+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 13:38:11 on 30-Jul-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01sot057 in C2/c CELL 0.71073 12.8588 10.7382 23.1122 90 93.811 90 ZERR 8 0.0002 0.0002 0.0004 0 0.003 0 LATT 7 SYMM -X, Y, 1/2-Z SFAC C H N O S UNIT 128 176 16 16 8 V = 3184.28 F(000) = 1312.0 Mu = 0.21 mm-1 Cell Wt = 2451.33 Rho = 1.278 SHEL 7 0.84 OMIT 2 0 0 TEMP -153 SIZE 0.2 0.2 0.2 EQIV $1 -x+1, y, -z+1/2 HTAB N1 O2_$1 HTAB FMAP 2 PLAN 30 BOND L.S. 4 WGHT 0.049300 0.782500 EXTI 0.002349 FVAR 0.22684 S1 5 0.432079 0.013353 0.341113 11.00000 0.01863 0.02326 = 0.01718 -0.00222 -0.00128 0.00629 N1 3 0.532058 -0.069397 0.324410 11.00000 0.02050 0.02356 = 0.01327 0.00182 -0.00016 0.00670 N2 3 0.586952 -0.130131 0.372035 11.00000 0.02017 0.02277 = 0.01459 0.00039 -0.00422 0.00733 O1 4 0.363486 -0.063336 0.371627 11.00000 0.02163 0.02821 = 0.02717 -0.00270 0.00350 -0.00014 O2 4 0.395919 0.069680 0.286978 11.00000 0.02835 0.03034 = 0.01928 -0.00130 -0.00614 0.01300 C1 1 0.645278 0.382277 0.507151 11.00000 0.05492 0.03924 = 0.04286 -0.01060 -0.00349 -0.01442 C2 1 0.586229 0.294962 0.465599 11.00000 0.03418 0.02295 = 0.02967 -0.00273 -0.00191 0.00108 C3 1 0.525252 0.200043 0.486138 11.00000 0.03177 0.02772 = 0.01749 -0.00302 0.00203 0.00338 C4 1 0.473100 0.117204 0.448268 11.00000 0.02294 0.02205 = 0.02214 0.00073 0.00338 0.00394 C5 1 0.481823 0.129780 0.389048 11.00000 0.01991 0.02078 = 0.01884 -0.00011 0.00002 0.00725 C6 1 0.540010 0.226210 0.367719 11.00000 0.04089 0.03319 = 0.01975 0.00441 0.00228 -0.00321 C7 1 0.592034 0.307495 0.405847 11.00000 0.04588 0.02704 = 0.03524 0.00556 0.00323 -0.01093 C8 1 0.686786 -0.069081 0.392225 11.00000 0.02070 0.02236 = 0.02051 -0.00239 -0.00313 0.00263 C9 1 0.729575 -0.166436 0.435971 11.00000 0.02444 0.03198 = 0.01764 0.00067 -0.00369 0.00605 C10 1 0.693005 -0.291033 0.408008 11.00000 0.02782 0.02714 = 0.02262 0.00319 -0.00293 0.00753 C11 1 0.621033 -0.256549 0.354272 11.00000 0.02244 0.02117 = 0.02061 -0.00050 -0.00244 0.00774 C12 1 0.682812 -0.245217 0.299473 11.00000 0.02676 0.02884 = 0.02004 -0.00311 -0.00130 0.01093 C13 1 0.757249 -0.136843 0.300879 11.00000 0.02135 0.03511 = 0.02296 0.00811 0.00082 0.01223 C14 1 0.757959 -0.054024 0.343561 11.00000 0.02026 0.02945 = 0.02642 0.00646 -0.00165 0.00235 C15 1 0.827544 -0.126985 0.251815 11.00000 0.03611 0.05257 = 0.03012 0.01007 0.01137 0.01469 C16 1 0.528856 -0.342370 0.344424 11.00000 0.03196 0.02551 = 0.03042 -0.00033 -0.00375 0.00269 H1A 2 0.702324 0.409892 0.490684 11.00000 0.05727 H1B 2 0.598326 0.447477 0.521251 11.00000 0.07563 H1C 2 0.669974 