+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007may0016 started at 17:28:58 on 02-Oct-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007may0016 in P-1 CELL 0.71073 10.0846 10.4718 10.9149 106.718 111.473 95.603 ZERR 6.00 0.0003 0.0003 0.0003 0.001 0.002 0.002 LATT 1 SFAC C H N O S UNIT 36 42 6 6 6 V = 1000.33 F(000) = 444.0 Mu = 0.39 mm-1 Cell Wt = 847.12 Rho = 1.406 MERG 2 OMIT -3.00 55.00 DFIX 0.88 0.02 N1 H1N N1 H2N N2 H3N N2 H4N N3 H5N N3 H6N EQIV $1 -x, -y , -z EQIV $2 x - 1, y , z - 1 EQIV $3 x, y + 1, z EQIV $4 -x + 1, -y + 2 , -z +1 EQIV $5 x, y , z + 1 EQIV $6 -x + 1, -y + 1, -z + 2 HTAB N1 O1_$1 HTAB N1 O3_$2 HTAB N2 O1_$3 HTAB N2 O2_$4 HTAB N3 O1_$5 HTAB N3 O2_$6 FMAP 2 PLAN 5 SIZE 0.02 0.06 0.06 ACTA BOND $H WGHT 0.09830 1.48460 L.S. 6 TEMP -153.00 FVAR 0.67617 MOLE 1 C1 1 0.153705 0.253492 0.344536 11.00000 0.02548 0.01620 = 0.02584 0.00609 0.00940 0.00454 C2 1 0.299335 0.300992 0.427640 11.00000 0.02413 0.01848 = 0.02826 0.00564 0.01031 0.00556 AFIX 43 H2 2 0.372757 0.272490 0.398222 11.00000 -1.20000 AFIX 0 C3 1 0.331551 0.396947 0.562207 11.00000 0.02575 0.01599 = 0.02633 0.00672 0.00489 0.00301 C4 1 0.206583 0.418287 0.577450 11.00000 0.03075 0.02146 = 0.02645 0.00039 0.00902 0.00247 AFIX 43 H4 2 0.205802 0.479357 0.660440 11.00000 -1.20000 AFIX 0 C5 1 0.088853 0.152175 0.199400 11.00000 0.02588 0.01559 = 0.02532 0.00752 0.00840 0.00348 C6 1 0.484320 0.466252 0.673736 11.00000 0.03043 0.01894 = 0.03090 -0.00182 0.00504 -0.00218 AFIX 137 H6A 2 0.517519 0.551958 0.663135 11.00000 -1.50000 H6B 2 0.550743 0.405689 0.663494 11.00000 -1.50000 H6C 2 0.483795 0.486067 0.766925 11.00000 -1.50000 AFIX 0 N1 3 -0.053894 0.129486 0.124001 11.00000 0.02628 0.02178 = 0.02711 0.00076 0.00946 0.00323 O1 4 0.170036 0.091387 0.152479 11.00000 0.02684 0.02150 = 0.02768 0.00304 0.00962 0.00666 S1 5 0.051290 0.324148 0.432256 11.00000 0.02438 0.02483 = 0.02525 0.00183 0.00887 0.00376 MOLE 2 C11 1 0.167410 0.748134 0.297674 11.00000 0.02532 0.01731 = 0.02616 0.00600 0.01174 0.00274 C12 1 0.053964 0.742638 0.177497 11.00000 0.02751 0.02135 = 0.02973 0.00875 0.01012 0.00364 AFIX 43 H12 2 0.050037 0.813266 0.138628 11.00000 -1.20000 AFIX 0 C13 1 -0.057071 0.620718 0.116992 11.00000 0.02644 0.02059 = 0.02850 0.00451 0.00926 0.00522 C14 1 -0.022346 0.537324 0.194215 11.00000 0.02740 0.02152 = 0.03367 0.00381 0.01092 -0.00259 AFIX 43 H14 2 -0.083079 0.450730 0.170023 11.00000 -1.20000 AFIX 0 C15 1 0.303883 0.853501 0.390725 11.00000 0.02512 0.01979 = 0.02294 0.00257 0.00990 0.00267 C16 1 -0.194676 0.589156 -0.013591 11.00000 0.02773 0.02660 = 0.03526 0.00587 0.00607 0.00243 AFIX 137 H16A 2 -0.220554 0.491154 -0.068625 11.00000 -1.50000 H16B 2 -0.178805 0.642047 -0.069884 11.00000 -1.50000 H16C 2 -0.274417 0.613681 0.012569 11.00000 -1.50000 AFIX 0 N2 3 0.319694 0.969045 0.363103 11.00000 0.02504 0.01914 = 0.02864 0.00840 0.00482 -0.00107 O2 4 0.400162 0.834064 0.489828 11.00000 0.02661 0.02148 = 0.02852 0.00757 0.00433 -0.00009 S2 5 0.140692 0.603463 0.338492 11.00000 0.02895 0.02032 = 0.02991 0.00848 0.00858 0.00086 MOLE 