+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 02src630 started at 11:21:18 on 02-Dec-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02SRC630 in C2/c CELL 0.71073 25.2246 6.2785 10.9206 90.000 94.662 90.000 ZERR 4.00 0.0023 0.0007 0.0011 0.000 0.007 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O UNIT 64 144 8 8 V = 1723.80 F(000) = 648.0 Mu = 0.07 mm-1 Cell Wt = 1153.87 Rho = 1.112 MERG 2 SHEL 7 0.9 ISOR 0.05 $C $O $N FREE C6 H5 FMAP 2 PLAN 25 SIZE 0.03 0.03 0.10 ACTA BOND $H WGHT 0.17020 10.17730 L.S. 10 TEMP -153.00 FVAR 0.30270 N1 3 0.967242 0.118352 0.077719 11.00000 0.06720 0.20442 = 0.10461 -0.10756 -0.02752 0.06194 AFIX 13 H1N 2 0.992925 0.174222 0.134738 11.00000 -1.20000 AFIX 0 O1 4 0.937763 0.354502 0.288620 11.00000 0.05152 0.15185 = 0.09193 -0.04358 0.00175 0.00299 AFIX 147 H1 2 0.963151 0.268698 0.301560 11.00000 -1.50000 AFIX 0 C1 1 0.803159 0.267906 0.120565 11.00000 0.05871 0.21821 = 0.08954 -0.06156 0.00134 -0.00213 AFIX 137 H1A 2 0.767583 0.303855 0.144183 11.00000 -1.50000 H1B 2 0.805822 0.113463 0.109609 11.00000 -1.50000 H1C 2 0.809332 0.339786 0.043344 11.00000 -1.50000 AFIX 0 C2 1 0.830880 0.245718 0.342629 11.00000 0.05859 0.10712 = 0.08966 -0.00111 0.00880 0.00549 AFIX 137 H2A 2 0.856872 0.293333 0.408526 11.00000 -1.50000 H2B 2 0.831557 0.089929 0.337419 11.00000 -1.50000 H2C 2 0.795249 0.292848 0.360233 11.00000 -1.50000 AFIX 0 C3 1 0.842674 0.579398 0.229717 11.00000 0.06174 0.13353 = 0.08536 0.01376 0.00698 -0.00157 AFIX 137 H3A 2 0.807379 0.623287 0.251616 11.00000 -1.50000 H3B 2 0.849553 0.641783 0.150288 11.00000 -1.50000 H3C 2 0.869710 0.628776 0.292872 11.00000 -1.50000 AFIX 0 C4 1 0.844794 0.340486 0.221083 11.00000 0.05037 0.10410 = 0.05950 -0.02563 0.01103 -0.00117 C5 1 0.901020 0.272824 0.194429 11.00000 0.04655 0.26607 = 0.11238 -0.11756 0.01314 0.00135 AFIX 13 H5 2 0.898206 0.131589 0.235731 11.00000 -1.20000 AFIX 0 C6 1 0.914636 0.197234 0.103443 11.00000 0.07218 0.41408 = 0.18884 -0.20144 -0.02694 0.08473 AFIX 23 H6A 2 0.905301 0.304387 0.038753 11.00000 -1.20000 H6B 2 0.890232 0.075728 0.085375 11.00000 -1.20000 AFIX 0 C7 1 0.970395 -0.113100 0.078773 11.00000 0.08621 0.20702 = 0.07943 -0.07500 -0.01426 0.03997 AFIX 23 H7A 2 0.941917 -0.171484 0.020573 11.00000 -1.20000 H7B 2 0.964325 -0.165761 0.161932 11.00000 -1.20000 AFIX 0 C8 1 1.023349 -0.192398 0.043954 11.00000 0.10820 0.16679 = 0.08875 -0.07801 -0.04660 0.06325 AFIX 23 H8A 2 1.051917 -0.140014 0.103959 11.00000 -1.20000 H8B 2 1.023853 -0.350040 0.045709 11.00000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 02SRC630 in C2/c C 0.770 H 0.320 N 0.700 O 0.660 N1 - C8_$1 C7 C6 O1 - C5 C1 - C4 C2 - C4 C3 - C4 C4 - C3 C2 C1 C5 C5 - C6 O1 C4 C6 - C5 N1 C7 - N1 C8 C8 - N1_$1 C7 Operators for generating equivalent atoms: $1 -x+2, -y, -z 6721 Reflections read, of which 1591 rejected -25 =< h =< 27, -6 =< k =< 6, -12 =< l =< 12, Max. 2-theta = 46.50 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) -16 2 9 0.29 0.75 3 6.51 12 2 9 2.50 0.61 4 3.91 2 Inconsistent equivalents 1223 Unique reflections, of which 0 suppressed R(int) = 0.0538 R(sigma) = 0.0531 Friedel opposites merged Maximum memory for data reduction = 1569 / 14484 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 = 1892 / 124835 wR2 = 0.4144 before cycle 1 for 1223 data and 95 / 95 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.1549 0.0500 ISOR U11 C6 -0.1870 0.0500 ISOR U22 C6 0.2014 0.0500 ISOR U23 C6 Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 60. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.050 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.064 0.000 GooF = S = 1.103; Restrained GooF = 1.117 for 60 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1702 * P )^2 + 10.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30270 0.00393 0.001 OSF Mean shift/su = 0.000 Maximum = -0.002 for x O1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for C5 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1892 / 124835 wR2 = 0.4144 before cycle 2 for 1223 data and 95 / 95 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.1549 0.0500 ISOR U11 C6 -0.1870 0.0500 ISOR U22 C6 0.2014 0.0500 ISOR U23 C6 Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 60. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.050 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.064 0.000 GooF = S = 1.103; Restrained GooF = 1.117 for 60 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1702 * P )^2 + 10.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30270 0.00393 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for x O1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for C6 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1892 / 124835 wR2 = 0.4144 before cycle 3 for 1223 data and 95 / 95 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 0.1549 0.0500 ISOR U11 C6 -0.1870 0.0500 ISOR U22 C6 0.2014 0.0500 ISOR U23 C6 Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 60. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.050 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.064 0.000 GooF = S = 1.103; Restrained GooF = 1.117 for 60 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1702 * P )^2 + 10.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30270 0.00393 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for U23 N1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for C6 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1892 / 124835 wR2 = 0.4144 before cycle 4 for 1223 data and 95 / 95 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.1549 0.0500 ISOR U11 C6 -0.1870 0.0500 ISOR U22 C6 0.2015 0.0500 ISOR U23 C6 Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 60. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.050 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.064 0.000 GooF = S = 1.103; Restrained GooF = 1.117 for 60 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1702 * P )^2 + 10.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30270 0.00393 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for U23 C5 Max. shift = 0.000 A for H2B Max. dU = 0.000 for C5 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1892 / 124835 wR2 = 0.4144 before cycle 5 for 1223 data and 95 / 95 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 0.1549 0.0500 ISOR U11 C6 -0.1870 0.0500 ISOR U22 C6 0.2015 0.0500 ISOR U23 C6 Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 60. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.050 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.064 0.000 GooF = S = 1.103; Restrained GooF = 1.117 for 60 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1702 * P )^2 + 10.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30270 0.00393 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x C2 Max. shift = 0.000 A for H2B Max. dU = 0.000 for C5 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1892 / 124835 wR2 = 0.4144 before cycle 6 for 1223 data and 95 / 95 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint 0.1549 0.0500 ISOR U11 C6 -0.1870 0.0500 ISOR U22 C6 0.2015 0.0500 ISOR U23 C6 Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 60. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.050 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.064 0.000 GooF = S = 1.103; Restrained GooF = 1.117 for 60 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1702 * P )^2 + 10.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30270 0.00393 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x C1 Max. shift = 0.000 A for H1A Max. dU = 0.000 for C6 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1892 / 124835 wR2 = 0.4144 before cycle 7 for 1223 data and 95 / 95 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint 0.1549 0.0500 ISOR U11 C6 -0.1870 0.0500 ISOR U22 C6 0.2015 0.0500 ISOR U23 C6 Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 60. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.050 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.064 0.000 GooF = S = 1.103; Restrained GooF = 1.117 for 60 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1702 * P )^2 + 10.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30270 0.00393 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x C2 Max. shift = 0.000 A for H2B Max. dU = 0.000 for C8 Least-squares cycle 8 Maximum vector length = 511 Memory required = 1892 / 124835 wR2 = 0.4144 before cycle 8 for 1223 data and 95 / 95 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint 0.1549 0.0500 ISOR U11 C6 -0.1870 0.0500 ISOR U22 C6 0.2015 0.0500 ISOR U23 C6 Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 60. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.050 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.064 0.000 GooF = S = 1.103; Restrained GooF = 1.117 for 60 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1702 * P )^2 + 10.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30270 0.00393 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x C2 Max. shift = 0.000 A for H1B Max. dU = 0.000 for C1 Least-squares cycle 9 Maximum vector length = 511 Memory required = 1892 / 124835 wR2 = 0.4144 before cycle 9 for 1223 data and 95 / 95 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint 0.1549 0.0500 ISOR U11 C6 -0.1870 0.0500 ISOR U22 C6 0.2015 0.0500 ISOR U23 C6 Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 60. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.050 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.064 0.000 GooF = S = 1.103; Restrained GooF = 1.117 for 60 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1702 * P )^2 + 10.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30270 0.00393 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x C2 Max. shift = 0.000 A for H3A Max. dU = 0.000 for C5 Least-squares cycle 10 Maximum vector length = 511 Memory required = 1892 / 124835 wR2 = 0.4144 before cycle 10 for 1223 data and 95 / 95 parameters Disagreeable restraints before cycle 10 Observed Target Error Sigma Restraint 0.1549 0.0500 ISOR U11 C6 -0.1870 0.0500 ISOR U22 C6 0.2015 0.0500 ISOR U23 C6 Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 60. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.050 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.064 0.000 GooF = S = 1.103; Restrained GooF = 1.117 for 60 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1702 * P )^2 + 10.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30270 0.00393 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H2B Max. dU = 0.000 for C6 Largest correlation matrix elements -0.674 U23 C6 / U22 C6 -0.578 U23 N1 / U33 N1 -0.518 U23 N1 / U22 N1 -0.643 U23 C6 / U33 C6 -0.541 U12 C6 / U13 C6 -0.504 U23 C8 / U22 C8 -0.596 U23 C5 / U22 C5 -0.539 U23 C5 / U33 C5 -0.579 z C6 / y C6 -0.522 z C5 / y C5 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1N 0.9929 0.1742 0.1347 13 0.930 0.000 N1 C8_$1 C7 C6 H1 0.9631 0.2687 0.3016 147 0.840 0.000 O1 C5 H1 H1A 0.7676 0.3039 0.1442 137 0.980 0.000 C1 C4 H1A H1B 0.8058 0.1135 0.1096 137 0.980 0.000 C1 C4 H1A H1C 0.8093 0.3398 0.0433 137 0.980 0.000 C1 C4 H1A H2A 0.8569 0.2933 0.4085 137 0.980 0.000 C2 C4 H2A H2B 0.8316 0.0899 0.3374 137 0.980 0.000 C2 C4 H2A H2C 0.7952 0.2928 0.3602 137 0.980 0.000 C2 C4 H2A H3A 0.8074 0.6233 0.2516 137 0.980 0.000 C3 C4 H3A H3B 0.8496 0.6418 0.1503 137 0.980 0.000 C3 C4 H3A H3C 0.8697 0.6288 0.2929 137 0.980 0.000 C3 C4 H3A H5 0.8982 0.1316 0.2357 13 1.000 0.000 C5 C6 O1 C4 H6A 0.9053 0.3044 0.0388 23 0.990 0.000 C6 C5 N1 H6B 0.8902 0.0757 0.0854 23 0.990 0.000 C6 C5 N1 H7A 0.9419 -0.1715 0.0206 23 0.990 0.000 C7 N1 C8 H7B 0.9643 -0.1658 0.1619 23 0.990 0.000 C7 N1 C8 H8A 1.0519 -0.1400 0.1040 23 0.990 0.000 C8 N1_$1 C7 H8B 1.0239 -0.3500 0.0457 23 0.990 0.000 C8 N1_$1 C7 02SRC630 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq N1 0.96724 0.11835 0.07772 1.00000 0.06721 0.20442 0.10461 -0.10756 -0.02752 0.06195 0.12729 0.01327 0.00028 0.00168 0.00076 0.00000 0.00453 0.00957 0.00649 0.00654 0.00396 0.00526 0.00394 H1N 0.99293 0.17422 0.13474 1.00000 0.15275 0.00000 0.00000 O1 0.93776 0.35450 0.28862 1.00000 0.05152 0.15186 0.09193 -0.04357 0.00175 0.00299 0.09866 0.00917 0.00020 0.00112 0.00055 0.00000 0.00316 0.00594 0.00403 0.00399 0.00269 0.00315 0.00238 H1 0.96315 0.26869 0.30157 1.00000 0.14799 0.00000 0.00000 C1 0.80316 0.26791 0.12057 1.00000 0.05871 0.21821 0.08954 -0.06156 0.00134 -0.00213 0.12241 0.01573 0.00033 0.00216 