+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007may0006 started at 12:02:18 on 29-Sep-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007may0006 in P2(1)2(1)2(1) CELL 0.71073 7.3989 11.2007 20.2402 90.000 90.000 90.000 ZERR 8.00 0.0003 0.0004 0.0007 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O UNIT 80 72 8 16 V = 1677.36 F(000) = 736.0 Mu = 0.10 mm-1 Cell Wt = 1401.46 Rho = 1.387 MERG 4 OMIT -3.00 55.00 OMIT 0 2 5 OMIT 1 1 1 EXTI 0.01405 DFIX 0.84 0.02 O2 H1O O3 H2O HTAB O2 O4 HTAB O3 O1 FMAP 2 PLAN 5 SIZE 0.10 0.20 0.30 ACTA BOND $H WGHT 0.06460 0.34780 L.S. 6 TEMP -153.00 FVAR 0.63639 MOLE 1 C1 1 0.397087 0.500922 0.011496 11.00000 0.02657 0.02238 = 0.02337 -0.00167 0.00343 0.00055 C2 1 0.276527 0.580920 -0.026247 11.00000 0.02661 0.02104 = 0.02095 -0.00131 0.00007 -0.00043 C3 1 0.353537 0.676996 -0.058856 11.00000 0.02363 0.02353 = 0.02405 -0.00262 0.00021 -0.00055 AFIX 43 H3 2 0.479340 0.693240 -0.056151 11.00000 -1.20000 AFIX 0 C4 1 0.237463 0.748674 -0.095828 11.00000 0.02528 0.02339 = 0.02152 0.00206 0.00115 0.00320 C5 1 0.122067 0.888172 -0.161587 11.00000 0.02889 0.03145 = 0.02964 0.00275 -0.00269 0.00387 AFIX 43 H5 2 0.113545 0.955535 -0.189935 11.00000 -1.20000 AFIX 0 C6 1 -0.020484 0.817927 -0.143495 11.00000 0.02377 0.03675 = 0.03245 0.00458 -0.00146 0.00477 AFIX 43 H6 2 -0.143046 0.827720 -0.156392 11.00000 -1.20000 AFIX 0 C7 1 0.050630 0.726646 -0.101316 11.00000 0.02354 0.02702 = 0.02456 -0.00005 0.00168 0.00269 C8 1 -0.024497 0.628202 -0.067396 11.00000 0.02206 0.03040 = 0.02605 -0.00408 0.00251 -0.00106 AFIX 43 H8 2 -0.150246 0.611619 -0.069790 11.00000 -1.20000 AFIX 0 C9 1 0.089610 0.556749 -0.030686 11.00000 0.02762 0.02473 = 0.02226 -0.00115 0.00360 -0.00204 AFIX 43 H9 2 0.041312 0.489814 -0.007899 11.00000 -1.20000 AFIX 0 N1 3 0.279134 0.848208 -0.133255 11.00000 0.02225 0.02618 = 0.02713 0.00418 0.00168 0.00171 O1 4 0.566149 0.518187 0.008453 11.00000 0.02532 0.03171 = 0.03125 0.00079 -0.00095 0.00199 O2 4 0.325575 0.416515 0.045343 11.00000 0.03175 0.03044 = 0.03764 0.01241 0.00035 0.00110 H1O 2 0.394060 0.363263 0.065071 11.00000 -1.50000 MOLE 2 C10 1 0.456650 0.902001 -0.140702 11.00000 0.02439 0.02782 = 0.03122 0.00576 0.00136 0.00185 AFIX 137 H10A 2 0.518360 0.866281 -0.178712 11.00000 -1.50000 H10B 2 0.527867 0.887893 -0.100632 11.00000 -1.50000 H10C 2 0.443463 0.988115 -0.147787 11.00000 -1.50000 AFIX 0 C11 1 0.716224 0.279487 0.095043 11.00000 0.02401 0.02546 = 0.02649 -0.00045 -0.00251 -0.00241 C12 1 0.842453 0.190476 0.123424 11.00000 0.02302 0.02281 = 0.02305 -0.00066 -0.00229 0.00052 C13 1 0.775660 0.103145 0.165374 11.00000 0.02128 0.02543 = 0.02219 -0.00174 -0.00096 0.00137 AFIX 43 H13 2 0.651376 0.099970 0.177029 11.00000 -1.20000 AFIX 0 C14 1 0.899526 0.020164 0.189663 11.00000 0.02206 0.02384 = 0.01976 -0.00301 -0.00151 0.00021 C15 1 1.033850 -0.135747 0.237901 11.00000 0.03077 0.02658 = 0.02634 -0.00074 -0.00337 0.00787 AFIX 43 H15 2 1.050706 -0.206031 0.263441 11.00000 -1.20000 AFIX 0 C16 1 1.167198 -0.077973 0.204007 11.00000 0.02289 0.03547 = 0.02627 -0.00386 -0.00349 0.00758 AFIX 43 H16 2 1.290790 -0.100585 0.201718 11.00000 -1.20000 AFIX 0 C17 1 1.085761 0.023180 0.172529 11.00000 0.02511 0.02748 = 0.02218 -0.00529 -0.00257 0.00147 C18 1 1.149461 0.114688 0.131409 11.00000 0.02176 0.03161 = 0.02910 -0.00290 0.00049 -0.00236 AFIX 43 H18 2 1.274121 0.120094 0.120573 11.00000 -1.20000 AFIX 0 C19 1 1.027109 0.196973 0.106924 11.00000 0.02675 0.02861 = 0.02349 -0.00077 -0.00011 -0.00353 AFIX 43 H19 2 1.068300 0.258808 0.078545 11.00000 -1.20000 AFIX 0 C20 1 0.701812 -0.111595 0.260951 11.00000 0.02713 0.03148 = 0.03518 0.00507 0.00107 -0.00283 AFIX 137 H20A 2 0.710896 -0.193639 0.277443 11.00000 -1.50000 H20B 2 0.603752 -0.106516 0.228525 11.00000 -1.50000 H20C 2 0.676532 -0.057486 0.297862 11.00000 -1.50000 AFIX 0 N2 3 0.871532 -0.077645 0.229794 11.00000 0.02440 0.02659 = 0.02390 0.00053 -0.00090 0.00178 O3 4 0.783267 0.360357 0.057978 11.00000 0.02816 0.02824 = 0.04798 0.01527 -0.00323 0.00106 O4 4 0.548593 0.272479 0.107784 11.00000 0.02379 0.04085 = 0.04371 0.01245 0.00319 0.00408 H2O 2 0.710638 0.409775 0.038837 11.00000 -1.50000 HKLF 4 Covalent radii and connectivity table for 2007may0006 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1 O2 C2 C2 - C3 C9 C1 C3 - C2 C4 C4 - N1 C3 C7 C5 - C6 N1 C6 - C5 C7 C7 - C4 C8 C6 C8 - C9 C7 C9 - C8 C2 N1 - C5 C4 C10 O1 - C1 O2 - C1 C10 - N1 C11 - O4 O3 C12 C12 - C13 C19 C11 C13 - C12 C14 C14 - N2 C13 C17 C15 - C16 N2 C16 - C15 C17 C17 - C18 C14 C16 C18 - C19 C17 C19 - C18 C12 C20 - N2 N2 - C15 C14 C20 O3 - C11 O4 - C11 15593 Reflections read, of which 66 rejected -9 =< h =< 9, -14 =< k =< 14, -26 =< l =< 25, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 2213 Unique reflections, of which 0 suppressed R(int) = 0.0809 R(sigma) = 0.0556 Friedel opposites merged Maximum memory for data reduction = 2332 / 21625 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 = 2990 / 302741 wR2 = 0.1212 before cycle 1 for 2213 data and 244 / 244 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.051 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0646 * P )^2 + 0.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.63638 0.00209 -0.005 OSF 2 0.01405 0.00315 -0.002 EXTI Mean shift/esd = 0.002 Maximum = -0.009 for U22 C6 Max. shift = 0.000 A for H10C Max. dU = 0.000 for C6 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2990 / 302741 wR2 = 0.1212 before cycle 2 for 2213 data and 244 / 244 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.050 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0646 * P )^2 + 0.