+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + ssf1338 started at 12:36:20 on 23-Jan-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL ssf1338 in P-1 CELL 0.69050 5.5097 9.5290 13.0300 104.839 91.938 95.093 ZERR 2.00 0.0015 0.0020 0.0030 0.003 0.003 0.003 LATT 1 SFAC C H N O UNIT 20 36 8 12 V = 657.54 F(000) = 308.0 Mu = 0.12 mm-1 Cell Wt = 580.57 Rho = 1.466 MERG 2 SHEL 7 0.77 EQIV_$1 -x+1, -y, -z+1 HTAB O1A O22_$1 HTAB N21 O1B_$1 EQIV_$2 -x-1, -y+1, -z+2 HTAB O31A O42_$2 HTAB N41 O31B_$2 EQIV_$3 -x+1, -y+1, -z+1 HTAB N23 O31B_$3 EQIV_$4 -x, -y+1, -z+2 HTAB N43 O1B_$4 EQIV_$5 -x+1, -y+1, -z+1 MPLA C31 O31A O31B MPLA C31_$5 O31A_$5 O31B_$5 FMAP 2 PLAN 10 SIZE 0.04 0.08 0.12 ACTA BOND $H WGHT 0.08450 0.30350 L.S. 4 TEMP -153.00 FVAR 0.72143 MOLE 1 C1 1 0.095992 0.322376 0.909495 11.00000 0.01899 0.01553 = 0.01780 0.00335 0.00505 0.00200 C2 1 -0.054006 0.421327 0.984615 11.00000 0.01673 0.01677 = 0.02132 0.00329 0.00740 0.00162 AFIX 23 H2A 2 -0.070195 0.386784 1.049770 11.00000 -1.20000 H2B 2 -0.219731 0.415317 0.950960 11.00000 -1.20000 AFIX 0 O1A 4 0.021178 0.184379 0.895709 11.00000 0.02638 0.01466 = 0.02682 0.00149 0.01272 0.00006 AFIX 147 H1 2 0.109119 0.133134 0.852861 11.00000 -1.50000 AFIX 0 O1B 4 0.269338 0.365342 0.865367 11.00000 0.02593 0.01722 = 0.03153 0.00313 0.01692 0.00097 MOLE 2 C22 1 0.597038 -0.016627 0.292758 11.00000 0.01980 0.01579 = 0.02122 0.00403 0.00211 0.00326 C24 1 0.280604 0.043341 0.403664 11.00000 0.02125 0.01849 = 0.02376 0.00406 0.00701 0.00058 AFIX 23 H24A 2 0.143275 0.082347 0.372654 11.00000 -1.20000 H24B 2 0.278901 0.073460 0.482190 11.00000 -1.20000 AFIX 0 C25 1 0.268057 -0.123730 0.361966 11.00000 0.02404 0.01916 = 0.02428 0.00539 0.00540 0.00059 AFIX 23 H25A 2 0.302641 -0.169965 0.420092 11.00000 -1.20000 H25B 2 0.106271 -0.165293 0.326569 11.00000 -1.20000 AFIX 0 N21 3 0.458936 -0.141980 0.286250 11.00000 0.02800 0.01513 = 0.03724 -0.00056 0.01335 0.00063 AFIX 43 H21 2 0.480932 -0.225631 0.241452 11.00000 -1.20000 AFIX 0 N23 3 0.513232 0.091665 0.367671 11.00000 0.02440 0.01462 = 0.02622 0.00141 0.01038 -0.00122 AFIX 43 H23 2 0.589415 0.179895 0.391565 11.00000 -1.20000 AFIX 0 O22 4 0.775320 0.001999 0.239434 11.00000 0.02392 0.01939 = 0.02671 0.00326 0.01019 0.00334 MOLE 3 C31 1 0.236261 0.500940 0.593711 11.00000 0.01712 0.01699 = 0.01908 0.00376 0.00576 0.00103 C32 1 0.409889 0.441647 0.510722 11.00000 0.01854 0.01559 = 0.02013 0.00175 0.00820 0.00126 AFIX 23 H32A 2 0.314985 0.390367 0.443696 11.00000 -1.20000 H32B 2 0.500869 0.369286 0.534262 11.00000 -1.20000 AFIX 0 O31A 