0.00087 0.00000 0.00503 0.01174 0.00632 0.00717 0.00445 0.00607 0.00417 H1A 0.76758 0.30386 0.14418 1.00000 0.18361 0.00000 0.00000 H1B 0.80582 0.11346 0.10961 1.00000 0.18361 0.00000 0.00000 H1C 0.80933 0.33979 0.04334 1.00000 0.18361 0.00000 0.00000 C2 0.83088 0.24572 0.34263 1.00000 0.05859 0.10711 0.08966 -0.00111 0.00880 0.00549 0.08497 0.01571 0.00031 0.00152 0.00078 0.00000 0.00458 0.00655 0.00591 0.00476 0.00407 0.00424 0.00263 H2A 0.85687 0.29334 0.40853 1.00000 0.12746 0.00000 0.00000 H2B 0.83156 0.08993 0.33742 1.00000 0.12746 0.00000 0.00000 H2C 0.79525 0.29284 0.36023 1.00000 0.12746 0.00000 0.00000 C3 0.84267 0.57940 0.22972 1.00000 0.06174 0.13354 0.08536 0.01375 0.00697 -0.00158 0.09349 0.01665 0.00032 0.00163 0.00082 0.00000 0.00506 0.00866 0.00582 0.00550 0.00413 0.00498 0.00293 H3A 0.80738 0.62329 0.25162 1.00000 0.14024 0.00000 0.00000 H3B 0.84955 0.64178 0.15029 1.00000 0.14024 0.00000 0.00000 H3C 0.86971 0.62878 0.29287 1.00000 0.14024 0.00000 0.00000 C4 0.84479 0.34049 0.22108 1.00000 0.05038 0.10410 0.05950 -0.02563 0.01104 -0.00117 0.07096 0.01237 0.00027 0.00140 0.00063 0.00000 0.00415 0.00652 0.00425 0.00413 0.00316 0.00390 0.00228 C5 0.90102 0.27282 0.19443 1.00000 0.04656 0.26606 0.11239 -0.11757 0.01313 0.00134 0.14130 0.01592 0.00032 0.00241 0.00101 0.00000 0.00480 0.01398 0.00728 0.00893 0.00460 0.00624 0.00524 H5 0.89821 0.13159 0.23573 1.00000 0.16957 0.00000 0.00000 C6 0.91464 0.19723 0.10344 1.00000 0.07218 0.41408 0.18885 -0.20145 -0.02694 0.08473 0.22709 0.02282 0.00044 0.00326 0.00145 0.00000 0.00683 0.02358 0.01272 0.01512 0.00756 0.01043 0.00966 H6A 0.90530 0.30439 0.03875 1.00000 0.27250 0.00000 0.00000 H6B 0.89023 0.07573 0.08537 1.00000 0.27250 0.00000 0.00000 C7 0.97039 -0.11310 0.07877 1.00000 0.08621 0.20703 0.07943 -0.07500 -0.01426 0.03997 0.12537 0.01747 0.00038 0.00213 0.00085 0.00000 0.00654 0.01240 0.00620 0.00743 0.00479 0.00730 0.00449 H7A 0.94192 -0.17148 0.02057 1.00000 0.15044 0.00000 0.00000 H7B 0.96433 -0.16576 0.16193 1.00000 0.15044 0.00000 0.00000 C8 1.02335 -0.19240 0.04395 1.00000 0.10820 0.16679 0.08875 -0.07802 -0.04660 0.06325 0.12423 0.01632 0.00040 0.00187 0.00092 0.00000 0.00742 0.01010 0.00684 0.00687 0.00549 0.00687 0.00452 H8A 1.05192 -0.14001 0.10396 1.00000 0.14907 0.00000 0.00000 H8B 1.02385 -0.35004 0.04571 1.00000 0.14907 0.00000 0.00000 Final Structure Factor Calculation for 02SRC630 in C2/c Total number of l.s. parameters = 95 Maximum vector length = 511 Memory required = 1797 / 22995 wR2 = 0.4144 before cycle 11 for 1223 data and 0 / 95 parameters Disagreeable restraints before cycle 11 Observed Target Error Sigma Restraint 0.1549 0.0500 ISOR U11 C6 -0.1870 0.0500 ISOR U22 C6 0.2015 0.0500 ISOR U23 C6 Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 60. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.050 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.064 0.000 GooF = S = 1.103; Restrained GooF = 1.117 for 60 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1702 * P )^2 + 10.