+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src1290 started at 11:36:25 on 11-Oct-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src1290 in P-1 CELL 0.71073 6.6318 9.4254 12.0872 112.574 90.804 96.144 ZERR 2.00 0.0003 0.0004 0.0004 0.002 0.002 0.002 LATT 1 SFAC C H N O S UNIT 28 28 8 6 2 V = 692.39 F(000) = 332.0 Mu = 0.25 mm-1 Cell Wt = 636.70 Rho = 1.527 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 dfix 0.89 0.01 n3 h3a n3 h3b FMAP 2 PLAN 5 SIZE 0.09 0.08 0.04 EQIV $1 -X+1, -Y+1, -Z+1 htab N3 O1 htab N3 O2 htab N4 O1_$1 SIZE 0.04 0.08 0.09 ACTA BOND $H L.S. 9 TEMP -153.00 WGHT 0.010000 1.412900 FVAR 0.64592 C1 1 0.558767 0.845392 0.321630 11.00000 0.01957 0.01600 = 0.01820 0.00466 -0.00166 0.00135 C2 1 0.448141 0.790697 0.395123 11.00000 0.01845 0.01630 = 0.01946 0.00616 -0.00184 0.00070 C3 1 0.268409 0.864020 0.416129 11.00000 0.02042 0.01543 = 0.01789 0.00461 -0.00316 -0.00013 C4 1 0.125772 0.831454 0.493388 11.00000 0.01875 0.01796 = 0.01980 0.00579 0.00111 0.00274 AFIX 43 H4 2 0.004384 0.879085 0.509881 11.00000 -1.20000 AFIX 0 C5 1 0.170303 0.729930 0.542283 11.00000 0.02291 0.01903 = 0.01805 0.00465 -0.00108 0.00031 C6 1 0.489270 0.677592 0.442489 11.00000 0.02113 0.01734 = 0.02261 0.00735 -0.00195 0.00000 C7 1 0.040817 0.691877 0.629581 11.00000 0.02811 0.02479 = 0.02532 0.01073 0.00422 0.00025 AFIX 137 H7A 2 -0.083317 0.741986 0.637651 11.00000 -1.50000 H7B 2 0.115897 0.729190 0.707846 11.00000 -1.50000 H7C 2 0.004888 0.579481 0.600541 11.00000 -1.50000 AFIX 0 C8 1 0.298583 0.858488 0.075250 11.00000 0.02276 0.01940 = 0.01983 0.00901 0.00007 -0.00078 C9 1 0.374004 0.721114 0.007746 11.00000 0.02670 0.02688 = 0.02906 0.00689 0.00320 0.00417 AFIX 43 H9 2 0.511731 0.708395 0.019689 11.00000 -1.20000 AFIX 0 C10 1 0.245142 0.603102 -0.077190 11.00000 0.03833 0.02724 = 0.02942 0.00236 0.00472 0.00549 AFIX 43 H10 2 0.295440 0.508965 -0.124112 11.00000 -1.20000 AFIX 0 C11 1 0.043443 0.620490 -0.094704 11.00000 0.03552 0.03168 = 0.02006 0.01176 -0.00154 -0.00661 C12 1 -0.027093 0.759541 -0.026602 11.00000 0.02330 0.03601 = 0.03103 0.01749 -0.00065 0.00072 AFIX 43 H12 2 -0.164095 0.773179 -0.039451 11.00000 -1.20000 AFIX 0 C13 1 0.098889 0.879277 0.060071 11.00000 0.02258 0.02581 = 0.02517 0.01203 0.00164 0.00300 AFIX 43 H13 2 0.048582 0.973119 0.107667 11.00000 -1.20000 AFIX 0 C14 1 -0.097732 0.490445 -0.186191 11.00000 0.04866 0.03778 = 0.03228 0.01135 -0.00637 -0.01446 AFIX 137 H14A 2 -0.125750 0.405980 -0.158154 11.00000 -1.50000 H14B 2 -0.033585 0.452313 -0.263035 11.00000 -1.50000 H14C 2 -0.225358 0.528758 -0.196676 11.00000 -1.50000 AFIX 0 N1 3 0.446651 0.951226 0.303699 11.00000 0.01841 0.02124 = 0.01978 0.00970 0.00093 0.00473 N2 3 0.259078 0.959068 0.358792 11.00000 0.01940 0.02106 = 0.02250 0.00944 0.00395 0.00429 N3 3 0.739191 0.808175 0.275219 11.00000 0.02063 0.02516 = 0.02844 0.01342 0.00491 0.00497 AFIX 1 0.8900 H3A 2 0.802465 0.757571 0.310869 11.00000 -1.50000 H3B 2 0.813702 0.871468 0.248521 11.00000 -1.50000 AFIX 0 N4 3 0.343673 0.655085 0.515628 11.00000 0.02562 0.02125 = 0.02580 0.01418 0.00062 0.00409 AFIX 43 H4A 2 0.361430 0.588019 0.548216 11.00000 -1.20000 AFIX 0 O1 4 