4 0.067435 0.400809 0.604326 11.00000 0.03239 0.01866 = 0.03388 -0.00183 0.02149 -0.00510 AFIX 147 H31 2 -0.020454 0.436926 0.653803 11.00000 -1.50000 AFIX 0 O31B 4 0.249743 0.628190 0.645503 11.00000 0.02392 0.01684 = 0.02753 -0.00057 0.01347 0.00029 MOLE 4 C42 1 -0.720384 0.398263 1.208420 11.00000 0.01623 0.01994 = 0.01846 0.00481 0.00500 0.00113 C44 1 -0.536331 0.212105 1.099300 11.00000 0.02116 0.01796 = 0.02355 0.00375 0.00859 0.00269 AFIX 23 H44A 2 -0.389207 0.189927 1.135519 11.00000 -1.20000 H44B 2 -0.527369 0.175102 1.021405 11.00000 -1.20000 AFIX 0 C45 1 -0.771188 0.148089 1.137883 11.00000 0.02216 0.01880 = 0.02215 0.00417 0.00604 0.00149 AFIX 23 H45A 2 -0.901616 0.117485 1.080216 11.00000 -1.20000 H45B 2 -0.741568 0.064028 1.166548 11.00000 -1.20000 AFIX 0 N41 3 -0.831772 0.272671 1.221571 11.00000 0.02180 0.01914 = 0.02220 0.00484 0.01040 -0.00041 AFIX 43 H41 2 -0.927527 0.266517 1.273273 11.00000 -1.20000 AFIX 0 N43 3 -0.563941 0.367601 1.129530 11.00000 0.02153 0.01615 = 0.02296 0.00544 0.01048 0.00251 AFIX 43 H43 2 -0.489661 0.432409 1.100695 11.00000 -1.20000 AFIX 0 O42 4 -0.753817 0.524705 1.258506 11.00000 0.02370 0.01872 = 0.02672 0.00245 0.01242 0.00208 HKLF 4 Covalent radii and connectivity table for ssf1338 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - C1 C2_$4 O1A - C1 O1B - C1 C22 - O22 N21 N23 C24 - N23 C25 C25 - N21 C24 N21 - C22 C25 N23 - C22 C24 O22 - C22 C31 - O31B O31A C32 C32 - C31 C32_$3 O31A - C31 O31B - C31 C42 - O42 N41 N43 C44 - N43 C45 C45 - N41 C44 N41 - C42 C45 N43 - C42 C44 O42 - C42 Operators for generating equivalent atoms: $1 -x+1, -y, -z+1 $2 -x-1, -y+1, -z+2 $3 -x+1, -y+1, -z+1 $4 -x, -y+1, -z+2 $5 -x+1, -y+1, -z+1 6671 Reflections read, of which 977 rejected -7 =< h =< 7, -12 =< k =< 12, -16 =< l =< 16, Max. 2-theta = 53.27 0 Systematic absence violations 0 Inconsistent equivalents 2909 Unique reflections, of which 0 suppressed R(int) = 0.0277 R(sigma) = 0.0424 Friedel opposites merged Maximum memory for data reduction = 2339 / 29221 Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 2870 / 227223 wR2 = 0.1485 before cycle 1 for 2909 data and 183 / 183 parameters GooF = S = 1.034; Restrained GooF = 1.034 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0845 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72144 0.00245 0.003 OSF Mean shift/esd = 0.003 Maximum = 0.008 for U12 O1B Max. shift = 0.000 A for H31 Max. dU = 0.000 for C25 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2870 / 227223 wR2 = 0.1485 before cycle 2 for 2909 data and 183 / 183 parameters