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1386 for 700 Fo > 4sig(Fo) and 0.1942 for all 1223 data wR2 = 0.4144, GooF = S = 1.103, Restrained GooF = 1.117 for all data Occupancy sum of asymmetric unit = 10.00 for non-hydrogen and 18.00 for hydrogen atoms Principal mean square atomic displacements U 0.3007 0.0493 0.0320 N1 may be split into 0.9697 0.1503 0.0656 and 0.9648 0.0864 0.0898 0.1754 0.0692 0.0514 O1 0.2430 0.0673 0.0569 C1 may be split into 0.8029 0.2989 0.1134 and 0.8034 0.2369 0.1278 0.1078 0.0897 0.0574 C2 0.1373 0.0817 0.0615 C3 0.1158 0.0546 0.0425 C4 0.3299 0.0559 0.0381 C5 may be split into 0.9005 0.3095 0.1830 and 0.9015 0.2362 0.2059 0.5571 0.0788 0.0454 C6 may be split into 0.9166 0.2437 0.0874 and 0.9127 0.1507 0.1195 0.2570 0.0743 0.0448 C7 may be split into 0.9723 -0.0835 0.0705 and 0.9685 -0.1427 0.0871 0.2667 0.0679 0.0381 C8 may be split into 1.0271 -0.1668 0.0335 and 1.0196 -0.2180 0.0544 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.005 0.009 0.014 0.020 0.028 0.039 0.056 0.080 0.133 1.000 Number in group 151. 105. 116. 127. 122. 113. 125. 121. 121. 122. GooF 1.153 1.030 0.888 1.162 0.946 1.209 1.132 1.239 1.212 0.973 K 27.322 5.395 2.236 1.706 1.236 1.133 0.986 1.031 1.041 0.996 Resolution(A) 0.90 0.93 0.97 1.02 1.07 1.14 1.23 1.35 1.53 1.94 inf Number in group 123. 126. 119. 121. 123. 125. 122. 119. 123. 122. GooF 0.983 0.861 1.059 1.227 1.368 1.164 1.240 1.026 1.073 0.935 K 1.552 1.224 1.231 1.280 1.061 1.217 1.084 1.015 1.113 0.967 R1 0.481 0.411 0.394 0.378 0.307 0.245 0.200 0.188 0.123 0.075 Recommended weighting scheme: WGHT 0.1703 10.1724 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)/su Fc/Fc(max) Resolution(A) -2 4 5 227.91 7.16 6.16 0.017 1.27 -5 5 5 124.43 0.45 4.89 0.004 1.07 0 4 7 79.73 1.23 4.10 0.007 1.10 -2 4 6 112.36 0.03 4.06 0.001 1.19 -3 3 3 89.45 5.64 3.95 0.015 1.79 -4 4 4 68.31 333.51 3.84 0.116 1.34 -3 5 7 150.47 27.52 3.66 0.033 0.98 -5 5 3 287.99 98.21 3.48 0.063 1.16 6 4 6 111.28 19.74 3.41 0.028 1.13 -7 5 3 61.11 0.03 3.40 0.001 1.14 -13 3 7 507.18 210.98 3.38 0.092 1.08 0 4 6 0.00 96.31 3.18 0.062 1.19 -1 5 6 68.55 0.33 3.18 0.004 1.03 -15 3 7 257.50 96.46 3.09 0.062 1.03 -4 4 3 9.15 92.88 2.77 0.061 1.41 2 4 8 59.48 3.93 2.71 0.013 1.02 -3 5 6 53.19 6.56 2.70 0.016 1.03 -9 5 3 165.01 60.86 2.69 0.050 1.10 -22 4 3 94.08 18.85 2.65 0.028 0.91 -7 3 1 110.73 34.62 2.62 0.037 1.80 -15 3 6 118.77 295.28 2.60 0.109 1.09 -11 3 8 20.08 106.70 2.58 0.066 1.05 -12 4 2 247.67 113.05 2.56 0.068 1.24 -10 4 4 457.36 242.28 2.53 0.099 1.22 -1 3 1 9.52 76.83 2.47 0.056 2.05 -14 4 7 36.11 1.32 2.47 0.007 0.97 11 5 1 48.33 6.33 2.43 0.016 1.09 4 4 8 57.19 1.72 2.39 0.008 1.00 1 1 9 404.49 218.06 2.38 0.094 1.18 -18 2 6 375.09 198.28 2.37 0.089 1.08 -3 3 6 286.92 145.88 2.36 0.077 1.37 -22 2 3 56.08 2.22 2.36 0.009 1.05 -9 5 1 27.44 0.00 2.35 0.000 1.14 -17 3 5 459.36 256.23 2.34 0.102 1.09 6 6 2 32.73 0.09 2.34 0.002 0.99 -5 3 5 83.72 25.85 2.33 0.032 1.47 -5 3 6 73.75 20.81 2.33 0.029 1.34 14 0 8 244.51 119.16 2.29 0.069 1.04 -2 0 12 57.41 8.73 2.28 0.019 0.91 1 3 6 7.64 65.69 2.28 0.052 1.36 6 0 10 529.57 298.87 2.27 0.110 1.03 -15 3 5 137.30 54.42 2.26 0.047 1.15 -2 0 6 1604.93 1022.97 2.24 0.203 1.82 -6 