+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0461p-1 started at 12:19:52 on 12-May-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0461p-1 in P-1 CELL 0.71073 6.1693 7.0845 10.3537 87.871 74.394 69.471 ZERR 2.00 0.0005 0.0006 0.0008 0.005 0.005 0.005 LATT 1 SFAC C N O S H UNIT 16 6 2 2 10 V = 407.34 F(000) = 196.0 Mu = 0.35 mm-1 Cell Wt = 382.42 Rho = 1.559 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 EADP C2b C3b C4b EADP C1 C2 C3 C4 EQIV_$1 x-1, y, z HTAB N12 N6_$1 EQIV_$2 -x+1, -y+1, -z+1 HTAB N12 N11_$2 FMAP 2 PLAN 10 SIZE 0.01 0.06 0.11 ACTA BOND $H WGHT 0.00000 0.73890 L.S. 25 TEMP -153.00 FVAR 0.89435 0.61732 PART 1 C1 1 1.152565 0.205007 -0.100200 21.00000 0.03086 0.02562 = 0.01773 -0.00235 -0.00697 -0.00907 C2 1 1.064861 0.196139 -0.212976 21.00000 0.03086 0.02562 = 0.01773 -0.00235 -0.00697 -0.00907 AFIX 43 H2 5 0.902457 0.217276 -0.209323 21.00000 -1.20000 AFIX 0 C3 1 1.475928 0.125251 -0.307019 21.00000 0.03086 0.02562 = 0.01773 -0.00235 -0.00697 -0.00907 AFIX 43 H3 5 1.626223 0.091602 -0.373324 21.00000 -1.20000 AFIX 0 C4 1 1.264151 0.149447 -0.334881 21.00000 0.03086 0.02562 = 0.01773 -0.00235 -0.00697 -0.00907 AFIX 43 H4 5 1.248531 0.137377 -0.422724 21.00000 -1.20000 AFIX 0 S1 4 1.439988 0.162454 -0.138847 21.00000 0.01717 0.03282 = 0.02181 -0.00131 -0.00164 -0.00854 PART 2 SAME C1 > S1 C1B 1 1.130696 0.208403 -0.106378 -21.00000 0.00562 0.00997 = 0.02234 0.00362 -0.00744 -0.00149 C2B 1 1.387263 0.165440 -0.139017 -21.00000 0.02116 0.03352 = 0.02285 0.00095 0.00384 -0.01318 AFIX 43 H2B 5 1.476727 0.158361 -0.076137 -21.00000 -1.20000 AFIX 0 C3B 1 1.309625 0.149626 -0.347459 -21.00000 0.02116 0.03352 = 0.02285 0.00095 0.00384 -0.01318 AFIX 43 H3B 5 1.338665 0.130708 -0.441780 -21.00000 -1.20000 AFIX 0 C4B 1 1.485895 0.134705 -0.285184 -21.00000 0.02116 0.03352 = 0.02285 0.00095 0.00384 -0.01318 AFIX 43 H4B 5 1.650207 0.107927 -0.331192 -21.00000 -1.20000 AFIX 0 S1B 4 1.035164 0.205681 -0.235886 -21.00000 0.02672 0.03004 = 0.01753 -0.00128 -0.00672 -0.01058 PART 0 C8 1 0.655971 0.331595 0.191811 11.00000 0.02236 0.02161 = 0.01930 -0.00046 -0.00262 -0.00845 C5 1 0.995525 0.255841 0.033699 11.00000 0.02112 0.01870 = 0.02336 0.00039 -0.00748 -0.00632 C10 1 0.827468 0.352690 0.381005 11.00000 0.01914 0.02782 = 0.02384 0.00181 -0.00582 -0.00847 C7 1 0.839723 0.327082 0.244562 11.00000 0.01889 0.02423 = 0.02082 0.00025 -0.00386 -0.00832 N11 2 0.817083 0.371509 0.493200 11.00000 0.02622 0.04649 = 0.02226 0.00085 -0.00436 -0.01475 N12 2 0.422002 0.373388 0.242269 11.00000 0.01975 0.03901 = 0.02529 -0.00782 -0.00390 -0.01128 N6 2 1.054065 0.279682 0.140622 11.00000 0.02242 0.02253 = 0.01805 -0.00075 -0.00442 -0.00784 O9 3 0.752514 0.286107 0.056858 11.00000 0.02165 0.02781 = 0.01913 -0.00172 -0.00684 -0.00849 H12B 5 0.336386 0.348459 0.195265 11.00000 0.03074 H12A 5 0.348342 0.432283 0.325744 11.00000 0.06178 HKLF 4 Covalent radii and connectivity table for 2009src0461p-1 in P-1 C 0.770 N 0.700 O 0.660 S 1.030 H 0.320 C1_a - C2_a C5 S1_a C2_a - C1_a C4_a C3_a - C4_a S1_a C4_a - C3_a C2_a S1_a - C1_a C3_a C1B_b - C2B_b C5 S1B_b C2B_b - C1B_b C4B_b C3B_b - C4B_b S1B_b C4B_b - C3B_b C2B_b S1B_b - C1B_b C3B_b C8 - N12 O9 C7 C5 - N6 O9 C1_a C1B_b C10 - N11 C7 C7 - C8 N6 C10 N11 - C10 N12 - C8 N6 - C5 C7 O9 - C8 C5 Operators for generating equivalent atoms: $1 x-1, y, z $2 -x+1, -y+1, -z+1 6884 Reflections read, of which 17 rejected -7 =< h =< 7, -9 =< k =< 9, -13 =< l =< 13, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) -4 -1 4 7.86 0.75 3 4.64 1 Inconsistent equivalents 1849 Unique reflections, of which 0 suppressed R(int) = 0.0607 R(sigma) = 0.0594 Friedel opposites merged Maximum memory for data reduction = 1649 / 18673 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 = 2055 / 179578 wR2 = 0.1271 before cycle 1 for 1849 data and 142 / 142 parameters 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. