+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007may0003 started at 13:09:33 on 29-Sep-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007may0003 in C2/c CELL 0.71073 20.4199 9.0684 13.7141 90.000 132.070 90.000 ZERR 8.00 0.0005 0.0004 0.0003 0.000 0.001 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O UNIT 80 72 24 16 V = 1885.15 F(000) = 848.0 Mu = 0.10 mm-1 Cell Wt = 1625.62 Rho = 1.432 MERG 2 OMIT -3.00 55.00 DFIX 0.84 0.02 O1 H1O FMAP 2 PLAN 5 ACTA SIZE 0.08 0.04 0.1 EQIV $1 x, -y +1, z + 1/2 HTAB O1 N3_$1 BOND $H L.S. 6 TEMP -153.00 WGHT 0.016200 3.176700 EXTI 0.003801 FVAR 0.54447 C1 1 0.126187 0.104091 0.664412 11.00000 0.02001 0.01769 = 0.02286 -0.00042 0.01506 -0.00181 C2 1 0.092027 0.079019 0.536285 11.00000 0.01898 0.02134 = 0.02223 -0.00085 0.01439 -0.00250 C3 1 0.115151 -0.049908 0.511245 11.00000 0.02585 0.02664 = 0.02404 -0.00318 0.01706 -0.00125 AFIX 43 H3 2 0.091599 -0.068574 0.424751 11.00000 -1.20000 AFIX 0 C4 1 0.171810 -0.152223 0.609385 11.00000 0.03130 0.02303 = 0.03729 -0.00115 0.02552 0.00235 AFIX 43 H4 2 0.187486 -0.238993 0.590293 11.00000 -1.20000 AFIX 0 C5 1 0.205426 -0.127203 0.735420 11.00000 0.02455 0.02324 = 0.03026 0.00548 0.01781 0.00333 AFIX 43 H5 2 0.244456 -0.196576 0.803225 11.00000 -1.20000 AFIX 0 C6 1 0.181854 -0.000440 0.762175 11.00000 0.02278 0.02516 = 0.02127 0.00205 0.01376 -0.00051 AFIX 43 H6 2 0.203900 0.015381 0.848165 11.00000 -1.20000 AFIX 0 C7 1 0.105834 0.242049 0.699427 11.00000 0.02083 0.02305 = 0.02145 -0.00072 0.01489 -0.00183 C8 1 0.029453 0.182962 0.422243 11.00000 0.01808 0.02693 = 0.01884 0.00043 0.01134 -0.00151 AFIX 23 H8A 2 -0.007944 0.125789 0.339399 11.00000 -1.20000 H8B 2 -0.009752 0.229795 0.431857 11.00000 -1.20000 AFIX 0 C9 1 0.067062 0.443301 0.409292 11.00000 0.02680 0.02421 = 0.02091 0.00447 0.01708 0.00675 AFIX 43 H9 2 0.029533 0.494492 0.415805 11.00000 -1.20000 AFIX 0 C10 1 0.158196 0.390009 0.390300 11.00000 0.02545 0.02802 = 0.02536 0.00089 0.01796 0.00035 AFIX 43 H10 2 0.199614 0.400883 0.380133 11.00000 -1.20000 AFIX 0 N1 3 0.135071 0.260352 0.402062 11.00000 0.02410 0.02784 = 0.02742 0.00136 0.01875 0.00339 N2 3 0.075990 0.297910 0.414307 11.00000 0.01948 0.02443 = 0.01694 0.00154 0.01201 0.00234 N3 3 0.118279 0.507076 0.393818 11.00000 0.02872 0.02489 = 0.02101 0.00243 0.01692 0.00190 O1 4 0.125048 0.231929 0.812492 11.00000 0.05217 0.02376 = 0.02877 -0.00032 0.03160 0.00109 O2 4 0.076222 0.352770 0.632521 11.00000 0.03928 0.02546 = 0.02900 0.00657 0.02541 0.01012 H1O 2 0.120937 0.319211 0.837577 11.00000 0.05036 HKLF 4 Covalent radii and connectivity table for 2007may0003 in C2/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - C6 C2 C7 C2 - C3 C1 C8 C3 - C4 C2 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 - O2 O1 C1 C8 - N2 C2 C9 - N2 N3 C10 - N1 N3 N1 - C10 N2 N2 - C9 N1 C8 N3 - C9 C10 O1 - C7 O2 - C7 Operators for generating equivalent atoms: $1 x, -y+1, z+1/2 7121 Reflections read, of which 348 rejected -21 =< h =< 26, -6 =< k =< 11, -17 =< l =< 16, Max. 2-theta = 54.98 0 