0.638797 0.603985 0.418837 11.00000 0.02307 0.02615 = 0.03717 0.01832 0.00368 0.00677 O2 4 0.664750 0.997425 0.154078 11.00000 0.02190 0.02762 = 0.02925 0.01488 0.00501 0.00065 O3 4 0.372131 1.147308 0.220959 11.00000 0.03298 0.01910 = 0.02895 0.01104 0.00249 0.00609 S1 5 0.458156 1.006278 0.186497 11.00000 0.02186 0.01936 = 0.02150 0.01020 0.00090 0.00125 HKLF 4 Covalent radii and connectivity table for 2007src1290 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C1 - N3 C2 N1 C2 - C1 C3 C6 C3 - N2 C2 C4 C4 - C5 C3 C5 - C4 N4 C7 C6 - O1 N4 C2 C7 - C5 C8 - C13 C9 S1 C9 - C10 C8 C10 - C9 C11 C11 - C10 C12 C14 C12 - C11 C13 C13 - C8 C12 C14 - C11 N1 - C1 N2 S1 N2 - C3 N1 N3 - C1 N4 - C6 C5 O1 - C6 O2 - S1 O3 - S1 S1 - O3 O2 N1 C8 Operators for generating equivalent atoms: $1 -x+1, -y+1, -z+1 11780 Reflections read, of which 36 rejected -8 =< h =< 8, -12 =< k =< 12, -15 =< l =< 13, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 3162 Unique reflections, of which 0 suppressed R(int) = 0.0494 R(sigma) = 0.0507 Friedel opposites merged Maximum memory for data reduction = 2019 / 31596 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 = 2568 / 250142 wR2 = 0.1204 before cycle 1 for 3162 data and 201 / 201 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.076; Restrained GooF = 1.076 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 1.41 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64546 0.00129 -0.357 OSF Mean shift/esd = 0.015 Maximum = -0.357 for OSF Max. shift = 0.000 A for H14A Max. dU = 0.000 for O1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2568 / 250142 wR2 = 0.1203 before cycle 2 for 3162 data and 201 / 201 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.076; Restrained GooF = 1.075 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 1.41 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64537 0.00129 -0.067 OSF Mean shift/esd = 0.005 Maximum = -0.067 for OSF Max. shift = 0.000 A for H14A Max. dU = 0.000 for O1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2568 / 250142 wR2 = 0.1203 before cycle 3 for 3162 data and 201 / 201 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.076; Restrained GooF = 1.075 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 1.41 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64537 0.00129 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H14B Max. dU = 0.000 for C14 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2568 / 250142 wR2 = 0.1203 before cycle 4 for 3162 data and 201 / 201 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.076; Restrained GooF = 1.075 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 1.41 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64537 0.00129 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H14B Max. dU = 0.000 for C12 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2568 / 250142 wR2 = 0.1203 before cycle 5 for 3162 data and 201 / 201 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.076; Restrained GooF = 1.075 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 1.41 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64537 0.00129 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O3 