032 0.00024 0.00020 0.00000 0.00134 0.00150 0.00151 0.00122 0.00116 0.00117 0.00062 C212 0.28134 0.34982 1.22489 1.00000 0.02952 0.03399 0.03364 0.01180 0.00725 0.01064 0.03194 0.00557 0.00030 0.00022 0.00019 0.00000 0.00129 0.00126 0.00137 0.00109 0.00109 0.00103 0.00054 H21A 0.48894 0.78280 1.66768 1.00000 0.04125 0.06047 0.00332 0.00236 0.00204 0.00000 0.00746 H22A 0.10508 0.53198 1.12789 1.00000 0.05248 0.06610 0.00357 0.00264 0.00224 0.00000 0.00847 H24 0.27201 0.60184 1.58209 1.00000 0.04520 0.06159 0.00332 0.00238 0.00212 0.00000 0.00767 H25 0.10182 0.47387 1.43430 1.00000 0.04075 0.06122 0.00326 0.00241 0.00198 0.00000 0.00714 H27 0.18762 0.72027 1.29509 1.00000 0.02380 0.05108 0.00273 0.00193 0.00179 0.00000 0.00574 H28 0.37219 0.85680 1.44517 1.00000 0.03365 0.05661 0.00300 0.00223 0.00180 0.00000 0.00644 H210 0.54300 0.43628 1.07976 1.00000 0.05758 0.07009 0.00389 0.00267 0.00235 0.00000 0.00905 H211 0.61540 0.31071 1.18273 1.00000 0.04864 0.06466 0.00371 0.00245 0.00212 0.00000 0.00783 H212 0.21354 0.32852 1.26180 1.00000 0.04158 0.05952 0.00334 0.00230 0.00203 0.00000 0.00752 H21B 0.61219 0.97186 1.78961 1.00000 0.08110 0.08969 0.00489 0.00346 0.00288 0.00000 0.01395 Final Structure Factor Calculation for s92 in P-1 Total number of l.s. parameters = 449 Maximum vector length = 511 Memory required = 3513 / 24017 wR2 = 0.1162 before cycle 5 for 4550 data and 0 / 449 parameters GooF = S = 1.036; Restrained GooF = 1.036 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0619 * P )^2 + 0.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0422 for 3709 Fo > 4sig(Fo) and 0.0551 for all 4550 data wR2 = 0.1162, GooF = S = 1.036, Restrained GooF = 1.036 for all data Occupancy sum of asymmetric unit = 40.00 for non-hydrogen and 22.00 for hydrogen atoms Principal mean square atomic displacements U 0.0359 0.0237 0.0205 S1 0.0440 0.0330 0.0209 O1 0.0492 0.0305 0.0203 O2 0.1166 0.0420 0.0284 O3 0.0362 0.0292 0.0229 N1 0.0336 0.0227 0.0192 N2 0.0298 0.0245 0.0237 N3 0.0329 0.0268 0.0207 N4 0.0430 0.0404 0.0306 C1 0.0444 0.0347 0.0298 C2 0.0295 0.0276 0.0229 C3 0.0343 0.0282 0.0214 C4 0.0296 0.0285 0.0225 C5 0.0314 0.0235 0.0224 C6 0.0401 0.0354 0.0213 C7 0.0265 0.0248 0.0180 C9 0.0440 0.0344 0.0228 C8 0.0319 0.0261 0.0238 C10 0.0352 0.0263 0.0253 C11 0.0306 0.0252 0.0219 C12 0.0281 0.0240 0.0217 S21 0.0371 0.0341 0.0198 O21 0.0388 0.0290 0.0227 O22 0.0596 0.0373 0.0253 O23 0.0404 0.0247 0.0242 N21 0.0284 0.0269 0.0205 N22 0.0381 0.0284 0.0239 N23 0.0515 0.0377 0.0230 N24 0.0569 0.0369 0.0259 C21 0.0357 0.0271 0.0256 C22 0.0309 0.0244 0.0227 C23 0.0484 0.0303 0.0226 C24 0.0422 0.0290 0.0224 C25 0.0266 0.0237 0.0209 C26 0.0342 0.0284 0.0204 C27 0.0339 0.0303 0.0235 C28 0.0337 0.0255 0.0174 C29 0.0502 0.0324 0.0261 C210 0.0586 0.0356 0.0236 C211 0.0352 0.0348 0.0259 C212 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.022 0.032 0.044 0.058 0.073 0.093 0.120 0.167 1.000 Number in group 467. 