Systematic absence violations 0 Inconsistent equivalents 2131 Unique reflections, of which 0 suppressed R(int) = 0.0347 R(sigma) = 0.0446 Friedel opposites merged Maximum memory for data reduction = 1432 / 26582 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 = 1807 / 177390 wR2 = 0.1052 before cycle 1 for 2131 data and 141 / 141 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 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 0.049 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.086; Restrained GooF = 1.087 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0162 * P )^2 + 3.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54447 0.00154 0.003 OSF 2 0.00380 0.00062 0.000 EXTI Mean shift/esd = 0.002 Maximum = 0.006 for U23 N2 Max. shift = 0.000 A for H1O Max. dU = 0.000 for C5 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1807 / 177390 wR2 = 0.1052 before cycle 2 for 2131 data and 141 / 141 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 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 0.049 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.086; Restrained GooF = 1.087 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0162 * P )^2 + 3.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54447 0.00154 0.001 OSF 2 0.00380 0.00062 0.000 EXTI Mean shift/esd = 0.001 Maximum = 0.002 for U23 N2 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C9 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1807 / 177390 wR2 = 0.1052 before cycle 3 for 2131 data and 141 / 141 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 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 0.049 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.086; Restrained GooF = 1.087 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0162 * P )^2 + 3.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54447 0.00154 0.000 OSF 2 0.00380 0.00062 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x C1 Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 4 Maximum vector length = 511 Memory required = 1807 / 177390 wR2 = 0.1052 before cycle 4 for 2131 data and 141 / 141 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 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 0.049 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.086; Restrained GooF = 1.087 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0162 * P )^2 + 3.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54448 0.00154 0.000 OSF 2 0.00380 0.00062 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y N3 Max. shift = 0.000 A for H1O Max. dU = 0.000 for O2 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1807 / 177390 wR2 = 0.1052 before cycle 5 for 2131 data and 141 / 141 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 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 0.049 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.086; Restrained GooF = 1.087 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0162 * P )^2 + 3.