1 H1N 2 -0.086218 0.069521 0.039030 11.00000 0.03818 H2N 2 -0.117594 0.160312 0.153554 11.00000 0.01844 MOLE 2 H3N 2 0.252540 0.978967 0.291192 11.00000 0.02674 H4N 2 0.403502 1.027707 0.411780 11.00000 0.03798 MOLE 3 H5N 2 0.419533 0.136053 1.180716 11.00000 0.02974 H6N 2 0.560690 0.169723 1.308682 11.00000 0.02011 C21 1 0.501097 0.174659 1.000764 11.00000 0.02838 0.01649 = 0.03096 0.00769 0.01427 0.00494 C22 1 0.355017 0.123877 0.916324 11.00000 0.02578 0.01976 = 0.02748 0.00671 0.01044 0.00465 AFIX 43 H22 2 0.285656 0.095769 0.948774 11.00000 -1.20000 AFIX 0 C23 1 0.316992 0.117239 0.774874 11.00000 0.03112 0.02179 = 0.02982 0.00779 0.01114 0.00847 C24 1 0.437564 0.164131 0.757708 11.00000 0.03719 0.03163 = 0.03027 0.01201 0.01358 0.00678 AFIX 43 H24 2 0.434445 0.168117 0.670861 11.00000 -1.20000 AFIX 0 C25 1 0.587276 0.195030 1.150204 11.00000 0.02506 0.01616 = 0.02773 0.00354 0.00920 0.00697 C26 1 0.166784 0.061673 0.658061 11.00000 0.03294 0.04397 = 0.03460 0.01177 0.01026 0.00661 AFIX 137 H26A 2 0.166986 0.079134 0.574601 11.00000 -1.50000 H26B 2 0.097049 0.106729 0.687187 11.00000 -1.50000 H26C 2 0.138090 -0.037179 0.636008 11.00000 -1.50000 AFIX 0 N3 3 0.513841 0.169616 1.223159 11.00000 0.02719 0.02343 = 0.02316 0.00488 0.00684 0.00538 O3 4 0.721772 0.235200 1.202952 11.00000 0.02385 0.03195 = 0.03246 0.00491 0.00869 0.00493 S3 5 0.595438 0.215203 0.908578 11.00000 0.03010 0.04396 = 0.03192 0.01319 0.01228 -0.00294 HKLF 4 Covalent radii and connectivity table for 2007may0016 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C1 - C2 C5 S1 C2 - C1 C3 C3 - C4 C2 C6 C4 - C3 S1 C5 - O1 N1 C1 C6 - C3 N1 - C5 O1 - C5 S1 - C4 C1 C11 - C12 C15 S2 C12 - C11 C13 C13 - C14 C12 C16 C14 - C13 S2 C15 - O2 N2 C11 C16 - C13 N2 - C15 O2 - C15 S2 - C14 C11 C21 - C22 C25 S3 C22 - C21 C23 C23 - C24 C22 C26 C24 - C23 S3 C25 - O3 N3 C21 C26 - C23 N3 - C25 O3 - C25 S3 - C24 C21 Operators for generating equivalent atoms: $1 -x, -y, -z $2 x-1, y, z-1 $3 x, y+1, z $4 -x+1, -y+2, -z+1 $5 x, y, z+1 $6 -x+1, -y+1, -z+2 20443 Reflections read, of which 27 rejected -13 =< h =< 12, -13 =< k =< 13, -14 =< l =< 14, Max. 2-theta = 54.99 0 Systematic absence violations 0 Inconsistent equivalents 4571 Unique reflections, of which 0 suppressed R(int) = 0.0709 R(sigma) = 0.0530 Friedel opposites merged Maximum memory for data reduction = 2675 / 46302 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 = 3396 / 338377 wR2 = 0.1960 before cycle 1 for 4571 data and 271 / 271 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.126; Restrained GooF = 1.125 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0983 * P )^2 + 1.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.67610 0.00222 -0.034 OSF Mean shift/esd = 0.003 Maximum = -0.034 for OSF Max. shift = 0.000 A for H5N Max. dU = 0.000 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 3396 / 338377 wR2 = 0.1960 before cycle 2 for 4571 data and 271 / 271 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.126; Restrained GooF = 1.125 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0983 * P )^2 + 1.