GooF = S = 1.034; Restrained GooF = 1.034 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0845 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72144 0.00245 -0.001 OSF Mean shift/esd = 0.001 Maximum = -0.002 for U23 O31A Max. shift = 0.000 A for H31 Max. dU = 0.000 for C25 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2870 / 227223 wR2 = 0.1485 before cycle 3 for 2909 data and 183 / 183 parameters GooF = S = 1.034; Restrained GooF = 1.034 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0845 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72144 0.00245 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z N43 Max. shift = 0.000 A for H31 Max. dU = 0.000 for O1A Least-squares cycle 4 Maximum vector length = 511 Memory required = 2870 / 227223 wR2 = 0.1485 before cycle 4 for 2909 data and 183 / 183 parameters GooF = S = 1.034; Restrained GooF = 1.034 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0845 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72144 0.00245 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z N41 Max. shift = 0.000 A for H1 Max. dU = 0.000 for O31A No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A -0.0702 0.3868 1.0498 23 0.990 0.000 C2 C1 C2_$4 H2B -0.2197 0.4153 0.9510 23 0.990 0.000 C2 C1 C2_$4 H1 0.1091 0.1331 0.8529 147 0.840 0.000 O1A C1 H1 H24A 0.1433 0.0823 0.3727 23 0.990 0.000 C24 N23 C25 H24B 0.2789 0.0735 0.4822 23 0.990 0.000 C24 N23 C25 H25A 0.3026 -0.1700 0.4201 23 0.990 0.000 C25 N21 C24 H25B 0.1063 -0.1653 0.3266 23 0.990 0.000 C25 N21 C24 H21 0.4809 -0.2256 0.2415 43 0.880 0.000 N21 C22 C25 H23 0.5894 0.1799 0.3916 43 0.880 0.000 N23 C22 C24 H32A 0.3150 0.3904 0.4437 23 0.990 0.000 C32 C31 C32_$3 H32B 0.5009 0.3693 0.5343 23 0.990 0.000 C32 C31 C32_$3 H31 -0.0205 0.4369 0.6538 147 0.840 0.000 O31A C31 H31 H44A -0.3892 0.1899 1.1355 23 0.990 0.000 C44 N43 C45 H44B -0.5274 0.1751 1.0214 23 0.990 0.000 C44 N43 C45 H45A -0.9016 0.1175 1.0802 23 0.990 0.000 C45 N41 C44 H45B -0.7416 0.0640 1.1665 23 0.990 0.000 C45 N41 C44 H41 -0.9275 0.2665 1.2733 43 0.880 0.000 N41 C42 C45 H43 -0.4897 0.4324 1.1007 43 0.880 0.000 N43 C42 C44 ssf1338 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.09599 0.32238 0.90949 1.00000 0.01899 0.01553 0.01780 0.00335 0.00505 0.00200 0.01751 0.00324 0.00030 0.00017 0.00013 0.00000 0.00078 0.00075 0.00074 0.00059 0.00059 0.00060 0.00034 C2 -0.05401 0.42133 0.98461 1.00000 0.01673 0.01677 0.02132 0.00329 0.00740 0.00162 0.01844 0.00323 0.00029 0.00017 0.00013 0.00000 0.00076 0.00082 0.00078 0.00061 0.00059 0.00061 0.00035 