0.339029 0.545123 11.00000 0.07142 H1N 2 0.567129 -0.030936 0.301173 11.00000 0.03356 H3 2 0.517182 0.188505 0.525220 11.00000 0.02946 H4 2 0.430885 0.048918 0.462368 11.00000 0.02029 H6 2 0.546524 0.234110 0.327979 11.00000 0.03436 H7 2 0.637384 0.369038 0.391979 11.00000 0.05739 H8 2 0.671913 0.011943 0.409453 11.00000 0.01454 H9A 2 0.806966 -0.164414 0.440841 11.00000 0.01926 H9B 2 0.699990 -0.152922 0.472438 11.00000 0.02587 H10A 2 0.652512 -0.338814 0.435365 11.00000 0.03669 H10B 2 0.753060 -0.343790 0.398118 11.00000 0.02677 H12A 2 0.719869 -0.320745 0.292404 11.00000 0.04069 H12B 2 0.635561 -0.234821 0.265054 11.00000 0.03410 H14 2 0.806881 0.010130 0.342110 11.00000 0.02495 H15A 2 0.787564 -0.127063 0.214305 11.00000 0.04266 H15B 2 0.875159 -0.200897 0.252642 11.00000 0.06071 H15C 2 0.871216 -0.045550 0.255590 11.00000 0.05477 H16A 2 0.554158 -0.422774 0.332550 11.00000 0.04006 H16B 2 0.480319 -0.308591 0.310891 11.00000 0.03944 H16C 2 0.491166 -0.348546 0.379081 11.00000 0.03121 HKLF 4 Covalent radii and connectivity table for 01sot057 in C2/c C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 S1 - O1 O2 N1 C5 N1 - N2 S1 N2 - N1 C8 C11 O1 - S1 O2 - S1 C1 - C2 C2 - C3 C7 C1 C3 - C2 C4 C4 - C5 C3 C5 - C6 C4 S1 C6 - C7 C5 C7 - C6 C2 C8 - N2 C14 C9 C9 - C8 C10 C10 - C11 C9 C11 - N2 C16 C10 C12 C12 - C13 C11 C13 - C14 C15 C12 C14 - C13 C8 C15 - C13 C16 - C11 Operators for generating equivalent atoms: $1 -x+1, y, -z+1/2 9730 Reflections read, of which 1564 rejected -15 =< h =< 15, -12 =< k =< 12, -27 =< l =< 27, Max. 2-theta = 50.05 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 11 1 1 5.74 0.54 3 3.32 1 1 2 157.42 4.03 3 42.23 3 3 11 13.73 0.21 5 2.76 2 4 12 90.03 0.12 4 84.26 4 Inconsistent equivalents 2784 Unique reflections, of which 0 suppressed R(int) = 0.0554 R(sigma) = 0.0544 Friedel opposites merged Maximum memory for data reduction = 2108 / 33231 Least-squares cycle 1 Maximum vector length = 511 Memory required = 2768 / 348773 wR2 = 0.0986 before cycle 1 for 2784 data and 279 / 279 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0493 * P )^2 + 0.78 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22684 0.00060 0.002 OSF 2 0.00235 0.00052 0.000 EXTI Mean shift/esd = 0.002 Maximum = 0.020 for U13 S1 Max. shift = 0.000 A for H1B Max. dU = 0.000 for H1C Least-squares cycle 2 Maximum vector length = 511 Memory required = 2768 / 348773 wR2 = 0.0986 before cycle 2 for 2784 data and 279 / 279 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0493 * P )^2 + 0.78 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22684 0.00060 