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.63637 0.00209 -0.003 OSF 2 0.01404 0.00315 -0.001 EXTI Mean shift/esd = 0.001 Maximum = -0.004 for tors H10A Max. shift = 0.000 A for H10C Max. dU = 0.000 for C6 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2990 / 302741 wR2 = 0.1212 before cycle 3 for 2213 data and 244 / 244 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.051 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0646 * P )^2 + 0.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.63637 0.00209 0.000 OSF 2 0.01404 0.00315 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.003 for tors H10A Max. shift = 0.000 A for H10A Max. dU = 0.000 for C4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2990 / 302741 wR2 = 0.1212 before cycle 4 for 2213 data and 244 / 244 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.050 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0646 * P )^2 + 0.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.63637 0.00209 0.000 OSF 2 0.01404 0.00315 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for tors H10A Max. shift = 0.000 A for H10A Max. dU = 0.000 for C11 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2990 / 302741 wR2 = 0.1212 before cycle 5 for 2213 data and 244 / 244 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.051 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0646 * P )^2 + 0.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.63637 0.00209 0.000 OSF 2 0.01404 0.00315 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for tors H10A Max. shift = 0.000 A for H10A Max. dU = 0.000 for C20 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2990 / 302741 wR2 = 0.1212 before cycle 6 for 2213 data and 244 / 244 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.051 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0646 * P )^2 + 0.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.63637 0.00209 0.000 OSF 2 0.01404 0.00315 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for tors H10A Max. shift = 0.000 A for H10A Max. dU = 0.000 for N1 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.4793 0.6932 -0.0562 43 0.950 0.000 C3 C2 C4 H5 0.1135 0.9555 -0.1899 43 0.950 0.000 C5 C6 N1 H6 -0.1430 0.8277 -0.1564 43 0.950 0.000 C6 C5 C7 H8 -0.1502 0.6116 -0.0698 43 0.950 0.000 C8 C9 C7 H9 0.0413 0.4898 -0.0079 43 0.950 0.000 C9 C8 C2 H10A 0.5184 0.8663 -0.1787 137 0.980 0.000 C10 N1 H10A H10B 0.5279 0.8879 -0.1006 137 0.980 0.000 C10 N1 H10A H10C 0.4435 0.9881 -0.1478 137 0.980 0.000 C10 N1 H10A H13 0.6514 0.1000 0.1770 43 0.950 0.000 C13 C12 C14 H15 1.0507 -0.2060 0.2634 43 0.950 0.000 C15 C16 N2 H16 1.2908 -0.1006 0.2017 43 0.950 0.000 C16 C15 C17 H18 1.2741 0.1201 0.1206 43 0.950 0.000 C18 C19 C17 H19 1.0683 0.2588 0.0785 43 0.950 0.000 C19 C18 C12 H20A 0.7109 -0.1936 0.2775 137 0.980 0.000 C20 N2 H20A H20B 0.6038 -0.1065 0.2285 137 0.980 0.000 C20 N2 H20A H20C 0.6765 -0.0575 0.2979 137 0.980 0.000 C20 N2 H20A 2007may0006 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.39709 0.50092 0.01150 1.00000 