H2A -0.07020 0.38678 1.04977 1.00000 0.02212 0.00000 0.00000 H2B -0.21973 0.41532 0.95096 1.00000 0.02212 0.00000 0.00000 O1A 0.02118 0.18438 0.89571 1.00000 0.02638 0.01466 0.02682 0.00149 0.01272 0.00006 0.02320 0.00247 0.00023 0.00013 0.00010 0.00000 0.00065 0.00058 0.00065 0.00047 0.00050 0.00047 0.00030 H1 0.10912 0.13313 0.85286 1.00000 0.03481 0.00000 0.00000 O1B 0.26934 0.36534 0.86537 1.00000 0.02594 0.01723 0.03153 0.00313 0.01692 0.00097 0.02520 0.00258 0.00023 0.00013 0.00010 0.00000 0.00066 0.00061 0.00069 0.00050 0.00052 0.00050 0.00031 C22 0.59704 -0.01663 0.29276 1.00000 0.01980 0.01579 0.02122 0.00403 0.00211 0.00326 0.01897 0.00336 0.00031 0.00018 0.00013 0.00000 0.00079 0.00075 0.00078 0.00060 0.00061 0.00061 0.00035 C24 0.28060 0.04334 0.40366 1.00000 0.02125 0.01849 0.02376 0.00406 0.00701 0.00058 0.02139 0.00347 0.00031 0.00019 0.00014 0.00000 0.00084 0.00081 0.00083 0.00065 0.00064 0.00064 0.00037 H24A 0.14327 0.08235 0.37266 1.00000 0.02567 0.00000 0.00000 H24B 0.27890 0.07346 0.48219 1.00000 0.02567 0.00000 0.00000 C25 0.26806 -0.12373 0.36197 1.00000 0.02404 0.01916 0.02428 0.00539 0.00540 0.00059 0.02254 0.00356 0.00033 0.00019 0.00014 0.00000 0.00087 0.00082 0.00084 0.00065 0.00067 0.00066 0.00037 H25A 0.30264 -0.16997 0.42009 1.00000 0.02705 0.00000 0.00000 H25B 0.10627 -0.16529 0.32657 1.00000 0.02705 0.00000 0.00000 N21 0.45894 -0.14198 0.28625 1.00000 0.02800 0.01513 0.03724 -0.00056 0.01336 0.00063 0.02797 0.00325 0.00029 0.00017 0.00013 0.00000 0.00082 0.00070 0.00088 0.00061 0.00067 0.00059 0.00038 H21 0.48093 -0.22563 0.24145 1.00000 0.03357 0.00000 0.00000 N23 0.51323 0.09166 0.36767 1.00000 0.02440 0.01462 0.02622 0.00141 0.01038 -0.00122 0.02245 0.00301 0.00027 0.00016 0.00012 0.00000 0.00076 0.00068 0.00074 0.00056 0.00058 0.00056 0.00034 H23 0.58941 0.17990 0.39156 1.00000 0.02694 0.00000 0.00000 O22 0.77532 0.00200 0.23943 1.00000 0.02392 0.01939 0.02671 0.00326 0.01019 0.00334 0.02357 0.00248 0.00022 0.00013 0.00010 0.00000 0.00065 0.00062 0.00065 0.00049 0.00050 0.00049 0.00030 C31 0.23626 0.50094 0.59371 1.00000 0.01712 0.01699 0.01908 0.00376 0.00576 0.00103 0.01783 0.00324 0.00029 0.00017 0.00013 0.00000 0.00077 0.00077 0.00076 0.00061 0.00059 0.00060 0.00035 C32 0.40989 0.44165 0.51072 1.00000 0.01854 0.01559 0.02013 0.00175 0.00820 0.00126 0.01848 0.00327 0.00029 0.00017 0.00013 0.00000 0.00079 0.00074 0.00076 0.00059 0.00060 0.00061 0.00035 H32A 0.31499 0.39037 0.44370 1.00000 0.02218 0.00000 0.00000 H32B 0.50087 0.36929 0.53426 1.00000 0.02218 0.00000 0.00000 O31A 0.06744 