0.001 OSF 2 0.00235 0.00052 0.000 EXTI Mean shift/esd = 0.001 Maximum = 0.007 for U13 S1 Max. shift = 0.000 A for H16B Max. dU = 0.000 for H15B Least-squares cycle 3 Maximum vector length = 511 Memory required = 2768 / 348773 wR2 = 0.0986 before cycle 3 for 2784 data and 279 / 279 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0493 * P )^2 + 0.78 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22684 0.00060 0.001 OSF 2 0.00235 0.00052 0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H16B Max. dU = 0.000 for H15B Least-squares cycle 4 Maximum vector length = 511 Memory required = 2768 / 348773 wR2 = 0.0986 before cycle 4 for 2784 data and 279 / 279 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0493 * P )^2 + 0.78 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22684 0.00060 0.001 OSF 2 0.00235 0.00052 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for z S1 Max. shift = 0.000 A for H15B Max. dU = 0.000 for H1B Largest correlation matrix elements 0.580 U33 S1 / OSF 0.521 EXTI / OSF 0.569 U11 S1 / OSF 0.519 U22 S1 / OSF 01sot057 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S1 0.43208 0.01335 0.34111 1.00000 0.01863 0.02326 0.01718 -0.00222 -0.00128 0.00629 0.01980 0.00073 0.00003 0.00004 0.00002 0.00000 0.00028 0.00029 0.00025 0.00017 0.00016 0.00019 0.00018 N1 0.53206 -0.06940 0.32441 1.00000 0.02050 0.02356 0.01327 0.00182 -0.00016 0.00670 0.01917 0.00251 0.00011 0.00015 0.00006 0.00000 0.00081 0.00089 0.00069 0.00060 0.00058 0.00067 0.00036 N2 0.58695 -0.13013 0.37203 1.00000 0.02017 0.02277 0.01459 0.00039 -0.00422 0.00733 0.01942 0.00238 0.00010 0.00014 0.00005 0.00000 0.00077 0.00086 0.00068 0.00057 0.00053 0.00064 0.00035 O1 0.36349 -0.06334 0.37163 1.00000 0.02163 0.02821 0.02717 -0.00270 0.00350 -0.00014 0.02559 0.00208 0.00009 0.00012 0.00005 0.00000 0.00068 0.00078 0.00066 0.00054 0.00050 0.00057 0.00032 O2 0.39592 0.06968 0.28698 1.00000 0.02835 0.03034 0.01928 -0.00130 -0.00614 0.01300 0.02633 0.00215 0.00009 0.00013 0.00005 0.00000 0.00070 0.00080 0.00061 0.00052 0.00049 0.00060 0.00033 C1 0.64528 0.38228 0.50715 1.00000 0.05492 0.03924 0.04286 -0.01060 -0.00349 -0.01442 0.04597 0.00388 0.00023 0.00026 0.00011 0.00000 0.00161 0.00150 0.00132 0.00112 0.00116 0.00130 0.00061 C2 0.58623 0.29496 0.46560 1.00000 0.03418 0.02295 0.02967 -0.00273 -0.00191 0.00108 0.02911 0.00324 0.00015 0.00019 0.00008 0.00000 0.00110 0.00111 0.00099 0.00079 0.00079 0.00087 0.00046 C3 0.52525 0.20004 0.48614 1.00000 0.03177 0.02773 0.01749 -0.00302 0.00203 0.00338 0.02564 0.00321 0.00014 0.00018 0.00008 0.00000 0.00104 0.00112 0.00088 