Max. shift = 0.000 A for H14B Max. dU = 0.000 for N4 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2568 / 250142 wR2 = 0.1203 before cycle 6 for 3162 data and 201 / 201 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.076; Restrained GooF = 1.075 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 1.41 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64537 0.00129 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O3 Max. shift = 0.000 A for C2 Max. dU = 0.000 for O1 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2568 / 250142 wR2 = 0.1203 before cycle 7 for 3162 data and 201 / 201 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.076; Restrained GooF = 1.075 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 1.41 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64537 0.00129 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O3 Max. shift = 0.000 A for H7C Max. dU = 0.000 for N1 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2568 / 250142 wR2 = 0.1203 before cycle 8 for 3162 data and 201 / 201 parameters Summary of restraints applied in cycle 8 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.076; Restrained GooF = 1.075 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 1.41 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64537 0.00129 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O3 Max. shift = 0.000 A for H7C Max. dU = 0.000 for N1 Least-squares cycle 9 Maximum vector length = 511 Memory required = 2568 / 250142 wR2 = 0.1203 before cycle 9 for 3162 data and 201 / 201 parameters Summary of restraints applied in cycle 9 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.076; Restrained GooF = 1.075 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 1.41 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64537 0.00129 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O3 Max. shift = 0.000 A for H7B Max. dU = 0.000 for C3 Largest correlation matrix elements 0.545 U23 O1 / U22 O1 0.528 U23 N4 / U33 N4 0.511 U23 C13 / U22 C13 0.540 U23 N4 / U22 N4 0.521 U23 C12 / U33 C12 0.509 U23 O2 / U33 O2 0.534 U23 O1 / U33 O1 0.519 U23 O2 / U22 O2 0.504 U23 O3 / U22 O3 0.532 U23 S1 / U22 S1 0.515 U23 N3 / U22 N3 0.502 U23 N3 / U33 N3 0.532 U23 C12 / U22 C12 0.514 U23 S1 / U33 S1 Idealized hydrogen atom generation before cycle 10 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H4 0.0044 0.8791 0.5099 43 0.950 0.000 C4 C5 C3 H7A -0.0833 0.7420 0.6376 137 0.980 0.000 C7 C5 H7A H7B 0.1159 0.7292 0.7078 137 0.980 0.000 C7 C5 H7A H7C 0.0049 0.5795 0.6005 137 0.980 0.000 C7 C5 H7A H9 0.5117 0.7084 0.0197 43 0.950 0.000 C9 C10 C8 H10 0.2954 0.5090 -0.1241 43 0.950 0.000 C10 C9 C11 H12 -0.1641 0.7732 -0.0394 43 0.950 0.000 C12 C11 C13 H13 0.0486 0.9731 0.1077 43 0.950 0.000 C13 C8 C12 H14A -0.1258 0.4060 -0.1582 137 0.980 0.000 C14 C11 H14A H14B -0.0336 0.4523 -0.2630 137 0.980 0.000 C14 C11 H14A H14C -0.2254 0.5288 -0.1967 137 0.980 0.000 C14 C11 H14A H4A 0.3614 0.5880 0.5482 43 0.880 0.000 N4 C6 C5 2007src1290 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.55877 0.84539 0.32163 1.00000 0.01953 0.01597 0.01816 0.00466 -0.00166 