463. 440. 463. 477. 429. 463. 440. 454. 454. GooF 0.866 1.040 1.156 0.999 1.053 1.105 0.999 1.058 0.974 1.095 K 1.319 0.929 0.909 0.962 0.959 0.970 0.994 1.019 1.033 0.998 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.26 1.44 1.82 inf Number in group 455. 457. 459. 449. 457. 454. 456. 451. 457. 455. GooF 0.914 0.928 0.874 0.940 0.944 0.944 0.871 0.892 1.191 1.623 K 0.988 1.002 1.013 1.013 1.034 1.033 1.036 1.030 1.038 0.964 R1 0.126 0.096 0.070 0.063 0.055 0.045 0.038 0.034 0.041 0.045 Recommended weighting scheme: WGHT 0.0619 0.6381 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) -1 4 0 203.57 124.99 5.58 0.068 2.82 0 -1 2 995.69 1456.78 5.28 0.233 6.66 2 0 4 22.41 4.56 5.13 0.013 2.27 0 3 0 142.27 90.33 4.74 0.058 3.68 2 2 0 57.18 98.84 4.61 0.061 2.94 0 -1 6 188.09 282.31 4.49 0.102 2.31 1 -1 3 95.57 149.68 4.38 0.075 3.70 -1 -2 1 256.81 363.73 4.20 0.116 4.43 2 -1 3 221.92 308.92 3.91 0.107 2.77 -2 -2 6 74.29 115.08 3.85 0.065 2.20 -1 7 0 28.30 52.32 3.82 0.044 1.62 -1 -3 8 4.26 18.68 3.77 0.026 1.75 -3 -3 3 88.07 55.00 3.76 0.045 2.09 2 1 5 388.54 284.35 3.66 0.103 1.84 -1 -2 3 260.96 352.40 3.60 0.114 3.80 -3 -1 2 103.03 148.15 3.59 0.074 2.60 4 -5 1 36.43 62.29 3.57 0.048 1.67 -2 -1 2 251.64 336.22 3.51 0.112 3.66 2 2 1 2.45 11.73 3.47 0.021 2.67 -3 -3 4 129.80 179.95 3.44 0.082 2.04 0 -2 3 529.08 683.51 3.43 0.159 4.12 0 0 2 5.23 16.39 3.38 0.025 6.66 -2 -3 1 96.00 135.53 3.38 0.071 2.58 -4 5 0 3.31 13.89 3.38 0.023 1.68 -1 1 0 140.89 102.09 3.37 0.062 7.31 -4 -11 7 25.79 50.22 3.32 0.043 0.88 0 0 4 3.70 13.79 3.32 0.023 3.33 0 1 4 941.77 745.44 3.31 0.166 2.95 5 2 7 51.78 22.69 3.30 0.029 1.00 0 2 5 1075.86 858.46 3.25 0.179 2.16 0 -3 4 2.80 10.61 3.23 0.020 2.95 1 -2 3 504.76 642.62 3.22 0.154 3.53 -4 1 1 11.08 24.12 3.21 0.030 2.10 -6 -3 12 63.96 37.56 3.13 0.037 0.99 -1 5 2 1320.94 1072.93 3.12 0.200 2.01 0 2 7 11.48 28.03 3.11 0.032 1.65 -8 5 6 60.14 93.80 3.10 0.059 0.96 -1 -10 3 39.20 60.95 3.06 0.048 1.12 -3 -2 3 12.84 24.71 3.06 0.030 2.33 -7 2 12 37.74 11.64 3.05 0.021 0.91 -4 5 1 166.82 125.47 3.04 0.068 1.67 0 -4 7 50.95 32.46 3.03 0.035 1.85 -3 1 0 11.99 24.77 3.02 0.030 2.73 -1 1 2 365.82 461.44 2.97 0.131 5.06 6 -10 3 14.90 30.52 2.97 0.034 0.96 0 -5 8 252.12 194.33 2.97 0.085 1.58 -3 6 3 94.61 67.46 2.96 0.050 1.54 -5 -2 4 4.78 13.94 2.95 0.023 1.53 -1 -1 1 3902.24 4772.36 2.92 0.421 6.28 -2 0 1 9.90 20.74 2.90 0.028 4.16 Bond lengths and angles S1 - Distance Angles O1 1.4285 (0.0016) O2 1.4293 (0.0016) 120.33 (0.10) N2 1.6500 (0.0019) 107.96 (0.10) 103.69 (0.10) C6 1.7525 (0.0025) 108.61 (0.10) 