0.00077 0.00071 0.00085 0.00044 C4 0.47310 0.11720 0.44827 1.00000 0.02294 0.02205 0.02214 0.00073 0.00338 0.00394 0.02229 0.00323 0.00014 0.00018 0.00007 0.00000 0.00095 0.00105 0.00088 0.00075 0.00069 0.00083 0.00041 C5 0.48182 0.12978 0.38905 1.00000 0.01991 0.02078 0.01884 -0.00011 0.00002 0.00725 0.01990 0.00297 0.00013 0.00017 0.00007 0.00000 0.00089 0.00102 0.00082 0.00070 0.00063 0.00077 0.00040 C6 0.54001 0.22621 0.36772 1.00000 0.04089 0.03320 0.01975 0.00441 0.00228 -0.00321 0.03127 0.00343 0.00015 0.00020 0.00008 0.00000 0.00116 0.00122 0.00092 0.00081 0.00078 0.00097 0.00047 C7 0.59203 0.30750 0.40585 1.00000 0.04588 0.02704 0.03524 0.00556 0.00323 -0.01093 0.03603 0.00368 0.00017 0.00021 0.00008 0.00000 0.00128 0.00121 0.00111 0.00089 0.00091 0.00103 0.00052 C8 0.68679 -0.06908 0.39223 1.00000 0.02070 0.02236 0.02051 -0.00239 -0.00313 0.00263 0.02139 0.00306 0.00013 0.00018 0.00007 0.00000 0.00094 0.00107 0.00085 0.00074 0.00067 0.00080 0.00041 C9 0.72957 -0.16644 0.43597 1.00000 0.02444 0.03198 0.01764 0.00067 -0.00369 0.00605 0.02491 0.00323 0.00015 0.00019 0.00007 0.00000 0.00103 0.00116 0.00088 0.00077 0.00071 0.00085 0.00044 C10 0.69300 -0.29103 0.40801 1.00000 0.02782 0.02714 0.02262 0.00319 -0.00293 0.00753 0.02606 0.00328 0.00015 0.00019 0.00008 0.00000 0.00105 0.00114 0.00094 0.00079 0.00077 0.00091 0.00045 C11 0.62103 -0.25655 0.35427 1.00000 0.02244 0.02117 0.02061 -0.00050 -0.00244 0.00774 0.02158 0.00305 0.00013 0.00017 0.00007 0.00000 0.00093 0.00100 0.00086 0.00071 0.00067 0.00077 0.00041 C12 0.68281 -0.24522 0.29947 1.00000 0.02676 0.02884 0.02004 -0.00311 -0.00130 0.01093 0.02534 0.00331 0.00014 0.00019 0.00007 0.00000 0.00102 0.00115 0.00088 0.00076 0.00074 0.00088 0.00044 C13 0.75725 -0.13684 0.30088 1.00000 0.02135 0.03511 0.02296 0.00811 0.00082 0.01223 0.02651 0.00342 0.00014 0.00019 0.00007 0.00000 0.00094 0.00119 0.00089 0.00081 0.00068 0.00085 0.00045 C14 0.75796 -0.05402 0.34356 1.00000 0.02026 0.02945 0.02642 0.00646 -0.00165 0.00235 0.02552 0.00350 0.00015 0.00019 0.00007 0.00000 0.00096 0.00115 0.00095 0.00082 0.00072 0.00089 0.00044 C15 0.82754 -0.12699 0.25181 1.00000 0.03611 0.05257 0.03012 0.01007 0.01137 0.01469 0.03919 0.00485 0.00018 0.00027 0.00009 0.00000 0.00123 0.00165 0.00111 0.00103 0.00091 0.00121 0.00056 C16 0.52886 -0.34237 0.34442 1.00000 0.03196 0.02551 0.03042 -0.00033 -0.00375 0.00269 0.02955 0.00349 0.00016 0.00020 0.00009 0.00000 0.00112 0.00119 0.00106 0.00086 0.00086 0.00092 0.00046 H1A 0.70233 0.40989 0.49068 1.00000 0.05727 0.04473 0.00199 0.00266 0.00100 0.00000 0.00783 H1B 0.59833 0.44748 