0.00135 0.01857 0.00519 0.00038 0.00028 0.00022 0.00000 0.00125 0.00115 0.00120 0.00097 0.00097 0.00095 0.00051 C2 0.44815 0.79069 0.39512 1.00000 0.01840 0.01627 0.01942 0.00615 -0.00184 0.00070 0.01841 0.00519 0.00038 0.00028 0.00022 0.00000 0.00124 0.00117 0.00122 0.00099 0.00097 0.00095 0.00051 C3 0.26841 0.86402 0.41613 1.00000 0.02038 0.01539 0.01785 0.00460 -0.00315 -0.00012 0.01865 0.00513 0.00038 0.00028 0.00022 0.00000 0.00128 0.00115 0.00120 0.00097 0.00098 0.00097 0.00051 C4 0.12577 0.83146 0.49339 1.00000 0.01871 0.01792 0.01976 0.00578 0.00111 0.00274 0.01922 0.00526 0.00039 0.00028 0.00022 0.00000 0.00125 0.00120 0.00124 0.00101 0.00097 0.00097 0.00052 H4 0.00438 0.87909 0.50988 1.00000 0.02306 0.00000 0.00000 C5 0.17030 0.72993 0.54228 1.00000 0.02287 0.01899 0.01801 0.00464 -0.00107 0.00031 0.02092 0.00533 0.00040 0.00029 0.00022 0.00000 0.00134 0.00123 0.00123 0.00101 0.00101 0.00101 0.00054 C6 0.48927 0.67759 0.44249 1.00000 0.02109 0.01730 0.02257 0.00735 -0.00195 0.00000 0.02065 0.00540 0.00039 0.00029 0.00023 0.00000 0.00132 0.00119 0.00129 0.00103 0.00102 0.00100 0.00053 C7 0.04081 0.69188 0.62958 1.00000 0.02807 0.02475 0.02527 0.01072 0.00423 0.00025 0.02593 0.00601 0.00043 0.00032 0.00025 0.00000 0.00149 0.00137 0.00138 0.00114 0.00113 0.00112 0.00059 H7A -0.08333 0.74199 0.63765 1.00000 0.03889 0.00000 0.00000 H7B 0.11589 0.72920 0.70785 1.00000 0.03889 0.00000 0.00000 H7C 0.00488 0.57948 0.60055 1.00000 0.03889 0.00000 0.00000 C8 0.29858 0.85849 0.07525 1.00000 0.02272 0.01936 0.01979 0.00899 0.00007 -0.00079 0.02048 0.00548 0.00040 0.00029 0.00023 0.00000 0.00134 0.00122 0.00125 0.00103 0.00101 0.00101 0.00053 C9 0.37401 0.72111 0.00775 1.00000 0.02665 0.02684 0.02903 0.00686 0.00319 0.00416 0.02862 0.00615 0.00045 0.00032 0.00025 0.00000 0.00150 0.00144 0.00148 0.00120 0.00117 0.00116 0.00062 H9 0.51174 0.70839 0.01969 1.00000 0.03434 0.00000 0.00000 C10 0.24515 0.60310 -0.07719 1.00000 0.03828 0.02720 0.02937 0.00233 0.00471 0.00548 0.03409 0.00653 0.00049 0.00035 0.00027 0.00000 0.00178 0.00151 0.00155 0.00125 0.00131 0.00130 0.00070 H10 0.29544 0.50896 -0.12411 1.00000 0.04090 0.00000 0.00000 C11 0.04344 0.62049 -0.09470 1.00000 0.03547 0.03164 0.02003 0.01174 -0.00155 -0.00662 0.02939 0.00599 0.00046 0.00034 0.00024 0.00000 0.00166 0.00153 0.00134 0.00119 0.00118 0.00126 0.00064 C12 -0.02710 0.75955 -0.02660 1.00000 0.02325 0.03596 0.03099 0.01746 -0.00065 0.00071 0.02895 0.00626 0.00044 0.00034 0.00026 0.00000 0.00144 0.00160 0.00152 0.00131 0.00117 0.00120 0.00063 H12 -0.16410 0.77319 -0.03944 1.00000 0.03475 0.00000 0.00000 C13 0.09888 0.87928 0.06007 1.00000 0.02253 0.02577 0.02513 0.01200 0.00163 0.00300 0.02382 0.00584 0.00041 0.00032 0.00024 0.00000 0.00137 0.00137 0.00136 0.00114 0.00108 0.00108 0.00056 H13 0.04857 0.97312 0.10767 1.00000 0.02859 0.00000 0.00000 C14 -0.09774 0.49044 -0.18619 1.00000 0.04861 0.03774 0.03223 0.01132 -0.00638 -0.01448 0.04184 0.00647 0.00054 0.00038 0.00029 0.00000 0.00206 0.00178 0.00170 0.00143 0.00147 0.00152 0.00082 H14A -0.12577 0.40598 -0.15815 1.00000 0.06276 0.00000 0.00000 H14B -0.03358 0.45230 -0.26304 1.00000 0.06276 0.00000 0.00000 H14C -0.22536 0.52876 -0.19669 1.00000 0.06276 0.00000 0.00000 N1 0.44665 0.95123 0.30370 1.00000 0.01837 0.02120 0.01974 0.00970 0.00093 0.00473 0.01906 0.00456 0.00032 0.00024 0.00019 0.00000 0.00109 0.00107 0.00107 0.00088 0.00085 0.00085 0.00045 N2 0.25907 0.95907 0.35879 1.00000 0.01936 0.02101 0.02246 0.00943 0.00395 0.00428 0.02047 0.00468 0.00032 0.00025 0.00019 0.00000 0.00111 0.00108 0.00110 0.00091 0.00086 0.00086 0.00046 N3 0.73919 0.80817 0.27522 1.00000 0.02058 0.02512 0.02840 0.01340 0.00491 0.00497 0.02357 0.00494 0.00033 0.00026 0.00020 0.00000 0.00115 0.00116 0.00121 0.00099 0.00093 0.00091 0.00049 H3A 0.80247 0.75757 0.31087 1.00000 0.03536 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 H3B 0.81370 0.87147 0.24852 1.00000 0.03536 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 N4 0.34368 0.65508 0.51563 1.00000 0.02556 0.02122 0.02576 0.01417 0.00063 0.00409 0.02255 0.00475 0.00034 0.00025 0.00020 0.00000 0.00121 0.00111 0.00117 0.00096 0.00093 0.00091 0.00048 H4A 0.36143 0.58802 0.54822 1.00000 0.02707 0.00000 0.00000 O1 0.63880 0.60399 0.41884 1.00000 0.02302 0.02610 0.03712 0.01829 0.00368 0.00676 0.02660 0.00424 0.00028 0.00022 0.00018 0.00000 0.00101 0.00101 0.00113 0.00089 0.00084 0.00080 0.00044 O2 0.66476 0.99742 0.15408 1.00000 0.02185 0.02758 0.02921 0.01486 0.00501 0.00065 0.02519 0.00409 0.00028 0.00022 0.00017 0.00000 0.00098 0.00101 0.00102 0.00084 0.00078 0.00077 0.00042 O3 0.37213 1.14731 0.22096 1.00000 0.03293 0.01905 0.02891 0.01102 0.00249 0.00609 0.02620 0.00411 0.00030 0.00021 0.00017 0.00000 0.00112 0.00092 0.00102 0.00081 0.00084 0.00080 0.00044 S1 0.45816 1.00628 0.18650 1.00000 0.02181 0.01932 0.02146 0.01019 0.00090 0.00125 0.02028 0.00139 0.00010 0.00007 0.00006 0.00000 0.00033 0.00031 0.00033 0.00026 0.00025 0.00024 0.00017 Final Structure Factor Calculation for 2007src1290 in P-1 Total number of l.s. parameters = 201 Maximum vector length = 511 Memory required = 2367 / 24017 wR2 = 0.1203 before cycle 10 for 3162 data and 0 / 201 parameters Summary of restraints applied in cycle 10 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.076; Restrained GooF = 1.075 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 1.41 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0572 for 2534 Fo > 4sig(Fo) and 0.0785 for all 3162 data wR2 = 0.1203, GooF = S = 1.076, Restrained GooF = 1.075 for all data Occupancy sum of asymmetric unit = 22.00 for non-hydrogen and 14.00 for hydrogen atoms Principal mean square atomic displacements U 0.0224 0.0184 0.0149 C1 0.0222 0.0177 0.0154 C2 0.0239 0.0185 0.0135 C3 0.0216 0.0188 0.0173 C4 0.0242 0.0226 0.0159 C5 0.0254 0.0201 0.0164 C6 0.0316 0.0258 0.0204 C7 0.0254 0.0195 0.0166 C8 0.0347 0.0273 0.0238 C9 0.0431 0.0380 0.0212 C10 0.0459 0.0238 0.0184 C11 0.0385 0.0256 0.0228 C12 0.0270 0.0225 0.0219 C13 0.0664 0.0354 0.0238 C14 0.0224 0.0194 0.0153 N1 0.0241 0.0199 0.0175 N2 0.0303 0.0214 0.0190 N3 0.0278 0.0258 0.0141 N4 0.0383 0.0240 0.0175 O1 0.0313 0.0272 0.0171 O2 0.0332 0.0288 0.0166 O3 0.0232 0.0213 0.0163 S1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.017 0.027 0.036 0.047 0.059 0.074 0.094 0.130 1.000 Number in group 334. 