0.40081 0.60433 1.00000 0.03239 0.01866 0.03388 -0.00183 0.02149 -0.00510 0.02992 0.00272 0.00025 0.00014 0.00011 0.00000 0.00073 0.00062 0.00073 0.00052 0.00057 0.00052 0.00034 H31 -0.02046 0.43693 0.65380 1.00000 0.04488 0.00000 0.00000 O31B 0.24974 0.62819 0.64550 1.00000 0.02392 0.01684 0.02753 -0.00057 0.01347 0.00029 0.02376 0.00246 0.00022 0.00013 0.00010 0.00000 0.00065 0.00060 0.00065 0.00048 0.00050 0.00048 0.00030 C42 -0.72038 0.39826 1.20842 1.00000 0.01623 0.01994 0.01846 0.00481 0.00500 0.00113 0.01819 0.00332 0.00029 0.00018 0.00013 0.00000 0.00075 0.00080 0.00076 0.00061 0.00059 0.00060 0.00034 C44 -0.53633 0.21210 1.09930 1.00000 0.02115 0.01796 0.02355 0.00375 0.00859 0.00270 0.02098 0.00355 0.00032 0.00019 0.00014 0.00000 0.00083 0.00078 0.00081 0.00062 0.00064 0.00063 0.00036 H44A -0.38921 0.18993 1.13552 1.00000 0.02518 0.00000 0.00000 H44B -0.52737 0.17510 1.02140 1.00000 0.02518 0.00000 0.00000 C45 -0.77119 0.14809 1.13788 1.00000 0.02216 0.01880 0.02215 0.00417 0.00604 0.00150 0.02117 0.00344 0.00032 0.00018 0.00013 0.00000 0.00084 0.00080 0.00082 0.00064 0.00064 0.00065 0.00037 H45A -0.90162 0.11748 1.08022 1.00000 0.02541 0.00000 0.00000 H45B -0.74157 0.06403 1.16655 1.00000 0.02541 0.00000 0.00000 N41 -0.83177 0.27267 1.22157 1.00000 0.02180 0.01914 0.02220 0.00484 0.01040 -0.00041 0.02109 0.00291 0.00026 0.00016 0.00011 0.00000 0.00072 0.00070 0.00070 0.00055 0.00055 0.00055 0.00033 H41 -0.92753 0.26652 1.27327 1.00000 0.02530 0.00000 0.00000 N43 -0.56394 0.36760 1.12953 1.00000 0.02153 0.01615 0.02296 0.00544 0.01048 0.00251 0.01990 0.00293 0.00026 0.00015 0.00011 0.00000 0.00072 0.00068 0.00072 0.00054 0.00056 0.00054 0.00033 H43 -0.48966 0.43241 1.10070 1.00000 0.02388 0.00000 0.00000 O42 -0.75382 0.52470 1.25851 1.00000 0.02370 0.01872 0.02672 0.00245 0.01242 0.00208 0.02343 0.00247 0.00022 0.00013 0.00010 0.00000 0.00065 0.00060 0.00065 0.00048 0.00050 0.00049 0.00030 Final Structure Factor Calculation for ssf1338 in P-1 Total number of l.s. parameters = 183 Maximum vector length = 511 Memory required = 2687 / 22995 wR2 = 0.1485 before cycle 5 for 2909 data and 0 / 183 parameters GooF = S = 1.034; Restrained GooF = 1.034 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0845 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0507 for 2337 Fo > 4sig(Fo) and 0.0626 for all 2909 data wR2 = 0.1485, GooF = S = 1.034, Restrained GooF = 1.034 for all data Occupancy sum of asymmetric unit = 20.00 for non-hydrogen and 18.00 for hydrogen atoms Principal mean square atomic displacements U 0.0227 0.0160 