0.52125 1.00000 0.07563 0.05199 0.00235 0.00314 0.00114 0.00000 0.00900 H1C 0.66997 0.33903 0.54512 1.00000 0.07143 0.04784 0.00206 0.00264 0.00122 0.00000 0.00816 H1N 0.56713 -0.03094 0.30117 1.00000 0.03357 0.03797 0.00167 0.00209 0.00093 0.00000 0.00610 H3 0.51718 0.18851 0.52522 1.00000 0.02946 0.03450 0.00142 0.00192 0.00087 0.00000 0.00512 H4 0.43088 0.04892 0.46237 1.00000 0.02029 0.03264 0.00142 0.00189 0.00072 0.00000 0.00457 H6 0.54653 0.23411 0.32798 1.00000 0.03436 0.03585 0.00146 0.00205 0.00089 0.00000 0.00538 H7 0.63739 0.36904 0.39198 1.00000 0.05739 0.04367 0.00191 0.00252 0.00097 0.00000 0.00719 H8 0.67191 0.01194 0.40945 1.00000 0.01454 0.03121 0.00131 0.00180 0.00071 0.00000 0.00427 H9A 0.80697 -0.16441 0.44084 1.00000 0.01926 0.03152 0.00145 0.00171 0.00068 0.00000 0.00447 H9B 0.69999 -0.15292 0.47244 1.00000 0.02587 0.03256 0.00136 0.00180 0.00085 0.00000 0.00483 H10A 0.65251 -0.33882 0.43537 1.00000 0.03669 0.03560 0.00158 0.00207 0.00088 0.00000 0.00555 H10B 0.75306 -0.34379 0.39812 1.00000 0.02676 0.03245 0.00147 0.00190 0.00074 0.00000 0.00493 H12A 0.71987 -0.32075 0.29240 1.00000 0.04069 0.03772 0.00164 0.00225 0.00085 0.00000 0.00591 H12B 0.63556 -0.23482 0.26505 1.00000 0.03410 0.03644 0.00151 0.00202 0.00088 0.00000 0.00523 H14 0.80688 0.01013 0.34211 1.00000 0.02495 0.03517 0.00154 0.00188 0.00078 0.00000 0.00510 H15A 0.78756 -0.12707 0.21430 1.00000 0.04266 0.04063 0.00168 0.00214 0.00096 0.00000 0.00587 H15B 0.87516 -0.20089 0.25264 1.00000 0.06070 0.04268 0.00197 0.00264 0.00099 0.00000 0.00752 H15C 0.87122 -0.04555 0.25559 1.00000 0.05477 0.04695 0.00199 0.00264 0.00094 0.00000 0.00730 H16A 0.55416 -0.42278 0.33255 1.00000 0.04006 0.03813 0.00170 0.00234 0.00084 0.00000 0.00590 H16B 0.48032 -0.30859 0.31089 1.00000 0.03944 0.03663 0.00156 0.00203 0.00088 0.00000 0.00569 H16C 0.49116 -0.34855 0.37908 1.00000 0.03121 0.03385 0.00150 0.00189 0.00087 0.00000 0.00530 Final Structure Factor Calculation for 01sot057 in C2/c Total number of l.s. parameters = 279 Maximum vector length = 511 Memory required = 2489 / 24017 wR2 = 0.0986 before cycle 5 for 2784 data and 0 / 279 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0493 * P )^2 + 0.78 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0376 for 2307 Fo > 4sig(Fo) and 0.0492 for all 2784 data wR2 = 0.0986, GooF = S = 1.055, Restrained GooF = 1.055 for all data Occupancy sum of asymmetric unit = 21.00 for non-hydrogen and 22.00 for hydrogen atoms Principal mean square atomic displacements U 0.0288 0.0165 0.0141 S1 0.0289 0.0165 0.0121 N1 0.0299 0.0183 0.0101 N2 0.0306 0.0254 