304. 330. 301. 341. 291. 325. 310. 312. 314. GooF 1.155 1.160 1.088 1.163 1.089 1.113 1.036 0.993 0.933 1.005 K 4.601 1.315 1.019 1.014 1.002 0.987 1.011 1.000 1.006 1.011 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.65 inf Number in group 322. 317. 317. 308. 322. 316. 310. 319. 313. 318. GooF 1.111 1.248 1.153 1.059 1.091 1.065 0.966 0.870 0.908 1.217 K 1.059 1.047 1.043 1.038 1.011 1.005 0.989 0.994 1.006 1.011 R1 0.189 0.164 0.127 0.116 0.105 0.084 0.052 0.040 0.038 0.034 Recommended weighting scheme: WGHT 0.0000 1.4097 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) -1 3 1 613.60 495.97 3.73 0.148 2.49 -6 0 10 30.01 72.97 3.64 0.057 0.81 8 -2 2 82.87 39.47 3.58 0.042 0.82 6 7 0 65.86 12.30 3.43 0.023 0.77 8 -3 2 121.94 64.24 3.24 0.053 0.82 1 -6 10 30.45 9.34 3.24 0.020 1.11 -7 5 5 66.87 23.41 3.23 0.032 0.78 -3 3 0 324.37 253.75 3.19 0.106 1.86 -6 -1 10 -1.32 13.24 3.11 0.024 0.82 -6 3 7 11.73 0.19 3.03 0.003 0.85 2 0 0 274.52 345.45 3.03 0.123 3.29 -2 3 3 589.34 492.83 3.02 0.147 1.76 -3 2 1 271.47 210.96 3.02 0.096 1.98 -4 -1 9 -0.02 18.12 2.98 0.028 1.04 1 -4 5 39.95 19.99 2.97 0.030 1.93 -4 0 2 168.79 224.99 2.93 0.099 1.60 4 2 7 23.80 3.64 2.86 0.013 0.99 0 -8 14 -3.24 14.15 2.85 0.025 0.81 -7 1 6 95.65 53.03 2.82 0.048 0.85 2 8 4 39.55 71.61 2.80 0.056 0.84 -3 -10 8 -14.00 19.66 2.80 0.029 0.81 6 5 0 21.30 1.09 2.79 0.007 0.88 1 -9 2 13.51 1.29 2.73 0.008 1.02 -5 -8 1 22.74 5.18 2.72 0.015 0.81 -7 2 6 71.67 36.18 2.70 0.040 0.83 -2 -2 12 12.63 0.10 2.67 0.002 0.96 6 4 2 57.65 95.99 2.67 0.065 0.89 4 -1 1 210.17 163.20 2.67 0.085 1.64 -4 0 12 93.47 45.88 2.66 0.045 0.83 3 -8 2 0.26 14.34 2.66 0.025 1.07 1 -11 4 -2.42 8.21 2.64 0.019 0.85 -8 -3 4 44.27 1.22 2.62 0.007 0.77 -3 -7 10 16.84 3.75 2.62 0.013 0.93 -7 4 2 20.44 4.18 2.57 0.014 0.88 3 4 6 18.39 40.00 2.55 0.042 1.01 3 1 10 13.64 33.38 2.55 0.038 0.92 -4 7 0 23.80 45.28 2.54 0.045 1.05 0 -2 14 18.04 1.00 2.54 0.007 0.84 -2 -3 3 236.97 188.86 2.54 0.091 2.09 1 -6 13 30.64 3.17 2.54 0.012 0.90 0 -9 8 3.96 19.51 2.53 0.029 0.99 5 -8 3 16.52 2.36 2.53 0.010 0.93 6 -1 9 43.33 74.52 2.53 0.057 0.82 -6 1 5 16.25 35.09 2.51 0.039 0.99 2 -7 11 162.73 115.39 2.50 0.071 0.96 1 0 14 -4.75 25.92 2.49 0.034 0.78 -3 -3 6 11.23 1.98 2.49 0.009 1.44 4 -8 7 40.11 17.54 2.46 0.028 0.96 -1 -2 5 58.84 86.11 2.42 0.061 2.25 0 -5 15 36.46 14.89 2.42 0.026 0.80 Bond lengths and angles C1 - Distance Angles N3 1.3517 (0.0033) C2 1.3719 (0.0035) 129.08 (0.24) N1 1.3839 (0.0032) 125.65 (0.23) 105.27 (0.22) C1 - N3 C2 C2 - Distance Angles C1 1.3719 (0.0035) C3 1.4188 (0.0035) 106.85 (0.22) C6 1.4370 (0.0035) 130.06 (0.24) 123.05 (0.23) C2 - C1 C3 C3 - Distance Angles N2 1.3320 (0.0032) C2 1.4188 (0.0035) 112.43 (0.23) C4 1.4296 (0.0035) 128.53 (0.24) 119.04 (0.23) C3 - N2 C2 C4 - Distance Angles C5 1.3572 (0.0036) C3 1.4296 (0.0035) 117.49 (0.24) H4 0.9500 121.25 121.25 C4 - C5 C3 C5 - Distance Angles C4 1.3572 (0.0036) N4 1.3904 (0.0033) 121.92 (0.24) C7 1.4932 (0.0036) 123.15 (0.25) 114.92 (0.23) C5 - C4 N4 C6 - Distance Angles O1 1.2447 (0.0031) N4 1.3722 (0.0034) 122.44 (0.23) C2 1.4370 (0.0035) 124.32 (0.24) 113.23 (0.23) C6 - O1 N4 C7 - Distance Angles C5 