0.0139 C1 0.0266 0.0167 0.0119 C2 0.0403 0.0153 0.0140 O1A 0.0462 0.0172 0.0123 O1B 0.0218 0.0200 0.0151 C22 0.0296 0.0184 0.0161 C24 0.0289 0.0207 0.0181 C25 0.0495 0.0203 0.0141 N21 0.0376 0.0158 0.0140 N23 0.0350 0.0206 0.0151 O22 0.0237 0.0169 0.0130 C31 0.0282 0.0157 0.0116 C32 0.0611 0.0165 0.0121 O31A 0.0421 0.0170 0.0121 O31B 0.0221 0.0196 0.0128 C42 0.0302 0.0184 0.0143 C44 0.0276 0.0188 0.0171 C45 0.0325 0.0193 0.0115 N41 0.0313 0.0160 0.0124 N43 0.0380 0.0191 0.0132 O42 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.020 0.041 0.063 0.090 0.117 0.149 0.190 0.255 0.370 1.000 Number in group 312. 278. 295. 282. 294. 284. 300. 281. 290. 293. GooF 0.936 1.022 1.011 1.153 1.033 1.033 1.079 0.970 1.022 1.076 K 0.979 0.972 1.013 1.077 1.037 1.009 0.993 1.002 1.006 1.018 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.14 1.29 1.58 inf Number in group 291. 296. 295. 289. 283. 297. 286. 288. 291. 293. GooF 0.893 0.821 0.864 0.868 0.914 0.919 0.916 1.029 1.269 1.591 K 1.039 1.028 1.014 1.006 0.980 0.995 0.998 1.006 1.034 1.026 R1 0.097 0.090 0.076 0.071 0.065 0.055 0.044 0.051 0.054 0.062 Recommended weighting scheme: WGHT 0.0845 0.3035 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) -2 2 4 476.23 278.75 6.11 0.401 1.86 0 1 1 148.50 249.06 4.88 0.379 6.63 0 -5 6 5.77 0.71 4.41 0.020 1.60 -1 0 7 19.47 8.46 4.36 0.070 1.74 2 2 3 8.02 1.38 4.28 0.028 1.85 -1 6 1 21.63 10.28 4.19 0.077 1.46 2 -5 4 49.84 30.45 3.98 0.133 1.55 2 3 2 4.48 0.33 3.74 0.014 1.76 1 -2 4 10.09 4.08 3.72 0.049 2.63 0 -3 6 68.52 104.25 3.71 0.245 1.99 -2 2 6 254.44 180.73 3.71 0.323 1.53 -1 -3 2 4.99 1.17 3.69 0.026 2.61 -4 -1 2 17.14 7.97 3.69 0.068 1.33 -1 0 6 131.01 91.14 3.64 0.229 2.00 2 -3 6 25.72 14.38 3.63 0.091 1.62 3 -3 3 83.44 56.65 3.58 0.181 1.58 -2 0 6 27.96 16.48 3.58 0.097 1.71 1 -4 3 25.34 41.79 3.54 0.155 2.15 -4 2 7 12.89 5.12 3.49 0.054 1.07 3 1 2 12.69 23.35 3.47 0.116 1.65 3 0 1 43.73 28.41 3.40 0.128 1.79 -2 4 9 18.47 9.69 3.38 0.075 1.03 2 0 6 15.12 7.71 3.26 0.067 1.62 -4 3 10 38.75 22.50 3.25 0.114 0.88 2 -1 7 22.17 12.47 3.25 0.085 1.51 -1 -1 3 245.59 180.78 3.23 0.323 3.38 -3 3 5 550.48 413.37 3.22 0.488 1.32 -1 -4 9 49.90 33.03 3.21 0.138 1.32 -3 1 10 22.40 12.37 3.14 0.084 1.04 -2 -3 5 4.07 0.65 3.14 0.019 1.72 1 3 8 13.50 6.98 3.07 0.063 1.21 2 -7 2 13.58 6.83 3.05 0.063 1.26 -5 5 9 93.86 65.37 2.95 0.194 0.77 2 9 1 15.09 7.96 2.90 0.068 0.91 2 -2 8 296.32 226.37 2.90 0.361 1.38 -5 -8 4 45.32 30.46 2.90 0.133 0.77 1 -4 9 29.53 44.18 2.90 0.160 1.32 2 2 11 10.21 4.43 2.89 0.051 0.95 -5 4 10 81.87 56.63 2.88 