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.67609 0.00222 -0.003 OSF Mean shift/esd = 0.001 Maximum = -0.007 for U33 S1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 3 Maximum vector length = 511 Memory required = 3396 / 338377 wR2 = 0.1960 before cycle 3 for 4571 data and 271 / 271 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.126; Restrained GooF = 1.125 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0983 * P )^2 + 1.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.67609 0.00222 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.002 for tors H16A Max. shift = 0.000 A for H16A Max. dU = 0.000 for H5N Least-squares cycle 4 Maximum vector length = 511 Memory required = 3396 / 338377 wR2 = 0.1960 before cycle 4 for 4571 data and 271 / 271 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.126; Restrained GooF = 1.125 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0983 * P )^2 + 1.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.67609 0.00222 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for tors H16A Max. shift = 0.000 A for H16B Max. dU = 0.000 for H5N Least-squares cycle 5 Maximum vector length = 511 Memory required = 3396 / 338377 wR2 = 0.1960 before cycle 5 for 4571 data and 271 / 271 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.126; Restrained GooF = 1.125 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0983 * P )^2 + 1.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.67609 0.00222 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for tors H6A Max. shift = 0.000 A for H6B Max. dU = 0.000 for H4N Least-squares cycle 6 Maximum vector length = 511 Memory required = 3396 / 338377 wR2 = 0.1960 before cycle 6 for 4571 data and 271 / 271 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.126; Restrained GooF = 1.125 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0983 * P )^2 + 1.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.67609 0.00222 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for tors H6A Max. shift = 0.000 A for H6C Max. dU = 0.000 for H3N Largest correlation matrix elements 0.727 z H2N / x H2N 0.521 y H2N / x H2N 0.502 U13 C11 / U11 C11 0.587 z H6N / y H6N 0.515 U13 C21 / U33 C21 0.583 z H3N / y H3N 0.513 U13 C21 / U11 C21 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.3728 0.2725 0.3982 43 0.950 0.000 C2 C1 C3 H4 0.2058 0.4794 0.6604 43 0.950 0.000 C4 C3 S1 H6A 0.5175 0.5520 0.6632 137 0.980 0.000 C6 C3 H6A H6B 0.5507 0.4057 0.6635 137 0.980 0.000 C6 C3 H6A H6C 0.4838 0.4860 0.7669 137 0.980 0.000 C6 C3 H6A H12 0.0500 0.8133 0.1386 43 0.950 0.000 C12 C11 C13 H14 -0.0831 0.4507 0.1700 43 0.950 0.000 C14 C13 S2 H16A -0.2206 0.4911 -0.0686 137 0.980 0.000 C16 C13 H16A H16B -0.1788 0.6420 -0.0699 137 0.980 0.000 C16 C13 H16A H16C -0.2744 0.6137 0.0126 137 0.980 0.000 C16 C13 H16A H22 0.2857 0.0958 0.9488 43 0.950 0.000 C22 C21 C23 H24 0.4344 0.1681 0.6709 43 0.950 0.000 C24 C23 S3 H26A 0.1670 0.0791 0.5746 137 0.980 0.000 C26 C23 H26A H26B 0.0970 0.1067 0.6872 137 0.980 0.000 C26 C23 H26A H26C 0.1381 -0.0372 0.6360 137 0.980 0.000 C26 C23 H26A 2007may0016 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.15370 0.25349 0.34453 1.00000 0.02548 0.01620 0.02582 0.00609 0.00939 0.00454 0.02318 0.00795 0.00036 0.00032 0.00034 0.00000 0.00156 0.00148 0.00159 0.00128 0.00132 0.00122 0.00066 C2 0.29934 0.30099 0.42764 1.00000 0.02412 0.01849 0.02825 0.00564 0.01031 0.00556 0.02432 0.00809 0.00036 0.00033 0.00035 0.00000 0.00157 0.00154 0.00164 0.00130 0.00134 0.00124 0.00067 H2 0.37276 0.27249 0.39822 1.00000 0.02919 0.00000 0.00000 C3 0.33155 0.39695 0.56221 1.00000 0.02575 0.01599 0.02632 0.00671 0.00489 0.00302 0.02479 0.00798 0.00036 0.00032 0.00035 0.00000 0.00160 0.00150 0.00163 0.00129 0.00133 0.00122 0.00068 C4 0.20658 0.41829 0.57745 1.00000 0.03075 0.02147 0.02646 0.00040 0.00903 0.00247 0.02924 0.00855 0.00039 0.00036 0.00038 0.00000 0.00177 0.00166 0.00165 0.00136 0.00142 0.00136 0.00074 H4 0.20580 0.47936 0.66044 1.00000 0.03509 0.00000 0.00000 C5 0.08885 0.15218 0.19940 1.00000 0.02588 0.01559 0.02531 0.00752 0.00840 0.00348 0.02294 0.00803 0.00036 0.00032 0.00035 0.00000 0.00158 0.00145 0.00155 0.00125 0.00130 0.00121 0.00065 C6 0.48432 0.46625 0.67374 1.00000 0.03043 0.01894 0.03090 -0.00181 0.00505 -0.00218 0.03220 0.00830 0.00040 0.00036 0.00039 0.00000 0.00180 0.00165 0.00179 0.00141 0.00149 0.00136 0.00079 H6A 0.51751 0.55197 0.66315 1.00000 0.04829 0.00000 0.00000 H6B 0.55075 0.40570 0.66348 1.00000 0.04829 0.00000 0.00000 H6C 0.48380 0.48604 0.76693 1.00000 0.04829 0.00000 0.00000 N1 -0.05389 0.12949 0.12400 1.00000 0.02628 0.02177 0.02710 0.00076 0.00946 0.00322 0.02754 0.00717 0.00032 0.00030 0.00032 0.00000 0.00147 0.00146 0.00149 0.00121 0.00124 0.00116 0.00063 O1 0.17004 0.09139 0.15248 1.00000 0.02683 0.02150 0.02767 0.00304 0.00961 0.00666 0.02706 0.00577 0.00026 0.00024 0.00025 0.00000 0.00121 0.00119 0.00121 0.00099 0.00101 0.00095 0.00053 S1 0.05129 0.32415 0.43226 1.00000 0.02438 0.02484 0.02524 0.00183 0.00887 0.00376 0.02702 0.00204 0.00009 0.00009 0.00009 0.00000 0.00042 0.00044 0.00042 0.00033 0.00033 0.00032 0.00023 C11 0.16741 0.74813 0.29768 1.00000 0.02531 0.01731 0.02615 0.00600 0.01173 0.00274 0.02312 0.00812 0.00036 0.00033 0.00035 0.00000 0.00159 0.00148 0.00157 0.00126 0.00132 0.00122 0.00065 C12 0.05396 0.74264 0.17749 1.00000 0.02750 0.02135 0.02972 0.00876 0.01011 0.00365 0.02691 0.00849 0.00037 0.00035 0.00037 0.00000 0.00167 0.00163 0.00170 0.00139 0.00139 0.00132 0.00071 H12 0.05003 0.81326 0.13862 1.00000 0.03229 0.00000 0.00000 C13 -0.05707 0.62072 0.11699 1.00000 0.02644 0.02059 0.02849 0.00451 0.00925 0.00523 0.02679 0.00837 0.00037 0.00035 0.00037 0.00000 0.00166 0.00161 0.00168 0.00136 0.00140 0.00130 0.00071 C14 -0.02234 0.53732 0.19422 1.00000 0.02740 0.02152 0.03366 0.00380 0.01092 -0.00258 0.03006 0.00866 0.00039 0.00036 0.00039 0.00000 0.00168 0.00167 0.00182 0.00143 0.00147 0.00133 0.00075 H14 -0.08307 0.45073 0.17002 1.00000 0.03607 0.00000 0.00000 C15 0.30388 0.85350 0.39072 1.00000 0.02511 0.01980 0.02293 0.00257 0.00990 0.00267 0.02397 0.00798 0.00036 0.00033 