109.01 (0.11) 106.35 (0.10) S1 - O1 O2 N2 O1 - Distance Angles S1 1.4285 (0.0016) O1 - O2 - Distance Angles S1 1.4293 (0.0016) O2 - O3 - Distance Angles C2 1.2173 (0.0030) O3 - N1 - Distance Angles C2 1.3774 (0.0031) C3 1.3969 (0.0030) 128.26 (0.21) N1 - C2 N2 - Distance Angles C9 1.3988 (0.0028) S1 1.6500 (0.0019) 124.38 (0.15) N2 - C9 N3 - Distance Angles C9 1.3364 (0.0028) C10 1.3446 (0.0028) 116.57 (0.19) N3 - C9 N4 - Distance Angles C12 1.3289 (0.0029) C11 1.3403 (0.0030) 117.53 (0.19) N4 - C12 C1 - Distance Angles C2 1.4961 (0.0036) C1 - C2 - Distance Angles O3 1.2173 (0.0030) N1 1.3774 (0.0031) 122.56 (0.24) C1 1.4961 (0.0036) 121.78 (0.23) 115.64 (0.22) C2 - O3 N1 C3 - Distance Angles N1 1.3969 (0.0030) C8 1.3992 (0.0032) 123.56 (0.20) C4 1.3997 (0.0031) 117.80 (0.20) 118.64 (0.22) C3 - N1 C8 C4 - Distance Angles C5 1.3763 (0.0033) C3 1.3997 (0.0031) 121.20 (0.21) C4 - C5 C5 - Distance Angles C4 1.3763 (0.0033) C6 1.3943 (0.0031) 119.55 (0.21) C5 - C4 C6 - Distance Angles C7 1.3858 (0.0032) C5 1.3943 (0.0031) 119.95 (0.22) S1 1.7525 (0.0024) 119.11 (0.17) 120.93 (0.17) C6 - C7 C5 C7 - Distance Angles C8 1.3828 (0.0035) C6 1.3858 (0.0032) 120.50 (0.21) C7 - C8 C9 - Distance Angles N3 1.3364 (0.0027) C12 1.3937 (0.0030) 121.37 (0.20) N2 1.3988 (0.0028) 115.21 (0.18) 123.40 (0.20) C9 - N3 C12 C8 - Distance Angles C7 1.3828 (0.0035) C3 1.3992 (0.0032) 120.15 (0.21) C8 - C7 C10 - Distance Angles N3 1.3446 (0.0028) C11 1.3711 (0.0033) 122.10 (0.21) C10 - N3 C11 - Distance Angles N4 1.3403 (0.0030) C10 1.3711 (0.0033) 121.12 (0.21) C11 - N4 C12 - Distance Angles N4 1.3289 (0.0029) C9 1.3937 (0.0030) 121.24 (0.21) C12 - N4 S21 - Distance Angles O21 1.4295 (0.0016) O22 1.4332 (0.0016) 119.70 (0.10) N22 1.6315 (0.0019) 103.70 (0.10) 108.73 (0.10) C26 1.7541 (0.0024) 109.63 (0.10) 108.26 (0.10) 105.97 (0.10) S21 - O21 O22 N22 O21 - Distance Angles S21 1.4295 (0.0016) O21 - O22 - Distance Angles S21 1.4332 (0.0015) O22 - O23 - Distance Angles C22 1.2258 (0.0028) O23 - N21 - Distance Angles C22 1.3574 (0.0029) C23 1.4084 (0.0030) 126.32 (0.20) N21 - C22 N22 - Distance Angles C29 1.3990 (0.0028) S21 1.6315 (0.0019) 125.98 (0.16) N22 - C29 N23 - Distance Angles C210 1.3307 (0.0031) C29 1.3394 (0.0029) 115.72 (0.21) N23 - C210 N24 - Distance Angles C212 1.3330 (0.0031) C211 1.3367 (0.0034) 116.75 (0.22) N24 - C212 C21 - Distance Angles C22 1.5018 (0.0036) C21 - C22 - Distance Angles O23 1.2258 (0.0028) N21 1.3574 (0.0029) 123.19 (0.22) C21 1.5018 (0.0036) 121.88 (0.22) 114.92 (0.22) C22 - O23 N21 C23 - Distance Angles C28 1.3891 (0.0032) C24 1.3929 (0.0032) 119.34 (0.22) N21 1.4084 (0.0030) 121.80 (0.20) 118.80 (0.20) C23 - C28 C24 C24 - Distance Angles C25 1.3716 (0.0035) C23 1.3929 (0.0032) 120.63 (0.22) C24 - C25 C25 - Distance