0.0208 O1 0.0445 0.0216 0.0129 O2 0.0636 0.0508 0.0236 C1 0.0372 0.0281 0.0220 C2 0.0339 0.0266 0.0164 C3 0.0270 0.0216 0.0183 C4 0.0278 0.0189 0.0130 C5 0.0422 0.0333 0.0183 C6 0.0513 0.0370 0.0198 C7 0.0279 0.0199 0.0164 C8 0.0357 0.0245 0.0145 C9 0.0353 0.0269 0.0160 C10 0.0309 0.0203 0.0135 C11 0.0400 0.0192 0.0168 C12 0.0440 0.0231 0.0123 C13 0.0346 0.0249 0.0171 C14 0.0654 0.0294 0.0228 C15 0.0379 0.0268 0.0239 C16 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.031 0.048 0.065 0.084 0.106 0.131 0.172 0.235 1.000 Number in group 293. 264. 284. 286. 266. 283. 275. 275. 279. 279. GooF 0.896 1.167 1.137 0.997 1.139 1.083 1.035 1.028 0.957 1.097 K 1.952 1.043 0.987 0.986 0.989 0.990 0.996 1.011 1.011 1.013 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.25 1.43 1.80 inf Number in group 286. 272. 287. 276. 276. 275. 276. 279. 278. 279. GooF 0.834 0.883 0.893 0.983 1.021 1.014 0.896 0.946 1.248 1.604 K 1.006 1.010 1.024 1.009 1.011 1.018 1.015 1.018 1.012 1.003 R1 0.101 0.089 0.069 0.060 0.054 0.041 0.032 0.030 0.041 0.038 Recommended weighting scheme: WGHT 0.0473 0.9411 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 1 6 7200.97 10641.56 6.40 0.399 3.43 -3 3 2 146.53 20.80 6.17 0.018 2.70 -2 0 14 125.84 35.36 4.31 0.023 1.62 2 2 6 65.28 112.38 4.14 0.041 2.75 5 5 15 263.11 453.75 4.14 0.082 1.10 4 2 4 90.96 45.91 4.14 0.026 2.43 -7 3 3 149.55 91.79 3.87 0.037 1.62 5 1 4 26.43 3.87 3.71 0.008 2.24 4 2 10 3342.57 2741.91 3.59 0.202 1.72 1 1 11 1633.12 1307.75 3.52 0.140 2.01 -2 4 4 55.97 1.68 3.50 0.005 2.30 0 6 5 627.09 443.57 3.49 0.081 1.67 -3 5 4 2815.72 3562.09 3.44 0.231 1.84 2 2 0 428.43 555.52 3.33 0.091 4.12 -1 1 10 87.70 138.96 3.28 0.046 2.25 3 7 19 468.93 651.06 3.21 0.099 0.92 1 5 0 759.41 550.26 3.20 0.091 2.12 -5 1 21 194.27 286.55 3.20 0.065 1.03 1 5 11 93.84 44.41 3.13 0.026 1.48 3 7 14 2257.18 1835.88 3.13 0.166 1.07 1 1 8 95.65 146.70 3.09 0.047 2.69 1 3 6 852.12 1046.52 3.07 0.125 2.54 1 3 7 849.18 673.65 3.06 0.100 2.36 1 7 16 65.77 24.34 3.04 0.019 1.04 -2 0 2 2336.44 2780.26 3.00 0.204 5.77 -2 6 3 -3.47 32.56 3.00 0.022 1.69 -8 0 16 1007.80 794.46 2.96 0.109 1.11 -9 1 19 329.39 457.74 2.86 0.083 0.95 -5 7 7 734.67 550.52 2.83 0.091 1.24 -2 2 10 1251.03 1047.16 2.79 0.125 2.05 3 1 0 7528.25 9243.34 2.76 0.372 3.97 -7 7 11 519.35 393.65 2.76 0.077 1.05 3 3 14 1278.15 1522.17 2.76 0.151 1.39 5 5 21 552.23 730.34 2.74 0.104 0.90 2 10 15 35.07 111.98 2.74 0.041 0.87 -10 6 15 198.82 89.46 2.70 0.037 0.89 -11 5 1 137.21 49.57 2.68 0.027 1.03 -4 2 2 5766.49 6769.45 2.68 0.318 2.71 5 1 9 3005.00 2582.36 2.66 0.196 1.73 4 4 0 