0.00034 0.00000 0.00158 0.00156 0.00152 0.00127 0.00131 0.00125 0.00066 C16 -0.19468 0.58915 -0.01359 1.00000 0.02773 0.02659 0.03525 0.00587 0.00606 0.00243 0.03346 0.00903 0.00040 0.00039 0.00041 0.00000 0.00175 0.00181 0.00192 0.00153 0.00152 0.00141 0.00080 H16A -0.22058 0.49115 -0.06861 1.00000 0.05019 0.00000 0.00000 H16B -0.17879 0.64202 -0.06991 1.00000 0.05019 0.00000 0.00000 H16C -0.27441 0.61371 0.01257 1.00000 0.05019 0.00000 0.00000 N2 0.31970 0.96904 0.36310 1.00000 0.02503 0.01915 0.02863 0.00840 0.00481 -0.00108 0.02667 0.00719 0.00032 0.00029 0.00032 0.00000 0.00145 0.00139 0.00149 0.00120 0.00121 0.00112 0.00062 O2 0.40016 0.83406 0.48983 1.00000 0.02661 0.02150 0.02852 0.00758 0.00433 -0.00008 0.02842 0.00576 0.00026 0.00024 0.00026 0.00000 0.00121 0.00118 0.00122 0.00099 0.00101 0.00094 0.00054 S2 0.14069 0.60346 0.33849 1.00000 0.02895 0.02032 0.02991 0.00848 0.00858 0.00086 0.02794 0.00208 0.00010 0.00009 0.00009 0.00000 0.00044 0.00042 0.00045 0.00034 0.00035 0.00032 0.00023 H1N -0.08623 0.06947 0.03905 1.00000 0.03825 0.06897 0.00457 0.00371 0.00260 0.00000 0.01187 H2N -0.11759 0.16032 0.15356 1.00000 0.01841 0.09212 0.00331 0.00369 0.00370 0.00000 0.00886 H3N 0.25253 0.97895 0.29119 1.00000 0.02680 0.08397 0.00343 0.00416 0.00305 0.00000 0.01008 H4N 0.40349 1.02772 0.41177 1.00000 0.03793 0.06115 0.00295 0.00371 0.00409 0.00000 0.01177 H5N 0.41955 0.13599 1.18071 1.00000 0.02975 0.07160 0.00220 0.00407 0.00398 0.00000 0.01051 H6N 0.56069 0.16974 1.30868 1.00000 0.02017 0.07860 0.00369 0.00391 0.00238 0.00000 0.00894 C21 0.50110 0.17466 1.00076 1.00000 0.02838 0.01651 0.03096 0.00769 0.01427 0.00494 0.02482 0.00837 0.00037 0.00033 0.00036 0.00000 0.00167 0.00150 0.00171 0.00133 0.00141 0.00125 0.00068 C22 0.35501 0.12388 0.91632 1.00000 0.02578 0.01977 0.02746 0.00671 0.01043 0.00465 0.02492 0.00825 0.00037 0.00034 0.00036 0.00000 0.00160 0.00156 0.00162 0.00131 0.00135 0.00125 0.00067 H22 0.28565 0.09577 0.94877 1.00000 0.02990 0.00000 0.00000 C23 0.31699 0.11724 0.77487 1.00000 0.03113 0.02179 0.02981 0.00779 0.01115 0.00847 0.02812 0.00885 0.00040 0.00035 0.00038 0.00000 0.00175 0.00166 0.00172 0.00140 0.00144 0.00135 0.00072 C24 0.43757 0.16413 0.75771 1.00000 0.03718 0.03162 0.03027 0.01201 0.01358 0.00678 0.03293 0.00944 0.00042 0.00039 0.00040 0.00000 0.00198 0.00193 0.00181 0.00156 0.00158 0.00156 0.00080 H24 0.43445 0.16811 0.67086 1.00000 0.03952 0.00000 0.00000 C25 0.58728 0.19503 1.15020 1.00000 0.02505 0.01616 0.02772 0.00355 0.00919 0.00697 0.02430 0.00813 0.00036 0.00033 0.00036 0.00000 0.00158 0.00147 0.00163 0.00128 0.00133 0.00122 0.00067 C26 0.16678 0.06167 0.65806 1.00000 0.03294 0.04396 0.03459 0.01176 0.01025 0.00661 0.03894 0.01012 0.00043 0.00046 0.00043 0.00000 0.00198 0.00231 0.00201 0.00178 0.00165 0.00170 0.00089 H26A 0.16698 0.07915 0.57461 1.00000 0.05841 0.00000 0.00000 H26B 0.09705 0.10672 0.68720 1.00000 0.05841 0.00000 0.00000 H26C 0.13809 -0.03718 0.63600 1.00000 0.05841 0.00000 0.00000 N3 0.51384 0.16962 1.22316 1.00000 0.02718 0.02343 0.02314 0.00488 0.00683 0.00538 