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54447 0.00154 0.000 OSF 2 0.00380 0.00062 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C5 Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 6 Maximum vector length = 511 Memory required = 1807 / 177390 wR2 = 0.1052 before cycle 6 for 2131 data and 141 / 141 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 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 0.049 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.086; Restrained GooF = 1.087 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0162 * P )^2 + 3.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54448 0.00154 0.000 OSF 2 0.00380 0.00062 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C5 Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O Largest correlation matrix elements 0.790 U13 O1 / U33 O1 0.764 U13 C9 / U33 C9 0.748 U13 C8 / U33 C8 0.785 U13 O2 / U33 O2 0.764 U13 C2 / U33 C2 0.743 U13 C6 / U33 C6 0.782 U13 C4 / U33 C4 0.764 U13 N3 / U33 N3 0.743 U13 C10 / U11 C10 0.778 U13 O1 / U11 O1 0.761 U13 C3 / U33 C3 0.743 U13 N3 / U11 N3 0.771 U13 N1 / U33 N1 0.760 U13 C7 / U33 C7 0.741 U13 N1 / U11 N1 0.770 U13 C10 / U33 C10 0.754 U13 C5 / U33 C5 0.740 U13 C9 / U11 C9 0.767 U13 O2 / U11 O2 0.754 U13 C4 / U11 C4 0.738 U13 C3 / U11 C3 0.765 U13 C1 / U33 C1 0.751 U13 N2 / U33 N2 0.737 U13 C1 / U11 C1 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.0916 -0.0686 0.4248 43 0.950 0.000 C3 C4 C2 H4 0.1875 -0.2390 0.5903 43 0.950 0.000 C4 C5 C3 H5 0.2445 -0.1966 0.8032 43 0.950 0.000 C5 C4 C6 H6 0.2039 0.0154 0.8482 43 0.950 0.000 C6 C5 C1 H8A -0.0079 0.1258 0.3394 23 0.990 0.000 C8 N2 C2 H8B -0.0098 0.2298 0.4319 23 0.990 0.000 C8 N2 C2 H9 0.0295 0.4945 0.4158 43 0.950 0.000 C9 N2 N3 H10 0.1996 0.4009 0.3801 43 0.950 0.000 C10 N1 N3 2007may0003 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.12619 0.10409 0.66441 1.00000 0.02001 0.01769 0.02286 -0.00042 0.01506 -0.00181 0.01962 0.00447 0.00011 0.00020 0.00016 0.00000 0.00082 0.00095 0.00086 0.00068 0.00073 0.00068 0.00038 C2 0.09203 0.07902 0.53629 1.00000 0.01898 0.02134 0.02223 -0.00085 0.01439 -0.00250 0.02037 0.00447 0.00011 0.00021 0.00016 0.00000 0.00082 0.00097 0.00087 0.00070 0.00074 0.00071 0.00039 C3 0.11515 -0.04991 0.51124 1.00000 0.02585 0.02664 0.02404 -0.00318 0.01706 -0.00125 0.02523 0.00485 0.00012 0.00023 0.00018 0.00000 0.00091 0.00112 0.00092 0.00075 0.00080 0.00078 0.00043 H3 0.09160 -0.06857 0.42475 1.00000 0.03028 0.00000 0.00000 C4 0.17181 -0.15222 0.60938 1.00000 0.03130 0.02303 0.03729 -0.00115 0.02552 0.00235 0.02848 0.00526 0.00013 0.00023 0.00019 0.00000 0.00098 0.00108 0.00108 0.00082 0.00091 0.00081 0.00045 H4 0.18749 -0.23899 0.59029 1.00000 0.03418 0.00000 0.00000 C5 0.20543 -0.12720 0.73542 1.00000 0.02455 0.02324 0.03026 0.00548 0.01781 0.00333 0.02647 0.00503 0.00012 0.00023 0.00018 0.00000 0.00091 0.00103 0.00098 0.00078 0.00083 0.00077 0.00043 H5 0.24446 -0.19658 0.80323 1.00000 0.03177 0.00000 0.00000 C6 0.18185 -0.00044 0.76218 1.00000 0.02278 0.02516 0.02127 0.00205 0.01376 -0.00051 0.02388 0.00479 0.00011 