4961.35 4249.00 2.59 0.252 2.06 -1 5 4 566.82 454.07 2.58 0.082 2.00 3 5 4 1410.57 1177.72 2.56 0.133 1.80 -1 3 7 485.77 396.29 2.56 0.077 2.40 2 4 0 891.34 1117.73 2.55 0.129 2.48 3 1 1 1583.18 1886.69 2.55 0.168 3.88 4 0 4 149.03 103.74 2.55 0.039 2.73 3 1 10 35.95 18.98 2.54 0.017 1.94 3 1 6 615.01 728.75 2.54 0.104 2.68 2 0 8 9.11 29.72 2.51 0.021 2.57 -1 5 2 1789.87 1495.68 2.51 0.150 2.09 Bond lengths and angles S1 - Distance Angles O1 1.4270 (0.0013) O2 1.4388 (0.0012) 119.85 (0.08) N1 1.6301 (0.0015) 109.00 (0.08) 103.74 (0.07) C5 1.7622 (0.0017) 108.01 (0.08) 109.35 (0.08) 106.06 (0.08) S1 - O1 O2 N1 N1 - Distance Angles N2 1.4254 (0.0018) S1 1.6301 (0.0015) 115.11 (0.11) N1 - N2 N2 - Distance Angles N1 1.4254 (0.0018) C8 1.4886 (0.0022) 114.40 (0.14) C11 1.4924 (0.0023) 110.07 (0.12) 102.94 (0.13) N2 - N1 C8 O1 - Distance Angles S1 1.4270 (0.0013) O1 - O2 - Distance Angles S1 1.4388 (0.0012) O2 - C1 - Distance Angles C2 1.5103 (0.0027) C1 - C2 - Distance Angles C3 1.3887 (0.0027) C7 1.3945 (0.0027) 118.55 (0.17) C1 1.5103 (0.0027) 120.64 (0.18) 120.80 (0.19) C2 - C3 C7 C3 - Distance Angles C2 1.3887 (0.0028) C4 1.3889 (0.0026) 120.97 (0.16) C3 - C2 C4 - Distance Angles C5 1.3873 (0.0023) C3 1.3889 (0.0026) 119.48 (0.18) C4 - C5 C5 - Distance Angles C6 1.3871 (0.0027) C4 1.3873 (0.0023) 120.28 (0.16) S1 1.7622 (0.0017) 119.21 (0.13) 120.10 (0.14) C5 - C6 C4 C6 - Distance Angles C7 1.3811 (0.0028) C5 1.3871 (0.0027) 119.66 (0.17) C6 - C7 C7 - Distance Angles C6 1.3811 (0.0028) C2 1.3945 (0.0027) 121.02 (0.19) C7 - C6 C8 - Distance Angles N2 1.4886 (0.0022) C14 1.5052 (0.0026) 111.57 (0.14) C9 1.5310 (0.0024) 99.84 (0.14) 110.93 (0.15) C8 - N2 C14 C9 - Distance Angles C8 1.5310 (0.0024) C10 1.5455 (0.0027) 103.24 (0.13) C9 - C8 C10 - Distance Angles C11 1.5438 (0.0022) C9 1.5455 (0.0027) 106.16 (0.15) C10 - C11 C11 - Distance Angles N2 1.4924 (0.0023) C16 1.5067 (0.0027) 110.82 (0.15) C10 1.5438 (0.0022) 99.68 (0.13) 113.47 (0.16) C12 1.5439 (0.0025) 109.30 (0.15) 111.52 (0.15) 111.42 (0.15) C11 - N2 C16 C10 C12 - Distance Angles C13 1.5058 (0.0028) C11 1.5439 (0.0025) 113.84 (0.15) C12 - C13 C13 - Distance Angles C14 1.3278 (0.0027) C15 1.5001 (0.0026) 122.66 (0.21) C12 1.5058 (0.0028) 120.44 (0.17) 116.89 (0.18) C13 - C14 C15 C14 - Distance Angles C13 1.3278 (0.0027) C8 1.5052 (0.0026) 120.58 (0.19) C14 - C13 C15 - Distance Angles C13 1.5001 (0.0026) C15 - C16 - Distance Angles C11 1.5067 (0.0027) C16 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.83(2) 2.38(2) 3.167(2) 157.4(19) N1-H1N...O2_$1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)