0.02649 0.00730 0.00033 0.00030 0.00031 0.00000 0.00148 0.00144 0.00140 0.00117 0.00121 0.00117 0.00061 O3 0.72177 0.23520 1.20295 1.00000 0.02385 0.03195 0.03245 0.00491 0.00868 0.00493 0.03193 0.00615 0.00026 0.00027 0.00027 0.00000 0.00120 0.00138 0.00132 0.00110 0.00104 0.00101 0.00058 S3 0.59544 0.21520 0.90858 1.00000 0.03009 0.04397 0.03191 0.01319 0.01228 -0.00294 0.03638 0.00239 0.00010 0.00011 0.00010 0.00000 0.00048 0.00058 0.00049 0.00042 0.00039 0.00039 0.00027 Final Structure Factor Calculation for 2007may0016 in P-1 Total number of l.s. parameters = 271 Maximum vector length = 511 Memory required = 3125 / 24017 wR2 = 0.1960 before cycle 7 for 4571 data and 0 / 271 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.126; Restrained GooF = 1.125 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0983 * P )^2 + 1.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0699 for 3522 Fo > 4sig(Fo) and 0.0943 for all 4571 data wR2 = 0.1960, GooF = S = 1.126, Restrained GooF = 1.125 for all data Occupancy sum of asymmetric unit = 27.00 for non-hydrogen and 21.00 for hydrogen atoms Principal mean square atomic displacements U 0.0282 0.0253 0.0161 C1 0.0309 0.0241 0.0179 C2 0.0361 0.0224 0.0158 C3 0.0371 0.0329 0.0177 C4 0.0294 0.0244 0.0151 C5 0.0460 0.0364 0.0142 C6 0.0371 0.0273 0.0182 N1 0.0360 0.0264 0.0188 O1 0.0359 0.0252 0.0199 S1 0.0284 0.0239 0.0171 C11 0.0319 0.0280 0.0208 C12 0.0342 0.0264 0.0198 C13 0.0395 0.0334 0.0173 C14 0.0294 0.0250 0.0175 C15 0.0457 0.0317 0.0230 C16 0.0386 0.0252 0.0163 N2 0.0400 0.0264 0.0189 O2 0.0362 0.0289 0.0187 S2 0.0324 0.0259 0.0162 C21 0.0290 0.0260 0.0198 C22 0.0345 0.0294 0.0204 C23 0.0382 0.0320 0.0286 C24 0.0339 0.0247 0.0143 C25 0.0456 0.0402 0.0310 C26 0.0331 0.0256 0.0208 N3 0.0430 0.0292 0.0236 O3 0.0537 0.0316 0.0238 S3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.023 0.035 0.049 0.065 0.081 0.101 0.131 0.189 1.000 Number in group 463. 465. 449. 461. 465. 457. 439. 458. 456. 458. GooF 1.145 1.163 1.315 1.166 1.113 0.967 0.987 0.942 0.989 1.377 K 2.864 1.202 0.977 1.031 0.982 0.993 1.054 1.023 1.012 1.066 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.66 inf Number in group 475. 449. 460. 461. 447. 456. 451. 457. 456. 459. GooF 1.222 1.179 1.129 1.112 1.016 0.905 0.934 0.909 1.130 1.557 K 1.064 1.070 1.052 1.063 1.016 1.006 0.992 1.014 1.017 1.087 R1 0.194 0.169 0.146 0.117 0.099 0.076 0.066 0.058 0.060 0.073 Recommended weighting scheme: WGHT 0.0984 1.4828 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) 0 2 0 5922.29 3390.63 5.27 0.450 4.88 0 5 0 1534.01 870.58 5.00 0.228 1.95 0 3 0 5029.85 3131.11 4.39 0.433 3.26 0 2 1 3551.96 2213.36 4.34 0.364 3.83 0 5 1 1340.67 832.15 4.25 0.223 1.79 0 7 1 1413.31 880.47 4.13 0.229 1.32 0 1 1 4308.69 2726.42 4.06 0.404 5.87 0 3 2 2467.97 1554.93 4.05 0.305 2.33 1 3 1 6924.46 4470.15 4.00 0.517 2.46 1 4 0 4192.67 2805.46 3.71 0.409 2.24 0 8 2 2365.80 1556.64 3.69 0.305 1.09 0 4 1 461.45 290.74 3.69 0.132 2.19 0 4 0 2215.15 1476.07 3.66 0.297 2.44 1 4 1 345.72 211.84 3.66 0.113 2.00 1 7 2 2519.74 1680.34 3.58 