0.02657 0.02238 0.02336 -0.00168 0.00343 0.00055 0.02410 0.00488 0.00040 0.00025 0.00013 0.00000 0.00148 0.00144 0.00133 0.00117 0.00115 0.00118 0.00061 C2 0.27653 0.58092 -0.02625 1.00000 0.02660 0.02104 0.02095 -0.00131 0.00006 -0.00043 0.02286 0.00485 0.00040 0.00025 0.00013 0.00000 0.00142 0.00135 0.00127 0.00112 0.00118 0.00120 0.00059 C3 0.35354 0.67700 -0.05886 1.00000 0.02363 0.02353 0.02404 -0.00263 0.00021 -0.00055 0.02373 0.00482 0.00041 0.00025 0.00013 0.00000 0.00144 0.00144 0.00135 0.00117 0.00120 0.00120 0.00062 H3 0.47934 0.69324 -0.05615 1.00000 0.02848 0.00000 0.00000 C4 0.23746 0.74867 -0.09583 1.00000 0.02528 0.02339 0.02152 0.00206 0.00115 0.00320 0.02339 0.00492 0.00041 0.00024 0.00013 0.00000 0.00150 0.00148 0.00128 0.00115 0.00117 0.00121 0.00062 C5 0.12207 0.88817 -0.16159 1.00000 0.02889 0.03145 0.02964 0.00276 -0.00269 0.00387 0.02999 0.00536 0.00042 0.00028 0.00014 0.00000 0.00158 0.00169 0.00148 0.00128 0.00131 0.00138 0.00069 H5 0.11355 0.95554 -0.18994 1.00000 0.03599 0.00000 0.00000 C6 -0.02048 0.81793 -0.14350 1.00000 0.02377 0.03673 0.03244 0.00457 -0.00147 0.00477 0.03098 0.00547 0.00043 0.00027 0.00015 0.00000 0.00153 0.00171 0.00150 0.00135 0.00132 0.00135 0.00070 H6 -0.14305 0.82772 -0.15639 1.00000 0.03718 0.00000 0.00000 C7 0.05063 0.72665 -0.10132 1.00000 0.02354 0.02702 0.02456 -0.00005 0.00169 0.00269 0.02504 0.00500 0.00040 0.00026 0.00013 0.00000 0.00146 0.00150 0.00130 0.00118 0.00119 0.00126 0.00063 C8 -0.02450 0.62820 -0.06740 1.00000 0.02206 0.03040 0.02605 -0.00408 0.00251 -0.00106 0.02617 0.00496 0.00040 0.00026 0.00013 0.00000 0.00141 0.00150 0.00134 0.00123 0.00121 0.00128 0.00063 H8 -0.15025 0.61162 -0.06979 1.00000 0.03140 0.00000 0.00000 C9 0.08961 0.55675 -0.03069 1.00000 0.02762 0.02472 0.02226 -0.00115 0.00360 -0.00204 0.02487 0.00490 0.00041 0.00025 0.00013 0.00000 0.00148 0.00145 0.00126 0.00116 0.00124 0.00122 0.00062 H9 0.04131 0.48981 -0.00790 1.00000 0.02984 0.00000 0.00000 N1 0.27913 0.84821 -0.13326 1.00000 0.02224 0.02617 0.02712 0.00418 0.00168 0.00171 0.02518 0.00424 0.00034 0.00021 0.00011 0.00000 0.00118 0.00128 0.00124 0.00104 0.00103 0.00105 0.00055 O1 0.56615 0.51819 0.00845 1.00000 0.02532 0.03171 0.03125 0.00078 -0.00094 0.00199 0.02942 0.00354 0.00028 0.00018 0.00009 0.00000 0.00104 0.00112 0.00103 0.00092 0.00089 0.00091 0.00049 O2 0.32557 0.41652 0.04534 1.00000 0.03175 0.03043 0.03763 0.01241 0.00035 0.00110 0.03327 0.00406 0.00030 0.00021 0.00011 0.00000 0.00123 0.00120 0.00122 0.00099 0.00095 0.00098 0.00054 H1O 0.39407 0.36326 0.06507 1.00000 0.04990 0.06560 0.00479 0.00278 0.00171 0.00000 0.00000 C10 0.45665 0.90200 -0.14070 1.00000 0.02439 0.02783 0.03122 0.00576 0.00137 0.00185 0.02781 0.00522 0.00040 0.00026 0.00015 0.00000 0.00143 0.00154 0.00144 0.00129 0.00127 0.00125 0.00065 H10A 0.51838 0.86626 -0.17870 1.00000 0.04172 0.00000 0.00000 H10B 0.52785 0.88792 -0.10063 1.00000 0.04172 0.00000 0.00000 H10C 0.44346 0.98811 -0.14780 1.00000 0.04172 0.00000 0.00000 C11 0.71622 0.27949 0.09504 1.00000 0.02401 0.02545 0.02649 -0.00045 -0.00251 -0.00241 0.02532 0.00495 0.00042 0.00026 0.00014 0.00000 0.00142 0.00150 0.00136 0.00125 0.00122 0.00128 0.00063 C12 0.84245 0.19048 0.12342 1.00000 0.02302 0.02281 0.02305 -0.00067 -0.00229 0.00052 0.02296 0.00473 0.00039 0.00025 0.00013 0.00000 0.00140 0.00147 0.00133 0.00114 0.00114 0.00116 0.00061 C13 0.77566 0.10314 0.16537 1.00000 0.02128 0.02542 0.02219 -0.00174 -0.00095 0.00137 0.02297 0.00489 0.00040 0.00026 0.00013 0.00000 0.00134 0.00151 0.00129 0.00116 0.00117 0.00122 0.00061 H13 0.65138 0.09997 0.17703 1.00000 0.02756 0.00000 0.00000 C14 0.89953 0.02016 0.18966 1.00000 0.02206 0.02383 0.01976 -0.00301 -0.00151 0.00021 0.02188 0.00459 0.00037 0.00025 0.00013 0.00000 0.00138 0.00146 0.00120 0.00113 0.00110 0.00120 0.00059 C15 1.03385 -0.13575 0.23790 1.00000 0.03077 0.02658 0.02634 -0.00074 -0.00338 0.00787 0.02790 0.00513 0.00041 0.00027 0.00014 0.00000 0.00161 0.00155 0.00143 0.00122 0.00129 0.00138 0.00068 H15 1.05071 -0.20603 0.26344 1.00000 0.03348 0.00000 0.00000 C16 1.16720 -0.07797 0.20401 1.00000 0.02288 0.03547 0.02626 -0.00385 -0.00349 0.00758 0.02820 0.00508 0.00039 0.00029 0.00013 0.00000 0.00146 0.00168 0.00149 0.00131 0.00119 0.00130 0.00069 H16 1.29079 -0.10058 0.20172 1.00000 0.03385 0.00000 0.00000 C17 1.08576 0.02318 0.17253 1.00000 0.02511 0.02747 0.02218 -0.00529 -0.00257 0.00148 0.02492 0.00478 0.00040 0.00026 0.00013 0.00000 0.00145 0.00154 0.00129 0.00116 0.00114 0.00128 0.00063 C18 1.14946 0.11469 0.13141 1.00000 0.02176 0.03162 0.02910 -0.00289 0.00049 -0.00236 0.02749 0.00486 0.00039 0.00026 0.00014 0.00000 0.00139 0.00161 0.00148 0.00130 0.00126 0.00128 0.00066 H18 1.27412 0.12009 0.12057 1.00000 0.03299 0.00000 0.00000 C19 1.02711 0.19697 0.10692 1.00000 0.02675 0.02861 0.02349 -0.00077 -0.00011 -0.00353 0.02628 0.00493 0.00041 0.00027 0.00013 0.00000 0.00156 0.00153 0.00131 0.00117 0.00122 0.00130 0.00065 H19 1.06830 0.25881 0.07855 1.00000 0.03154 0.00000 0.00000 C20 0.70181 -0.11160 0.26095 1.00000 0.02712 0.03148 0.03518 0.00507 0.00107 -0.00283 0.03126 0.00550 0.00042 0.00029 0.00015 0.00000 0.00149 0.00170 0.00165 0.00138 0.00131 0.00134 0.00072 H20A 0.71090 -0.19363 0.27745 1.00000 0.04689 0.00000 0.00000 H20B 0.60376 -0.10653 0.22852 1.00000 0.04689 0.00000 0.00000 H20C 0.67652 -0.05748 0.29786 1.00000 0.04689 0.00000 0.00000 N2 0.87153 -0.07765 0.22979 1.00000 0.02440 0.02659 0.02390 0.00053 -0.00090 0.00178 0.02496 0.00410 0.00032 0.00022 0.00011 0.00000 0.00119 0.00128 0.00112 0.00105 0.00102 0.00107 0.00054 O3 0.78327 0.36036 0.05798 1.00000 0.02816 0.02825 0.04797 0.01527 -0.00323 0.00106 0.03479 0.00407 0.00031 0.00020 0.00011 0.00000 0.00114 0.00117 0.00133 0.00101 0.00104 0.00097 0.00055 O4 0.54859 0.27248 0.10778 