0.00022 0.00017 0.00000 0.00087 0.00107 0.00087 0.00072 0.00076 0.00074 0.00042 H6 0.20390 0.01538 0.84817 1.00000 0.02866 0.00000 0.00000 C7 0.10583 0.24205 0.69943 1.00000 0.02083 0.02305 0.02145 -0.00072 0.01489 -0.00183 0.02119 0.00453 0.00011 0.00021 0.00017 0.00000 0.00083 0.00103 0.00087 0.00072 0.00074 0.00072 0.00040 C8 0.02945 0.18296 0.42224 1.00000 0.01808 0.02693 0.01884 0.00043 0.01134 -0.00152 0.02211 0.00453 0.00011 0.00022 0.00016 0.00000 0.00081 0.00107 0.00084 0.00072 0.00072 0.00074 0.00040 H8A -0.00794 0.12579 0.33940 1.00000 0.02654 0.00000 0.00000 H8B -0.00975 0.22979 0.43186 1.00000 0.02654 0.00000 0.00000 C9 0.06706 0.44330 0.40929 1.00000 0.02680 0.02421 0.02091 0.00447 0.01708 0.00675 0.02308 0.00483 0.00012 0.00022 0.00017 0.00000 0.00091 0.00103 0.00086 0.00072 0.00077 0.00076 0.00041 H9 0.02953 0.49449 0.41580 1.00000 0.02769 0.00000 0.00000 C10 0.15820 0.39001 0.39030 1.00000 0.02545 0.02802 0.02536 0.00089 0.01796 0.00035 0.02552 0.00489 0.00012 0.00023 0.00017 0.00000 0.00090 0.00114 0.00093 0.00077 0.00081 0.00079 0.00043 H10 0.19961 0.40088 0.38013 1.00000 0.03062 0.00000 0.00000 N1 0.13507 0.26035 0.40206 1.00000 0.02410 0.02784 0.02742 0.00136 0.01875 0.00339 0.02524 0.00416 0.00010 0.00019 0.00015 0.00000 0.00076 0.00095 0.00080 0.00067 0.00068 0.00067 0.00037 N2 0.07599 0.29791 0.41431 1.00000 0.01948 0.02443 0.01694 0.00154 0.01201 0.00234 0.02044 0.00378 0.00009 0.00018 0.00013 0.00000 0.00070 0.00087 0.00070 0.00059 0.00061 0.00062 0.00035 N3 0.11828 0.50708 0.39382 1.00000 0.02872 0.02489 0.02101 0.00243 0.01692 0.00190 0.02466 0.00407 0.00010 0.00018 0.00014 0.00000 0.00081 0.00092 0.00075 0.00063 0.00069 0.00067 0.00037 O1 0.12505 0.23193 0.81249 1.00000 0.05217 0.02376 0.02877 -0.00032 0.03160 0.00109 0.03127 0.00392 0.00010 0.00017 0.00013 0.00000 0.00089 0.00082 0.00073 0.00059 0.00070 0.00067 0.00036 O2 0.07622 0.35277 0.63252 1.00000 0.03928 0.02546 0.02900 0.00657 0.02541 0.01012 0.02919 0.00373 0.00009 0.00016 0.00013 0.00000 0.00078 0.00080 0.00071 0.00058 0.00065 0.00061 0.00035 H1O 0.12094 0.31921 0.83758 1.00000 0.05036 0.06314 0.00164 0.00218 0.00241 0.00000 0.00766 Final Structure Factor Calculation for 2007may0003 in C2/c Total number of l.s. parameters = 141 Maximum vector length = 511 Memory required = 1666 / 22995 wR2 = 0.1052 before cycle 7 for 2131 data and 0 / 141 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 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 0.049 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.086; Restrained GooF = 1.087 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0162 * P )^2 + 3.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0495 for 1639 Fo > 4sig(Fo) and 0.0721 for all 2131 data wR2 = 0.1052, GooF = S = 1.086, Restrained GooF = 1.087 for all data Occupancy sum of asymmetric unit = 15.00 for non-hydrogen and 9.00 for hydrogen atoms Principal mean square atomic displacements U 0.0229 0.0201 0.0159 C1 0.0230 0.0221 0.0161 C2 0.0288 0.0258 0.0211 C3 0.0374 0.0284 0.0197 C4 0.0344 0.0250 0.0200 C5 0.0283 0.0230 0.0203 C6 0.0241 0.0212 0.0183 C7 0.0279 0.0208 0.0177 C8 0.0324 0.0191 0.0177 C9 0.0283 0.0258 0.0225 C10 0.0300 0.0266 0.0192 N1 0.0254 0.0194 0.0165 N2 0.0301 0.0252 0.0186 N3 0.0528 0.0239 0.0170 O1 0.0447 0.0228 0.0201 O2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.023 0.035 0.048 0.063 0.082 0.104 0.135 0.200 1.000 Number in group 236. 