Angles C24 1.3716 (0.0035) C26 1.3799 (0.0031) 119.76 (0.22) C25 - C24 C26 - Distance Angles C25 1.3799 (0.0031) C27 1.3901 (0.0030) 120.22 (0.21) S21 1.7541 (0.0023) 121.24 (0.17) 118.53 (0.17) C26 - C25 C27 C27 - Distance Angles C28 1.3763 (0.0033) C26 1.3901 (0.0030) 120.00 (0.21) C27 - C28 C28 - Distance Angles C27 1.3763 (0.0033) C23 1.3891 (0.0032) 120.02 (0.21) C28 - C27 C29 - Distance Angles N23 1.3394 (0.0029) C212 1.3895 (0.0033) 122.05 (0.21) N22 1.3990 (0.0028) 113.78 (0.19) 124.16 (0.21) C29 - N23 C212 C210 - Distance Angles N23 1.3307 (0.0031) C211 1.3708 (0.0037) 122.73 (0.25) C210 - N23 C211 - Distance Angles N24 1.3367 (0.0034) C210 1.3708 (0.0037) 121.57 (0.24) C211 - N24 C212 - Distance Angles N24 1.3330 (0.0031) C29 1.3895 (0.0033) 121.17 (0.24) C212 - N24 FMAP and GRID set by program FMAP 2 1 21 GRID -2.778 -2 -2 2.778 2 2 R1 = 0.0548 for 4550 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.46 at 0.2702 0.0209 0.2573 [ 1.03 A from C21 ] Deepest hole -0.43 at 0.0532 0.4647 0.2550 [ 0.68 A from S21 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 3408 / 23649 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7298 0.9791 1.7427 1.00000 0.05 0.46 1.03 C21 1.32 H21B 2.06 C22 2.62 H21A Q2 1 0.5952 1.0830 1.7825 1.00000 0.05 0.45 1.04 C21 1.36 H21B 2.05 C22 2.50 O23 Q3 1 0.6968 1.0626 1.7441 1.00000 0.05 0.32 0.96 C21 1.55 H21B 2.01 C22 2.56 O23 Q4 1 -0.3097 -0.3536 0.4813 1.00000 0.05 0.29 1.06 O3 1.39 C2 2.27 N1 2.39 H8 Q5 1 0.5795 0.9807 1.7217 1.00000 0.05 0.24 0.46 C21 0.99 H21B 1.04 C22 1.99 O23 Q6 1 0.4729 0.3142 0.9993 1.00000 0.05 0.22 1.52 H210 1.75 C210 1.82 O1 1.96 H11 Q7 1 0.1619 0.0385 0.7990 1.00000 0.05 0.21 0.55 C6 1.21 S1 1.68 C7 1.78 C5 Q8 1 -0.3326 -0.4033 0.3621 1.00000 0.05 0.21 1.41 O3 1.43 H1D 1.44 C1 1.44 C2 Q9 1 0.0863 0.5408 1.3043 1.00000 0.05 0.20 0.72 C26 1.06 S21 1.84 C25 1.85 C27 Q10 1 -0.3952 -0.1734 0.5194 1.00000 0.05 0.20 1.63 N1 1.77 H1A 2.14 H28 2.19 N21 Shortest distances between peaks (including symmetry equivalents) 1 3 1.06 2 3 1.14 3 5 1.18 1 5 1.24 2 5 1.26 4 8 1.61 1 2 1.86 4 10 2.31 Time profile in seconds ----------------------- 0.11: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 1.27: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.06: Set up l.s. refinement 0.00: Generate idealized H-atoms 9.19: Structure factors and derivatives 54.33: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 6.21: Solve l.s. equations 0.00: Generate HTAB table 0.16: Other dependent quantities, CIF, tables 0.61: Analysis of variance 0.33: Merge reflections for Fourier and .fcf 0.22: Fourier summations 0.33: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 11:41:07 Total elapsed time: 72.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++