1.00000 0.02379 0.04085 0.04370 0.01244 0.00319 0.00408 0.03611 0.00395 0.00030 0.00020 0.00011 0.00000 0.00113 0.00129 0.00118 0.00104 0.00102 0.00104 0.00055 H2O 0.71063 0.40977 0.03883 1.00000 0.05417 0.06923 0.00470 0.00304 0.00183 0.00000 0.00000 Final Structure Factor Calculation for 2007may0006 in P2(1)2(1)2(1) Total number of l.s. parameters = 244 Maximum vector length = 511 Memory required = 2748 / 25046 wR2 = 0.1212 before cycle 7 for 2213 data and 2 / 244 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.051 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0646 * P )^2 + 0.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0465 for 1756 Fo > 4sig(Fo) and 0.0678 for all 2213 data wR2 = 0.1212, GooF = S = 1.050, Restrained GooF = 1.051 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 26.00 for non-hydrogen and 18.00 for hydrogen atoms Principal mean square atomic displacements U 0.0288 0.0236 0.0200 C1 0.0266 0.0223 0.0197 C2 0.0265 0.0236 0.0211 C3 0.0284 0.0218 0.0200 C4 0.0344 0.0319 0.0237 C5 0.0403 0.0312 0.0214 C6 0.0286 0.0251 0.0213 C7 0.0333 0.0245 0.0207 C8 0.0304 0.0238 0.0204 C9 0.0315 0.0225 0.0216 N1 0.0325 0.0312 0.0246 O1 0.0470 0.0317 0.0211 O2 0.0359 0.0244 0.0231 C10 0.0284 0.0263 0.0212 C11 0.0256 0.0226 0.0207 C12 0.0267 0.0216 0.0207 C13 0.0257 0.0222 0.0178 C14 0.0377 0.0259 0.0202 C15 0.0407 0.0249 0.0189 C16 0.0318 0.0244 0.0186 C17 0.0339 0.0273 0.0212 C18 0.0314 0.0244 0.0231 C19 0.0388 0.0305 0.0245 C20 0.0276 0.0247 0.0226 N2 0.0565 0.0287 0.0192 O3 0.0556 0.0299 0.0229 O4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.026 0.034 0.042 0.052 0.063 0.078 0.099 0.138 1.000 Number in group 231. 237. 229. 204. 223. 213. 215. 225. 215. 221. GooF 0.970 1.073 1.091 1.096 1.116 0.984 1.048 0.972 1.025 1.113 K 1.018 0.955 0.914 0.958 0.983 1.011 0.998 1.005 1.017 1.025 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.06 1.17 1.35 1.72 inf Number in group 228. 219. 221. 217. 224. 221. 221. 224. 215. 223. GooF 0.912 0.969 0.952 1.056 0.968 1.042 0.937 1.009 1.123 1.436 K 0.964 0.981 0.978 0.990 1.003 1.018 1.031 1.028 1.046 1.010 R1 0.203 0.153 0.110 0.106 0.069 0.051 0.038 0.039 0.038 0.040 Recommended weighting scheme: WGHT 0.0646 0.3475 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 1 3 15.56 43.02 5.78 0.040 5.78 6 10 5 0.38 40.08 4.10 0.039 0.81 1 6 0 395.04 291.51 3.99 0.104 1.81 5 10 1 -3.58 18.10 3.57 0.026 0.89 0 5 4 115.46 160.02 3.42 0.077 2.05 2 0 1 97.48 159.36 3.36 0.077 3.64 4 6 1 32.51 17.65 3.34 0.026 1.31 0 0 10 142.49 192.38 3.22 0.085 2.02 1 0 8 75.21 104.26 3.13 0.062 2.39 4 2 7 109.31 80.48 3.08 0.055 1.50 2 1 1 812.83 1009.66 3.03 0.194 3.46 4 4 5 479.00 382.55 2.99 0.119 1.44 3 10 10 6.53 19.45 2.97 0.027 0.91 0 5 6 68.53 47.48 2.93 0.042 1.87 1 0 7 269.65 339.67 2.92 0.112 2.69 1 1 0 605.66 779.60 2.87 0.170 6.17 5 7 13 157.74 108.12 2.84 0.063 0.89 0 9 12 25.84 46.16 