197. 215. 211. 210. 215. 208. 213. 212. 214. GooF 1.070 1.255 1.088 1.200 1.116 1.049 0.978 1.033 0.957 1.090 K 2.515 1.435 0.926 1.011 0.981 0.982 0.982 1.008 1.009 1.009 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.31 1.64 inf Number in group 218. 210. 211. 213. 218. 209. 214. 216. 207. 215. GooF 1.268 1.224 1.132 1.045 1.007 0.965 1.034 0.911 0.925 1.264 K 1.082 1.047 1.043 1.002 1.012 0.999 0.991 1.002 1.018 1.003 R1 0.224 0.183 0.126 0.112 0.081 0.060 0.050 0.043 0.035 0.029 Recommended weighting scheme: WGHT 0.0142 3.2436 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) -26 2 11 114.08 1.11 4.25 0.006 0.77 -15 3 3 57.61 12.02 3.44 0.018 1.13 12 0 0 261.82 155.81 3.14 0.066 1.26 3 1 5 1613.21 1924.13 3.08 0.232 1.54 3 5 10 137.09 16.04 3.08 0.021 0.80 -6 8 7 -34.36 45.31 3.05 0.036 0.98 -12 2 5 12751.53 11720.08 2.96 0.574 1.59 -2 2 6 3020.15 2653.58 2.95 0.273 1.80 1 5 0 636.96 473.95 2.86 0.115 1.80 -11 9 4 172.11 91.71 2.84 0.051 0.88 -11 7 14 38.57 2.26 2.84 0.008 0.77 -21 5 6 24.32 83.68 2.83 0.048 0.82 -3 5 12 -1.65 53.24 2.77 0.039 0.84 -10 10 1 -17.91 54.10 2.76 0.039 0.80 -2 8 5 64.51 138.05 2.76 0.062 1.03 -13 9 5 774.22 480.23 2.75 0.116 0.85 -11 9 11 82.50 155.53 2.73 0.066 0.78 -18 6 9 -20.30 31.06 2.72 0.030 0.90 -1 3 2 56.28 117.83 2.67 0.058 2.72 -12 0 4 14.24 55.21 2.64 0.039 1.66 -16 8 9 -13.16 15.91 2.63 0.021 0.84 -4 0 8 3666.26 3265.44 2.63 0.303 1.56 -5 1 11 248.38 366.36 2.61 0.101 1.11 -22 2 5 187.50 311.45 2.60 0.094 0.83 -9 5 15 164.39 80.50 2.58 0.048 0.78 -11 5 4 44.34 9.32 2.57 0.016 1.29 -7 9 4 149.91 263.34 2.57 0.086 0.95 8 8 5 107.71 35.07 2.55 0.031 0.78 -18 6 6 72.24 21.55 2.55 0.025 0.89 -7 7 6 387.80 512.86 2.55 0.120 1.12 9 9 3 -31.98 30.22 2.54 0.029 0.78 -1 3 1 496.16 639.84 2.53 0.134 2.95 -12 6 5 26.70 76.30 2.51 0.046 1.13 -21 1 4 132.24 47.65 2.50 0.037 0.86 -17 1 17 462.05 304.78 2.50 0.093 0.80 -5 1 3 2400.06 2677.16 2.49 0.274 3.59 14 0 0 44.04 8.52 2.47 0.015 1.08 -5 3 1 804.41 666.32 2.46 0.137 2.33 -9 1 3 115.68 68.96 2.46 0.044 2.15 -7 1 2 121.79 75.31 2.46 0.046 2.65 0 0 2 14.80 47.91 2.46 0.037 5.09 -10 6 5 699.35 856.11 2.44 0.155 1.21 -7 1 8 851.97 715.91 2.43 0.142 1.67 -4 0 4 1.00 24.29 2.41 0.026 3.43 -5 1 15 45.51 0.94 2.39 0.005 0.78 14 2 1 17.98 0.20 2.35 0.002 0.98 -15 3 16 87.57 15.19 2.35 0.021 0.82 4 0 2 8.22 32.43 2.35 0.030 2.37 -5 1 13 15.99 50.25 2.34 0.038 0.92 9 1 7 35.31 0.78 2.33 0.005 0.85 Bond lengths and angles C1 - Distance Angles C6 1.3950 (0.0025) C2 1.4083 (0.0024) 119.53 (0.17) C7 1.4953 (0.0026) 118.86 (0.16) 121.59 (0.16) C1 - C6 C2 C2 - Distance Angles C3 1.3875 (0.0026) C1 1.4083 (0.0024) 118.60 (0.17) C8 1.5130 (0.0024) 117.44 (0.16) 123.94 (0.16) C2 - C3 C1 C3 - Distance Angles C4 1.3871 (0.0027) C2 1.3875 (0.0026) 121.63 (0.17) H3 0.9500 119.19 119.19 C3 - C4 C2 C4 - Distance Angles C5 1.3857 (0.0027) C3 1.3871 (0.0027) 119.65 (0.19) H4 0.9500 120.17 120.17 C4 - C5 C3 C5 - Distance Angles C4 1.3857 (0.0027) C6 1.3872 (0.0028) 119.73 (0.18) H5 0.9500 120.14 120.13 C5 - C4 C6 C6 - Distance Angles C5 1.3872 (0.0028) C1 1.3950 (0.0025) 120.84 (0.17) H6 0.9500 119.58 119.58 C6 - C5 C1 C7 - Distance Angles O2 1.2133 (0.0022) O1 1.3234 (0.0021) 123.35 (0.17) C1 1.4953 (0.0026) 123.67 (0.16) 112.97 (0.16) C7 - O2 O1 C8 - Distance Angles N2 1.4629 (0.0023) C2 1.5130 (0.0024) 112.34 (0.14) H8A 0.9900 109.14 109.14 H8B 0.9900 109.14 109.14 107.86 C8 - N2 C2 H8A C9 - Distance Angles N2 1.3265 (0.0025) N3 1.3307 (0.0024) 110.17 (0.16) H9 0.9500 124.91 124.91 C9 - N2 N3 C10 - Distance Angles N1 1.3166 (0.0026) N3 1.3588 (0.0025) 114.86 (0.16) H10 0.9500 122.57 122.57 C10 - N1 N3 N1 - Distance Angles C10 1.3166 (0.0026) N2 1.3679 (0.0020) 102.18 (0.15) N1 - C10 N2 - Distance Angles C9 1.3265 (0.0025) N1 1.3679 (0.0020) 110.06 (0.15) C8 1.4629 (0.0023) 129.68 (0.16) 120.13 (0.16) N2 - C9 N1 N3 - Distance Angles C9 1.3307 (0.0024) C10 1.3588 (0.0025) 102.73 (0.16) N3 - C9 O1 - Distance Angles C7 1.3234 (0.0021) H1O 0.8891 (0.0170) 111.15 (1.67) O1 - C7 O2 - Distance Angles C7 1.2133 (0.0022) O2 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.889(17) 1.771(17) 2.659(2) 177(3) O1-H1O...N3_$1 FMAP and GRID set by program FMAP 2 1 42 GRID -0.641 -2 -1 0.641 2 1 R1 = 0.0720 for 2131 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.30 at 0.0645 0.1354 0.4900 [ 0.71 A from C2 ] Deepest hole -0.23 at 0.0379 0.3937 0.4181 [ 0.82 A from C9 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 1869 / 35547 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0645 0.1354 0.4900 1.00000 0.05 0.30 0.71 C2 0.82 C8 1.43 H8B 1.54 H8A Q2 1 0.1158 0.1023 0.6043 1.00000 0.05 0.26 0.70 C1 0.74 C2 1.86 C6 1.87 C3 Q3 1 0.1351 0.1913 0.6860 1.00000 0.05 0.22 0.82 C1 0.87 C7 1.72 O2 1.90 C2 Q4 1 0.1540 0.0575 0.7092 1.00000 0.05 0.22 0.64 C1 0.76 C6 1.49 H6 1.80 C2 Q5 1 0.1760 -0.0774 0.5854 1.00000 0.05 0.21 0.78 C4 0.97 C3 1.48 H4 1.66 H3 Shortest distances between peaks (including symmetry equivalents) 2 4 1.16 1 2 1.20 2 3 1.21 3 4 1.25 1 3 2.09 2 5 2.16 1 4 2.35 4 5 2.37 1 5 2.57 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.01: Interpret restraints etc. 0.00: Generate connectivity array 0.01: 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. 0.61: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.66: Structure factors and derivatives 1.09: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.04: Apply other restraints 0.21: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.01: Merge reflections for Fourier and .fcf 0.20: Fourier summations 0.04: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007may0003 finished at 13:09:45 Total CPU time: 3.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++