4 6 112.39 42.46 2.24 0.041 1.16 -10 0 10 5.73 61.18 2.23 0.050 1.03 2 4 7 -7.64 30.28 2.16 0.035 1.09 10 4 1 -1.92 37.00 2.16 0.039 1.31 -4 4 8 66.06 16.77 2.14 0.026 1.02 4 0 0 1276.01 823.87 2.11 0.182 6.29 8 2 5 111.90 45.91 2.10 0.043 1.51 Bond lengths and angles N1 - Distance Angles C8_$1 1.4454 (0.0151) C7 1.4553 (0.0140) 108.39 (0.69) C6 1.4648 (0.0124) 106.65 (1.06) 112.70 (1.23) H1N 0.9300 109.67 109.68 109.67 N1 - C8_$1 C7 C6 O1 - Distance Angles C5 1.4230 (0.0096) H1 0.8400 109.47 O1 - C5 C1 - Distance Angles C4 1.5258 (0.0105) H1A 0.9800 109.47 H1B 0.9800 109.47 109.47 H1C 0.9800 109.47 109.47 109.47 C1 - C4 H1A H1B C2 - Distance Angles C4 1.5215 (0.0112) H2A 0.9800 109.47 H2B 0.9800 109.47 109.47 H2C 0.9800 109.47 109.47 109.47 C2 - C4 H2A H2B C3 - Distance Angles C4 1.5042 (0.0117) H3A 0.9800 109.47 H3B 0.9800 109.47 109.47 H3C 0.9800 109.47 109.47 109.47 C3 - C4 H3A H3B C4 - Distance Angles C3 1.5042 (0.0117) C2 1.5215 (0.0112) 108.87 (0.66) C1 1.5258 (0.0105) 108.48 (0.80) 108.47 (0.73) C5 1.5309 (0.0111) 109.08 (0.82) 109.90 (0.84) 111.99 (0.63) C4 - C3 C2 C1 C5 - Distance Angles C6 1.1773 (0.0132) O1 1.4230 (0.0096) 122.53 (0.90) C4 1.5309 (0.0111) 127.64 (0.92) 108.76 (0.64) H5 1.0000 93.41 93.41 93.41 C5 - C6 O1 C4 C6 - Distance Angles C5 1.1773 (0.0132) N1 1.4648 (0.0124) 128.99 (1.09) H6A 0.9900 105.04 105.04 H6B 0.9900 105.04 105.04 105.87 C6 - C5 N1 H6A C7 - Distance Angles N1 1.4553 (0.0140) C8 1.5031 (0.0130) 112.20 (1.06) H7A 0.9900 109.17 109.17 H7B 0.9900 109.17 109.17 107.88 C7 - N1 C8 H7A C8 - Distance Angles N1_$1 1.4454 (0.0151) C7 1.5031 (0.0130) 109.98 (0.79) H8A 0.9900 109.67 109.67 H8B 0.9900 109.67 109.67 108.17 C8 - N1_$1 C7 H8A FMAP and GRID set by program FMAP 2 2 9 GRID -4.167 -2 -1 4.167 2 1 R1 = 0.1942 for 1223 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.49 at 0.0800 0.2694 0.4251 [ 0.56 A from H6A ] Deepest hole -0.40 at 0.0823 0.2146 0.3610 [ 0.41 A from C6 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2291 / 17817 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9200 0.2694 0.0749 1.00000 0.05 0.49 0.56 H6A 0.57 C6 1.43 C5 1.44 H6B Q2 1 0.9111 0.0906 0.1661 1.00000 0.05 0.43 0.89 H5 0.97 C6 0.99 H6B 1.22 C5 Q3 1 0.8862 0.1198 0.0170 1.00000 0.05 0.32 0.80 H6B 1.24 C6 1.27 H6A 2.10 N1 Q4 1 0.9364 0.4304 0.2056 1.00000 0.05 0.29 1.02 O1 1.33 C5 1.57 H1 1.89 C6 Q5 1 0.9193 0.4926 0.0713 1.00000 0.05 0.26 1.28 H6A 1.89 C6 2.01 C5 2.19 H8B Q6 1 0.9474 -0.2480 0.0620 1.00000 0.05 0.25 0.67 H7A 1.03 C7 1.25 H7B 1.97 C8 Q7 1 0.9689 0.1540 0.0265 1.00000 0.05 0.23 0.61 N1 0.84 C8 1.29 H1N 1.48 H8A Q8 1 0.8962 -0.0091 0.2389 1.00000 0.05 0.22 0.89 H5 1.75 H6B 1.84 C5 2.05 C6 Q9 1 0.9659 -0.0537 0.0620 1.00000 0.05 0.22 0.43 C7 1.04 H7A 1.09 N1 1.30 H7B Q10 1 1.0103 -0.2672 0.0606 1.00000 0.05 0.20 0.61 C8 0.65 H8B 1.37 H8A 1.42 C7 Q11 1 1.0383 -0.2199 0.1254 1.00000 0.05 0.17 0.66 H8A 0.95 C8 1.23 H8B 1.87 C7 Q12 1 0.8822 0.7398 0.2578 1.00000 0.05 0.17 0.87 H3C 1.43 C3 1.51 H3B 2.02 H3A Q13 1 0.8673 0.6322 0.3358 1.00000 0.05 0.17 0.48 H3C 1.31 C3 1.71 H3A 2.04 H3B Q14 1 0.8477 0.6949 0.1670 1.00000 0.05 0.16 0.38 