2.83 0.041 1.00 2 9 14 -8.62 12.80 2.79 0.022 0.91 0 3 3 83.11 109.39 2.78 0.064 3.27 3 1 2 135.11 171.81 2.76 0.080 2.34 1 4 12 622.89 510.09 2.70 0.138 1.42 1 3 0 902.88 1098.98 2.69 0.202 3.33 6 7 1 8.35 19.76 2.69 0.027 0.98 6 4 7 68.55 96.66 2.66 0.060 1.05 4 0 7 15.43 5.41 2.65 0.014 1.56 4 7 9 44.01 64.04 2.65 0.049 1.07 6 4 19 0.89 29.89 2.61 0.033 0.77 6 8 4 28.74 46.32 2.60 0.041 0.91 0 4 0 2169.78 2644.46 2.58 0.313 2.80 0 8 2 9.54 0.64 2.57 0.005 1.39 4 1 6 41.14 25.10 2.57 0.031 1.61 4 0 2 400.63 324.21 2.56 0.110 1.82 1 3 13 102.11 78.33 2.54 0.054 1.41 3 1 0 213.30 170.64 2.53 0.080 2.41 6 8 5 51.07 78.30 2.50 0.054 0.90 0 3 8 546.14 455.48 2.49 0.130 2.09 8 3 1 11.77 1.87 2.49 0.008 0.90 1 0 5 772.39 921.79 2.47 0.185 3.55 3 5 20 2.84 15.78 2.47 0.024 0.86 0 0 6 60.40 78.66 2.46 0.054 3.37 8 4 1 2.26 19.47 2.45 0.027 0.88 3 8 17 223.50 172.39 2.41 0.080 0.85 2 8 15 35.01 55.46 2.39 0.045 0.94 4 6 11 116.31 147.67 2.38 0.074 1.07 1 2 0 1271.62 1503.79 2.31 0.236 4.47 6 1 20 47.88 92.92 2.29 0.059 0.78 5 5 11 50.15 70.10 2.29 0.051 1.03 3 11 3 213.54 171.16 2.28 0.080 0.93 9 3 0 36.79 7.85 2.27 0.017 0.80 Bond lengths and angles C1 - Distance Angles O1 1.2672 (0.0036) O2 1.2818 (0.0036) 123.09 (0.28) C2 1.4772 (0.0040) 118.58 (0.27) 118.33 (0.26) C1 - O1 O2 C2 - Distance Angles C3 1.3850 (0.0040) C9 1.4121 (0.0042) 121.44 (0.27) C1 1.4772 (0.0040) 117.99 (0.27) 120.53 (0.26) C2 - C3 C9 C3 - Distance Angles C2 1.3850 (0.0040) C4 1.3936 (0.0040) 116.74 (0.27) H3 0.9500 121.63 121.63 C3 - C2 C4 C4 - Distance Angles N1 1.3827 (0.0036) C3 1.3936 (0.0040) 128.41 (0.28) C7 1.4086 (0.0042) 108.47 (0.25) 123.11 (0.27) C4 - N1 C3 C5 - Distance Angles C6 1.3659 (0.0044) N1 1.3710 (0.0038) 110.75 (0.26) H5 0.9500 124.62 124.62 C5 - C6 N1 C6 - Distance Angles C5 1.3659 (0.0044) C7 1.4321 (0.0041) 106.70 (0.26) H6 0.9500 126.65 126.65 C6 - C5 C7 C7 - Distance Angles C4 1.4086 (0.0042) C8 1.4128 (0.0040) 118.98 (0.27) C6 1.4321 (0.0041) 106.41 (0.26) 134.61 (0.28) C7 - C4 C8 C8 - Distance Angles C9 1.3804 (0.0040) C7 1.4128 (0.0040) 118.26 (0.28) H8 0.9500 120.87 120.87 C8 - C9 C7 C9 - Distance Angles C8 1.3804 (0.0040) C2 1.4121 (0.0042) 121.47 (0.27) H9 0.9500 119.26 119.26 C9 - C8 C2 N1 - Distance Angles C5 1.3710 (0.0038) C4 1.3827 (0.0036) 107.66 (0.24) C10 1.4529 (0.0038) 125.98 (0.23) 126.36 (0.24) N1 - C5 C4 O1 - Distance Angles C1 1.2672 (0.0036) O1 - O2 - Distance Angles C1 1.2818 (0.0036) H1O 0.8787 (0.0188) 120.36 (2.71) O2 - C1 C10 - Distance Angles N1 1.4529 (0.0038) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - N1 H10A H10B C11 - Distance Angles O4 1.2693 (0.0038) O3 1.2765 (0.0036) 122.89 (0.28) C12 1.4819 (0.0040) 119.70 (0.27) 117.41 (0.27) C11 - O4 O3 C12 - Distance Angles C13 1.3864 (0.0039) C19 1.4084 (0.0041) 121.84 (0.27) C11 1.4819 (0.0040) 119.17 (0.26) 118.99 (0.26) C12 - C13 C19 C13 - Distance Angles C12 1.3864 (0.0039) C14 1.3948 (0.0040) 116.86 (0.26) H13 0.9500 121.57 121.57 C13 - C12 C14 C14 - Distance Angles N2 1.3794 (0.0037) C13 1.3948 (0.0040) 129.65 (0.26) C17 1.4213 (0.0040) 107.95 (0.25) 122.36 (0.27) C14 - N2 C13 C15 - Distance Angles C16 1.3648 (0.0042) N2 1.3758 (0.0038) 110.29 (0.25) H15 0.9500 124.85 124.85 C15 - C16 N2 C16 - Distance Angles C15 1.3648 (0.0042) C17 1.4327 (0.0042) 107.13 (0.26) H16 0.9500 126.44 126.44 C16 - C15 C17 C17 - Distance Angles C18 1.4019 (0.0040) C14 1.4213 (0.0040) 119.22 (0.27) C16 1.4327 (0.0042) 134.49 (0.28) 106.29 (0.26) C17 - C18 C14 C18 - Distance Angles C19 1.3837 (0.0041) C17 1.4019 (0.0040) 118.66 (0.27) H18 0.9500 120.67 120.67 C18 - C19 C17 C19 - Distance Angles C18 1.3837 (0.0041) C12 1.4084 (0.0041) 121.02 (0.28) H19 0.9500 119.49 119.49 C19 - C18 C12 C20 - Distance Angles N2 1.4557 (0.0038) H20A 0.9800 109.47 H20B 0.9800 109.47 109.47 H20C 0.9800 109.47 109.47 109.47 C20 - N2 H20A H20B N2 - Distance Angles C15 1.3758 (0.0038) C14 1.3794 (0.0037) 108.35 (0.23) C20 1.4557 (0.0038) 125.30 (0.24) 126.30 (0.24) N2 - C15 C14 O3 - Distance Angles C11 1.2765 (0.0036) H2O 0.8633 (0.0190) 118.48 (2.80) O3 - C11 O4 - Distance Angles C11 1.2693 (0.0038) O4 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.879(19) 1.76(2) 2.631(3) 173(4) O2-H1O...O4 0.863(19) 1.73(2) 2.590(3) 174(4) O3-H2O...O1 FMAP and GRID set by program FMAP 2 3 25 GRID -1.136 -2 -2 1.136 2 2 R1 = 0.0678 for 2212 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.23 at 0.4637 0.3138 0.0775 [ 0.80 A from H1O ] Deepest hole -0.24 at 0.9476 0.5180 0.1460 [ 0.08 A from H10C ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2636 / 19659 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4637 0.3138 0.0775 1.00000 0.05 0.23 0.80 H1O 0.99 O4 1.67 O2 1.94 C11 Q2 1 0.4440 0.9581 -0.1892 1.00000 0.05 0.21 0.90 H10C 1.17 C10 1.19 H10A 2.05 H10B Q3 1 0.6169 0.0631 0.1699 1.00000 0.05 0.21 0.51 H13 1.26 C13 2.18 C14 2.24 H20B Q4 1 0.7627 -0.1991 0.3045 1.00000 0.05 0.20 0.67 H20A 1.39 C20 1.72 H20C 2.19 N2 Q5 1 0.2752 0.7097 -0.0896 1.00000 0.05 0.20 0.53 C4 0.93 C3 1.67 H3 1.69 C7 Shortest distances between peaks (including symmetry equivalents) 1 4 2.92 Time profile in seconds ----------------------- 0.10: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.01: Generate connectivity array 0.02: 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 0.01: Analyse other restraints etc. 1.27: Read intensity data, sort/merge etc. 0.01: Set up constraints 0.03: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.53: Structure factors and derivatives 1.63: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 0.29: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.13: Fourier summations 0.01: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007may0006 finished at 12:02:43 Total CPU time: 5.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++