0.317 1.17 3 7 6 12.64 65.85 3.49 0.063 0.79 -1 5 0 2598.22 1800.39 3.33 0.328 2.01 0 -6 2 1103.29 753.03 3.32 0.212 1.74 2 5 1 770.64 520.98 3.25 0.176 1.53 -1 6 0 4432.79 3103.35 3.24 0.431 1.67 -6 -10 5 41.25 0.42 3.21 0.005 0.84 8 -11 3 -5.05 19.24 3.16 0.034 0.77 2 -7 8 58.82 114.18 3.14 0.083 1.04 1 5 1 236.95 150.90 3.10 0.095 1.67 9 4 0 37.43 10.10 3.10 0.025 0.87 -1 -4 1 230.67 148.50 3.08 0.094 2.41 -1 -3 1 1040.21 722.84 3.08 0.208 3.15 0 -4 1 1039.17 729.74 3.08 0.209 2.59 1 2 1 35.42 13.84 3.03 0.029 3.17 3 -2 2 -1.93 14.71 3.02 0.030 2.29 0 3 1 379.45 252.13 3.00 0.123 2.80 -1 3 1 2722.15 1913.42 3.00 0.338 2.95 2 8 3 38.33 9.60 3.00 0.024 0.94 0 3 3 1538.81 1074.06 2.99 0.253 1.96 -1 10 1 671.53 456.12 2.99 0.165 0.96 -6 -9 9 70.45 23.02 2.96 0.037 0.87 -6 -1 13 604.34 392.34 2.95 0.153 0.82 -4 10 6 102.74 194.81 2.95 0.108 0.78 -1 8 1 1831.07 1310.35 2.92 0.280 1.19 -4 -6 13 22.31 0.78 2.92 0.007 0.82 -10 -5 10 49.64 8.28 2.92 0.022 0.82 -9 -3 12 180.00 101.22 2.90 0.078 0.82 1 -9 10 22.02 0.04 2.86 0.002 0.86 -7 -2 13 36.94 6.88 2.86 0.020 0.82 -1 4 1 598.37 421.01 2.86 0.159 2.29 -2 5 1 6025.97 4280.52 2.85 0.506 1.86 11 -6 2 66.10 29.25 2.85 0.042 0.78 0 -3 1 17126.81 12407.74 2.84 0.861 3.47 -9 7 7 54.72 12.79 2.80 0.028 0.82 -3 10 2 62.68 23.04 2.79 0.037 0.94 Bond lengths and angles C1 - Distance Angles C2 1.3600 (0.0046) C5 1.4839 (0.0046) 125.40 (0.31) S1 1.7311 (0.0034) 110.85 (0.25) 123.73 (0.25) C1 - C2 C5 C2 - Distance Angles C1 1.3600 (0.0046) C3 1.4179 (0.0047) 113.85 (0.30) H2 0.9500 123.08 123.08 C2 - C1 C3 C3 - Distance Angles C4 1.3613 (0.0051) C2 1.4179 (0.0047) 110.99 (0.30) C6 1.5108 (0.0046) 124.55 (0.32) 124.46 (0.31) C3 - C4 C2 C4 - Distance Angles C3 1.3613 (0.0051) S1 1.7083 (0.0036) 113.19 (0.27) H4 0.9500 123.40 123.40 C4 - C3 S1 C5 - Distance Angles O1 1.2486 (0.0041) N1 1.3264 (0.0043) 122.31 (0.31) C1 1.4839 (0.0046) 119.10 (0.29) 118.58 (0.30) C5 - O1 N1 C6 - Distance Angles C3 1.5108 (0.0046) H6A 0.9800 109.47 H6B 0.9800 109.47 109.47 H6C 0.9800 109.47 109.47 109.47 C6 - C3 H6A H6B N1 - Distance Angles C5 1.3264 (0.0043) H1N 0.8743 (0.0190) 114.83 (2.92) H2N 0.8679 (0.0183) 126.69 (2.49) 118.05 (3.85) N1 - C5 H1N O1 - Distance Angles C5 1.2486 (0.0041) O1 - S1 - Distance Angles C4 1.7083 (0.0036) C1 1.7311 (0.0034) 91.11 (0.17) S1 - C4 C11 - Distance Angles C12 1.3704 (0.0048) C15 1.4760 (0.0045) 130.74 (0.31) S2 1.7212 (0.0033) 111.56 (0.25) 117.69 (0.25) C11 - C12 C15 C12 - Distance Angles C11 1.3704 (0.0048) C13 1.4192 (0.0048) 113.16 (0.31) H12 0.9500 123.42 123.42 C12 - C11 C13 C13 - Distance Angles C14 1.3649 (0.0051) C12 1.4192 (0.0048) 110.81 (0.31) C16 1.5026 (0.0049) 124.88 (0.32) 124.31 (0.32) C13 - C14 C12 C14 - Distance Angles C13 1.3649 (0.0051) S2 1.7080 (0.0037) 113.60 (0.26) H14 0.9500 123.20 123.20 C14 - C13 S2 C15 - Distance Angles O2 1.2452 (0.0041) N2 1.3370 (0.0044) 121.88 (0.30) C11 1.4760 (0.0045) 120.88 (0.30) 117.24 (0.30) C15 - O2 N2 C16 - Distance Angles C13 1.5026 (0.0049) H16A 0.9800 109.47 H16B 0.9800 109.47 109.47 H16C 0.9800 109.47 109.47 109.47 