1.4932 (0.0036) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - C5 H7A H7B C8 - Distance Angles C13 1.3792 (0.0037) C9 1.3898 (0.0037) 121.59 (0.25) S1 1.7535 (0.0026) 119.08 (0.20) 119.28 (0.21) C8 - C13 C9 C9 - Distance Angles C10 1.3845 (0.0040) C8 1.3898 (0.0037) 118.91 (0.28) H9 0.9500 120.54 120.54 C9 - C10 C8 C10 - Distance Angles C9 1.3845 (0.0040) C11 1.3881 (0.0044) 120.88 (0.28) H10 0.9500 119.56 119.56 C10 - C9 C11 C11 - Distance Angles C10 1.3881 (0.0044) C12 1.3885 (0.0042) 118.88 (0.26) C14 1.5122 (0.0039) 120.74 (0.29) 120.37 (0.29) C11 - C10 C12 C12 - Distance Angles C11 1.3885 (0.0042) C13 1.3910 (0.0038) 121.30 (0.27) H12 0.9500 119.35 119.35 C12 - C11 C13 C13 - Distance Angles C8 1.3792 (0.0037) C12 1.3910 (0.0038) 118.41 (0.26) H13 0.9500 120.80 120.80 C13 - C8 C12 C14 - Distance Angles C11 1.5122 (0.0039) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - C11 H14A H14B N1 - Distance Angles C1 1.3839 (0.0032) N2 1.4148 (0.0029) 112.44 (0.20) S1 1.6855 (0.0021) 126.03 (0.18) 116.11 (0.16) N1 - C1 N2 N2 - Distance Angles C3 1.3320 (0.0032) N1 1.4148 (0.0029) 102.86 (0.20) N2 - C3 N3 - Distance Angles C1 1.3517 (0.0033) H3A 0.8859 112.38 H3B 0.8907 119.86 118.51 N3 - C1 H3A N4 - Distance Angles C6 1.3722 (0.0034) C5 1.3904 (0.0033) 125.12 (0.22) H4A 0.8800 117.44 117.44 N4 - C6 C5 O1 - Distance Angles C6 1.2447 (0.0031) O1 - O2 - Distance Angles S1 1.4326 (0.0019) O2 - O3 - Distance Angles S1 1.4177 (0.0019) O3 - S1 - Distance Angles O3 1.4177 (0.0019) O2 1.4326 (0.0019) 121.25 (0.12) N1 1.6855 (0.0021) 107.16 (0.11) 104.42 (0.11) C8 1.7535 (0.0026) 109.70 (0.12) 109.65 (0.12) 102.95 (0.11) S1 - O3 O2 N1 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.89 2.48 3.080(3) 125.8 N3-H3A...O1 0.89 2.22 2.783(3) 120.3 N3-H3B...O2 0.88 2.00 2.854(3) 164.5 N4-H4A...O1_$1 FMAP and GRID set by program FMAP 2 1 20 GRID -2.941 -2 -2 2.941 2 2 R1 = 0.0780 for 3162 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.34 at 0.2041 0.8691 0.4624 [ 0.70 A from C3 ] Deepest hole -0.42 at 0.4693 0.9351 0.1775 [ 0.65 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2441 / 19655 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2041 0.8691 0.4624 1.00000 0.05 0.34 0.70 C3 0.78 C4 1.45 H4 1.78 N2 Q2 1 0.2954 0.6511 0.0040 1.00000 0.05 0.32 0.78 C9 0.95 C10 1.46 H9 1.61 H10 Q3 1 0.4823 0.9769 0.2598 1.00000 0.05 0.31 0.70 N1 1.04 S1 1.79 C1 1.82 O2 Q4 1 0.5254 0.8017 0.3594 1.00000 0.05 0.30 0.70 C2 0.74 C1 1.77 N3 1.81 C6 Q5 1 0.5777 0.5309 0.3373 1.00000 0.05 0.30 1.01 O1 1.65 C6 2.15 H4A 2.53 C2 Shortest distances between peaks (including symmetry equivalents) 3 4 2.42 1 4 2.50 4 5 2.52 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.00: 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. 1.16: 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 1.16: Structure factors and derivatives 2.13: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.37: Solve l.s. equations 0.00: Generate HTAB table 0.04: Other dependent quantities, CIF, tables 0.07: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src1290 finished at 11:36:39 Total CPU time: 5.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++