H3B 1.01 C3 1.50 H3A 1.50 H3C Q15 1 0.8486 0.0819 0.0088 1.00000 0.05 0.16 1.29 H6B 1.62 H1B 1.95 H1C 2.01 H6A Q16 1 0.8781 0.3202 0.4360 1.00000 0.05 0.16 0.61 H2A 1.57 C2 2.02 H7A 2.10 H2B Q17 1 0.8337 -0.1568 0.3336 1.00000 0.05 0.15 1.55 H2B 1.70 H3C 1.75 H3A 2.03 C3 Q18 1 0.7581 0.1192 0.0046 1.00000 0.05 0.14 1.59 H1B 1.76 H1C 1.77 H1A 1.88 C1 Q19 1 0.9519 -0.3260 0.1967 1.00000 0.05 0.14 1.13 H7B 1.94 C7 2.15 H7A 2.28 O1 Q20 1 0.7855 0.0426 0.2235 1.00000 0.05 0.14 1.45 H1B 1.66 H2B 1.88 C1 1.89 H1A Q21 1 1.0155 -0.5022 0.1019 1.00000 0.05 0.14 1.16 H8B 1.84 H1 1.84 O1 2.05 H8B Q22 1 0.9217 -0.0873 -0.0645 1.00000 0.05 0.13 1.15 H7A 1.65 H8A 1.92 C7 2.09 H2A Q23 1 0.9298 0.4506 0.3596 1.00000 0.05 0.13 1.02 O1 1.58 H1 1.95 H8B 1.98 H3C Q24 1 0.7810 0.3521 0.3436 1.00000 0.05 0.13 0.54 H2C 1.43 C2 2.02 H2A 2.09 H2B Q25 1 0.8829 0.3921 0.3880 1.00000 0.05 0.13 0.94 H2A 1.65 C2 1.83 H3C 1.84 O1 Shortest distances between peaks (including symmetry equivalents) 16 25 0.71 3 15 0.97 10 11 1.00 2 8 1.10 12 13 1.17 12 14 1.29 23 25 1.30 6 9 1.31 7 10 1.33 7 9 1.36 1 3 1.39 1 5 1.40 21 23 1.44 1 2 1.53 4 5 1.54 6 19 1.54 10 21 1.54 1 7 1.56 13 17 1.57 4 19 1.58 6 10 1.59 8 12 1.63 13 25 1.65 12 17 1.66 18 18 1.69 7 11 1.71 2 3 1.71 4 23 1.71 9 22 1.72 9 10 1.75 1 4 1.77 5 6 1.78 6 22 1.79 16 23 1.80 16 22 1.83 3 22 1.85 11 21 1.87 13 14 1.91 5 19 1.91 13 23 1.95 12 19 1.98 15 17 1.98 11 19 2.05 17 20 2.06 2 9 2.07 7 9 2.07 3 7 2.09 5 16 2.10 14 17 2.10 7 22 2.12 20 24 2.14 8 17 2.16 9 11 2.17 6 16 2.18 22 25 2.19 10 19 2.21 11 23 2.22 1 15 2.22 2 7 2.23 2 15 2.24 13 16 2.25 5 25 2.25 2 4 2.26 19 21 2.27 8 22 2.27 15 18 2.29 21 21 2.30 11 22 2.30 9 19 2.30 11 12 2.30 3 9 2.31 3 17 2.32 8 14 2.33 15 22 2.33 10 21 2.34 6 11 2.35 1 9 2.35 20 24 2.35 6 21 2.36 19 23 2.37 9 9 2.37 5 23 2.37 4 21 2.38 1 10 2.39 12 23 2.40 4 21 2.41 5 21 2.42 22 23 2.44 10 23 2.44 6 7 2.46 11 19 2.46 4 12 2.47 18 20 2.48 8 19 2.50 5 14 2.50 8 11 2.51 4 25 2.51 9 10 2.52 1 11 2.52 3 13 2.53 5 7 2.53 19 21 2.54 3 5 2.54 3 8 2.55 2 12 2.55 6 23 2.56 11 13 2.56 7 21 2.56 6 25 2.56 16 24 2.58 4 6 2.58 7 7 2.58 24 25 2.59 19 19 2.60 12 25 2.60 5 21 2.61 18 24 2.61 1 8 2.61 6 21 2.61 2 6 2.61 8 13 2.62 6 7 2.62 14 19 2.63 3 11 2.63 21 25 2.64 7 21 2.64 4 13 2.66 9 11 2.67 13 15 2.68 14 16 2.70 1 22 2.71 8 9 2.73 13 19 2.73 2 5 2.74 8 15 2.76 5 10 2.76 10 22 2.76 5 10 2.77 15 16 2.77 10 19 2.77 5 12 2.78 17 18 2.78 14 20 2.79 4 7 2.79 7 22 2.79 2 22 2.79 4 14 2.79 1 21 2.80 3 6 2.80 6 12 2.80 8 20 2.80 13 24 2.81 10 22 2.81 2 19 2.82 6 8 2.84 17 22 2.85 7 10 2.86 6 14 2.87 1 13 2.90 5 13 2.90 3 16 2.90 4 11 2.91 2 22 2.93 1 19 2.95 15 20 2.95 2 14 2.96 3 12 2.96 3 10 2.96 1 23 2.96 9 22 2.97 16 21 2.97 4 8 2.97 14 15 2.98 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: 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. 0.33: 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 0.16: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.09: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 02src630 finished at 11:21:20 Total CPU time: 1.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++