C16 - C13 H16A H16B N2 - Distance Angles C15 1.3370 (0.0044) H3N 0.8700 (0.0186) 120.24 (2.76) H4N 0.8695 (0.0193) 117.64 (3.02) 121.57 (4.11) N2 - C15 H3N O2 - Distance Angles C15 1.2452 (0.0041) O2 - S2 - Distance Angles C14 1.7080 (0.0037) C11 1.7212 (0.0033) 90.87 (0.17) S2 - C14 C21 - Distance Angles C22 1.3687 (0.0047) C25 1.4789 (0.0048) 131.54 (0.32) S3 1.7221 (0.0034) 111.20 (0.26) 117.22 (0.25) C21 - C22 C25 C22 - Distance Angles C21 1.3687 (0.0047) C23 1.4266 (0.0049) 113.49 (0.32) H22 0.9500 123.26 123.26 C22 - C21 C23 C23 - Distance Angles C24 1.3630 (0.0054) C22 1.4266 (0.0049) 110.81 (0.32) C26 1.4986 (0.0051) 123.75 (0.34) 125.41 (0.33) C23 - C24 C22 C24 - Distance Angles C23 1.3630 (0.0054) S3 1.7147 (0.0039) 113.25 (0.29) H24 0.9500 123.37 123.37 C24 - C23 S3 C25 - Distance Angles O3 1.2352 (0.0041) N3 1.3299 (0.0047) 122.55 (0.32) C21 1.4789 (0.0048) 120.17 (0.32) 117.28 (0.29) C25 - O3 N3 C26 - Distance Angles C23 1.4986 (0.0051) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C23 H26A H26B N3 - Distance Angles C25 1.3299 (0.0047) H5N 0.8724 (0.0190) 119.74 (2.78) H6N 0.8780 (0.0185) 120.47 (2.50) 118.55 (3.78) N3 - C25 H5N O3 - Distance Angles C25 1.2352 (0.0041) O3 - S3 - Distance Angles C24 1.7147 (0.0039) C21 1.7221 (0.0035) 91.25 (0.18) S3 - C24 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.874(19) 2.08(2) 2.949(4) 173(4) N1-H1N...O1_$1 0.868(18) 2.04(2) 2.908(4) 174(3) N1-H2N...O3_$2 0.870(19) 2.16(3) 2.956(4) 152(4) N2-H3N...O1_$3 0.869(19) 2.04(2) 2.906(4) 175(4) N2-H4N...O2_$4 0.872(19) 2.40(2) 3.227(4) 158(4) N3-H5N...O1_$5 0.878(18) 2.10(2) 2.942(4) 160(3) N3-H6N...O2_$6 FMAP and GRID set by program FMAP 2 1 28 GRID -2.000 -2 -2 2.000 2 2 R1 = 0.0939 for 4571 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.90 at 0.4375 0.7988 0.0247 [ 0.82 A from C21 ] Deepest hole -0.60 at 0.2174 0.6814 0.3941 [ 0.94 A from S2 ] Mean = 0.00, Rms deviation from mean = 0.13 e/A^3, Highest memory used = 3101 / 24867 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5625 0.2012 0.9753 1.00000 0.05 0.90 0.82 C21 0.94 S3 1.85 C25 1.96 C22 Q2 1 -0.0216 0.3242 0.4610 1.00000 0.05 0.85 0.90 S1 2.14 C4 2.49 H4 2.58 C1 Q3 1 0.5178 0.2145 0.8365 1.00000 0.05 0.80 0.88 S3 0.90 C24 1.59 H24 1.95 C23 Q4 1 0.1221 0.3160 0.3955 1.00000 0.05 0.79 0.89 C1 0.94 S1 1.72 C2 1.78 C4 Q5 1 0.0413 0.6059 0.3429 1.00000 0.05 0.74 1.02 S2 1.43 C14 1.97 H14 2.14 C11 Shortest distances between peaks (including symmetry equivalents) 1 3 1.47 2 4 1.83 2 5 2.14 Time profile in seconds ----------------------- 0.12: Read and process instructions 0.00: Fit rigid groups 0.01: Interpret restraints etc. 0.01: 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. 0.96: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.27: Structure factors and derivatives 0.73: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.25: Solve l.s. equations 0.00: Generate HTAB table 0.01: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007may0016 finished at 17:29:11 Total CPU time: 2.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++