0.181 0.77 -3 1 7 943.99 740.84 2.81 0.654 1.29 -3 0 6 2.86 0.59 2.80 0.018 1.42 -1 2 6 8.77 4.38 2.68 0.050 1.70 4 0 5 3.52 0.57 2.64 0.018 1.17 -2 2 5 9.34 4.95 2.63 0.053 1.69 -3 1 0 0.33 2.80 2.62 0.040 1.83 -2 10 0 3.87 0.62 2.58 0.019 0.90 1 -6 7 13.20 7.70 2.57 0.067 1.32 2 -5 6 21.84 32.02 2.56 0.136 1.41 -4 3 11 165.85 125.85 2.56 0.269 0.84 -2 1 3 262.07 207.33 2.54 0.346 2.25 Bond lengths and angles C1 - Distance Angles O1B 1.2242 (0.0020) O1A 1.3073 (0.0020) 123.33 (0.14) C2 1.5002 (0.0021) 124.02 (0.15) 112.65 (0.13) C1 - O1B O1A C2 - Distance Angles C1 1.5002 (0.0021) C2_$4 1.5101 (0.0031) 113.23 (0.17) H2A 0.9900 108.93 108.93 H2B 0.9900 108.93 108.93 107.75 C2 - C1 C2_$4 H2A O1A - Distance Angles C1 1.3073 (0.0020) H1 0.8400 109.47 O1A - C1 O1B - Distance Angles C1 1.2242 (0.0020) O1B - C22 - Distance Angles O22 1.2480 (0.0021) N21 1.3399 (0.0023) 127.08 (0.16) N23 1.3528 (0.0021) 123.64 (0.16) 109.28 (0.15) C22 - O22 N21 C24 - Distance Angles N23 1.4564 (0.0022) C25 1.5393 (0.0024) 102.56 (0.13) H24A 0.9900 111.25 111.25 H24B 0.9900 111.25 111.25 109.16 C24 - N23 C25 H24A C25 - Distance Angles N21 1.4575 (0.0023) C24 1.5393 (0.0024) 102.31 (0.14) H25A 0.9900 111.31 111.31 H25B 0.9900 111.31 111.31 109.20 C25 - N21 C24 H25A N21 - Distance Angles C22 1.3399 (0.0023) C25 1.4575 (0.0023) 112.17 (0.14) H21 0.8800 123.91 123.91 N21 - C22 C25 N23 - Distance Angles C22 1.3528 (0.0021) C24 1.4564 (0.0022) 111.24 (0.14) H23 0.8800 124.38 124.38 N23 - C22 C24 O22 - Distance Angles C22 1.2480 (0.0021) O22 - C31 - Distance Angles O31B 1.2218 (0.0019) O31A 1.3090 (0.0020) 123.53 (0.15) C32 1.5022 (0.0021) 124.09 (0.15) 112.38 (0.13) C31 - O31B O31A C32 - Distance Angles C31 1.5022 (0.0021) C32_$3 1.5109 (0.0032) 113.14 (0.17) H32A 0.9900 108.95 108.95 H32B 0.9900 108.95 108.95 107.76 C32 - C31 C32_$3 H32A O31A - Distance Angles C31 1.3090 (0.0020) H31 0.8400 109.47 O31A - C31 O31B - Distance Angles C31 1.2218 (0.0019) O31B - C42 - Distance Angles O42 1.2475 (0.0020) N41 1.3491 (0.0022) 126.84 (0.15) N43 1.3549 (0.0021) 123.71 (0.16) 109.44 (0.14) C42 - O42 N41 C44 - Distance Angles N43 1.4556 (0.0022) C45 1.5363 (0.0023) 101.78 (0.13) H44A 0.9900 111.41 111.41 H44B 0.9900 111.41 111.41 109.27 C44 - N43 C45 H44A C45 - Distance Angles N41 1.4635 (0.0022) C44 1.5363 (0.0024) 101.42 (0.13) H45A 0.9900 111.49 111.49 H45B 0.9900 111.49 111.49 109.32 C45 - N41 C44 H45A N41 - Distance Angles C42 1.3491 (0.0022) C45 1.4635 (0.0022) 110.55 (0.13) H41 0.8800 124.72 124.72 N41 - C42 C45 N43 - Distance Angles C42 1.3549 (0.0021) C44 1.4556 (0.0022) 110.28 (0.14) H43 0.8800 124.86 124.86 N43 - C42 C44 O42 - Distance Angles C42 1.2475 (0.0020) O42 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.71 2.5293(17) 165.6 O1A-H1...O22_$1 0.88 2.26 3.047(2) 148.8 N21-H21...O1B_$1 0.84 1.72 2.5418(17) 166.6 O31A-H31...O42_$2 0.88 2.28 3.0023(19) 139.9 N41-H41...O31B_$2 0.88 2.13 2.914(2) 147.3 N23-H23...O31B_$3 0.88 2.12 2.879(2) 144.0 N43-H43...O1B_$4 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 3.2240 (0.0131) x - 4.3832 (0.0092) y + 9.9302 (0.0270) z = 4.4617 (0.0173) * 0.0000 (0.0000) C31 * 0.0000 (0.0000) O31A * 0.0000 (0.0000) O31B Rms deviation of fitted atoms = 0.0000 3.2240 (0.0131) x - 4.3832 (0.0092) y + 9.9302 (0.0270) z = 4.3094 (0.0057) Angle to previous plane (with approximate esd) = 0.00 ( 0.42 ) * 0.0000 (0.0000) C31_$5 * 0.0000 (0.0000) O31A_$5 * 0.0000 (0.0000) O31B_$5 Rms deviation of fitted atoms = 0.0000 FMAP and GRID set by program FMAP 2 1 16 GRID -3.846 -2 -2 3.846 2 2 R1 = 0.0625 for 2909 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.45 at 0.4326 0.5583 0.8590 [ 0.59 A from H43 ] Deepest hole -0.47 at 0.4993 0.5739 0.9191 [ 0.25 A from H43 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2786 / 18781 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.4326 0.4417 1.1410 1.00000 0.05 0.45 0.59 H43 0.94 N43 1.90 C42 2.00 O1B Q2 1 0.5411 0.1812 0.3468 1.00000 0.05 0.40 0.64 H23 0.96 N23 1.89 C22 2.04 O31B Q3 1 -0.9898 0.2740 1.2402 1.00000 0.05 0.33 0.56 H41 0.91 N41 1.94 C42 2.05 C45 Q4 1 0.4123 0.0646 0.3797 1.00000 0.05 0.31 0.63 N23 0.83 C24 1.38 H23 1.51 H24A Q5 1 0.2773 -0.0358 0.3866 1.00000 0.05 0.30 0.73 C24 0.81 C25 1.40 H24B 1.45 H24A Q6 1 -0.5394 0.2958 1.1176 1.00000 0.05 0.29 0.69 N43 0.77 C44 1.38 H43 1.42 H44A Q7 1 0.5000 0.5000 0.5000 0.50000 0.05 0.26 0.76 C32 1.43 H32A 1.43 H32B 1.43 H32A Q8 1 0.0457 0.3790 0.9544 1.00000 0.05 0.26 0.77 C1 0.77 C2 1.40 H2A 1.53 H2B Q9 1 -0.1126 0.4823 0.7003 1.00000 0.05 0.26 0.86 H31 0.93 O42 1.70 O31A 1.77 C42 Q10 1 0.8456 -0.0634 0.1999 1.00000 0.05 0.25 0.83 O22 0.89 H1 1.70 O1A 1.87 C22 Shortest distances between peaks (including symmetry equivalents) 4 5 1.18 1 6 1.41 2 4 1.43 3 9 2.26 8 8 2.41 2 5 2.59 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 0.39: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.36: Structure factors and derivatives 0.72: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.09: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + ssf1338 finished at 12:36:22 Total CPU time: 1.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++