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 -0.001 OSF 2 0.61732 0.00367 -0.001 FVAR 2 Mean shift/su = 0.001 Maximum = 0.005 for U13 O9 Max. shift = 0.000 A for H12B Max. dU = 0.000 for H12A Least-squares cycle 2 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 2 for 1849 data and 142 / 142 parameters 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. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.002 for U13 O9 Max. shift = 0.000 A for H12B Max. dU = 0.000 for N6 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 3 for 1849 data and 142 / 142 parameters 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. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for y C4B_b Max. shift = 0.000 A for C4B_b Max. dU = 0.000 for H12B Least-squares cycle 4 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 4 for 1849 data and 142 / 142 parameters 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. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C2B_b Max. dU = 0.000 for H12B Least-squares cycle 5 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 5 for 1849 data and 142 / 142 parameters 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. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for U22 C1_a Max. shift = 0.000 A for C1B_b Max. dU = 0.000 for H12A Least-squares cycle 6 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 6 for 1849 data and 142 / 142 parameters 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. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for U22 C1_a Max. shift = 0.000 A for C3B_b Max. dU = 0.000 for C1B_b Least-squares cycle 7 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 7 for 1849 data and 142 / 142 parameters 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. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for U22 S1_a Max. shift = 0.000 A for C1_a Max. dU = 0.000 for C1B_b Least-squares cycle 8 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 8 for 1849 data and 142 / 142 parameters 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. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for U12 C1_a Max. shift = 0.000 A for C3B_b Max. dU = 0.000 for C2B_b Least-squares cycle 9 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 9 for 1849 data and 142 / 142 parameters 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. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for U11 S1B_b Max. shift = 0.000 A for C3B_b Max. dU = 0.000 for S1B_b Least-squares cycle 10 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 10 for 1849 data and 142 / 142 parameters 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. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for U11 C1_a Max. shift = 0.000 A for C1B_b Max. dU = 0.000 for C2B_b Least-squares cycle 11 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 11 for 1849 data and 142 / 142 parameters 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. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C2_a Max. dU = 0.000 for C1_a Least-squares cycle 12 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 12 for 1849 data and 142 / 142 parameters Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H12B Max. dU = 0.000 for H12B Least-squares cycle 13 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 13 for 1849 data and 142 / 142 parameters Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C2B_b Max. dU = 0.000 for C2B_b Least-squares cycle 14 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 14 for 1849 data and 142 / 142 parameters Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for x S1B_b Max. shift = 0.000 A for C3B_b Max. dU = 0.000 for C1_a Least-squares cycle 15 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 15 for 1849 data and 142 / 142 parameters Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for U22 C1_a Max. shift = 0.000 A for C4B_b Max. dU = 0.000 for C2B_b Least-squares cycle 16 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 16 for 1849 data and 142 / 142 parameters Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for x S1B_b Max. shift = 0.000 A for C1B_b Max. dU = 0.000 for C2B_b Least-squares cycle 17 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 17 for 1849 data and 142 / 142 parameters Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for U33 C1_a Max. shift = 0.000 A for C4B_b Max. dU = 0.000 for C1B_b Least-squares cycle 18 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 18 for 1849 data and 142 / 142 parameters Summary of restraints applied in cycle 18 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for U11 C1_a Max. shift = 0.000 A for C4B_b Max. dU = 0.000 for C1_a Least-squares cycle 19 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 19 for 1849 data and 142 / 142 parameters Summary of restraints applied in cycle 19 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for U22 C1_a Max. shift = 0.000 A for H12A Max. dU = 0.000 for C2B_b Least-squares cycle 20 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 20 for 1849 data and 142 / 142 parameters Summary of restraints applied in cycle 20 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for U33 C1_a Max. shift = 0.000 A for C2B_b Max. dU = 0.000 for H12A Least-squares cycle 21 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 21 for 1849 data and 142 / 142 parameters Summary of restraints applied in cycle 21 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for U12 C1_a Max. shift = 0.000 A for C2_a Max. dU = 0.000 for C2B_b Least-squares cycle 22 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 22 for 1849 data and 142 / 142 parameters Summary of restraints applied in cycle 22 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for x C8 Max. shift = 0.000 A for C2B_b Max. dU = 0.000 for C1B_b Least-squares cycle 23 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 23 for 1849 data and 142 / 142 parameters Summary of restraints applied in cycle 23 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for x S1B_b Max. shift = 0.000 A for C2B_b Max. dU = 0.000 for H12B Least-squares cycle 24 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 24 for 1849 data and 142 / 142 parameters Summary of restraints applied in cycle 24 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C2B_b Max. dU = 0.000 for H12B Least-squares cycle 25 Maximum vector length = 511 Memory required = 2055 / 179578 wR2 = 0.1271 before cycle 25 for 1849 data and 142 / 142 parameters Summary of restraints applied in cycle 25 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.89435 0.00260 0.000 OSF 2 0.61732 0.00367 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for U33 C1_a Max. shift = 0.000 A for C3B_b Max. dU = 0.000 for C1B_b Largest correlation matrix elements -0.971 y C1B_b / y C1_a -0.840 y C4B_b / y C3_a -0.703 z S1B_b / z C2_a -0.902 x C1B_b / x C1_a -0.830 y C3B_b / y C4_a -0.697 z C3B_b / x C3_a -0.899 y C2B_b / y S1_a -0.825 x S1B_b / x C2_a -0.690 U23 S1B_b / y C2_a -0.894 x C4B_b / x C3_a 0.781 y C2B_b / U12 S1_a 0.689 U13 C2B_b / x C3_a -0.886 y S1B_b / y C2_a 0.738 x C4B_b / z C3B_b -0.683 U12 S1_a / y S1_a -0.875 z C3B_b / z C4_a -0.726 U33 S1B_b / z C2_a 0.683 z C4_a / x C3_a -0.875 z C1B_b / z C1_a -0.720 x C4B_b / z C4_a 0.677 x C2B_b / U11 S1_a -0.870 z C2B_b / z S1_a 0.719 z C2B_b / U13 S1_a -0.666 U11 C2B_b / x S1_a Idealized hydrogen atom generation before cycle 26 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.9025 0.2173 -0.2093 43 0.950 0.000 C2_a C1_a C4_a H3 1.6262 0.0916 -0.3733 43 0.950 0.000 C3_a C4_a S1_a H4 1.2485 0.1374 -0.4227 43 0.950 0.000 C4_a C3_a C2_a H2B 1.4767 0.1584 -0.0761 43 0.950 0.000 C2B_b C1B_b C4B_b H3B 1.3387 0.1307 -0.4418 43 0.950 0.000 C3B_b C4B_b S1B_b H4B 1.6502 0.1079 -0.3312 43 0.950 0.000 C4B_b C3B_b C2B_b 2009src0461p-1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1_a 1.15256 0.20501 -0.10020 0.61732 0.03086 0.02562 0.01773 -0.00235 -0.00697 -0.00907 0.02482 0.02918 0.00271 0.00338 0.00110 0.00367 0.00267 0.00228 0.00229 0.00156 0.00175 0.00179 0.00132 C2_a 1.06486 0.19614 -0.21297 0.61732 0.03086 0.02562 0.01773 -0.00235 -0.00697 -0.00907 0.02482 0.01609 0.00231 0.00198 0.00107 0.00367 0.00267 0.00228 0.00229 0.00156 0.00175 0.00179 0.00132 H2_a 0.90246 0.21728 -0.20932 0.61732 0.02979 0.00367 0.00000 C3_a 1.47593 0.12525 -0.30702 0.61732 0.03086 0.02562 0.01773 -0.00235 -0.00697 -0.00907 0.02482 0.01280 0.00251 0.00147 0.00086 0.00367 0.00267 0.00228 0.00229 0.00156 0.00175 0.00179 0.00132 H3_a 1.62622 0.09161 -0.37333 0.61732 0.02979 0.00367 0.00000 C4_a 1.26415 0.14945 -0.33488 0.61732 0.03086 0.02562 0.01773 -0.00235 -0.00697 -0.00907 0.02482 0.01740 0.00133 0.00143 0.00112 0.00367 0.00267 0.00228 0.00229 0.00156 0.00175 0.00179 0.00132 H4_a 1.24853 0.13738 -0.42272 0.61732 0.02979 0.00367 0.00000 S1_a 1.43999 0.16245 -0.13885 0.61732 0.01717 0.03282 0.02181 -0.00131 -0.00164 -0.00854 0.02470 0.00410 0.00035 0.00050 0.00027 0.00367 0.00093 0.00086 0.00077 0.00059 0.00072 0.00083 0.00052 C1B_b 1.13070 0.20840 -0.10638 0.38268 0.00563 0.00996 0.02235 0.00362 -0.00744 -0.00149 0.01232 0.03567 0.00295 0.00421 0.00143 0.00367 0.00438 0.00409 0.00532 0.00365 0.00348 0.00368 0.00274 C2B_b 1.38726 0.16544 -0.13902 0.38268 0.02116 0.03352 0.02285 0.00095 0.00384 -0.01317 0.02689 0.02865 0.00252 0.00344 0.00187 0.00367 0.00399 0.00424 0.00387 0.00286 0.00339 0.00335 0.00239 H2B_b 1.47672 0.15837 -0.07614 0.38268 0.03227 0.00367 0.00000 C3B_b 1.30962 0.14963 -0.34746 0.38268 0.02116 0.03352 0.02285 0.00095 0.00384 -0.01317 0.02689 0.03009 0.00201 0.00240 0.00185 0.00367 0.00399 0.00424 0.00387 0.00286 0.00339 0.00335 0.00239 H3B_b 1.33866 0.13071 -0.44178 0.38268 0.03227 0.00367 0.00000 C4B_b 1.48589 0.13470 -0.28518 0.38268 0.02116 0.03352 0.02285 0.00095 0.00384 -0.01317 0.02689 0.02025 0.00359 0.00250 0.00137 0.00367 0.00399 0.00424 0.00387 0.00286 0.00339 0.00335 0.00239 H4B_b 1.65021 0.10792 -0.33119 0.38268 0.03227 0.00367 0.00000 S1B_b 1.03516 0.20568 -0.23589 0.38268 0.02672 0.03004 0.01753 -0.00128 -0.00673 -0.01059 0.02440 0.00566 0.00082 0.00075 0.00037 0.00367 0.00165 0.00140 0.00157 0.00119 0.00101 0.00112 0.00082 C8 0.65597 0.33159 0.19181 1.00000 0.02235 0.02162 0.01930 -0.00046 -0.00262 -0.00845 0.02149 0.00416 0.00051 0.00043 0.00028 0.00000 0.00143 0.00149 0.00135 0.00112 0.00113 0.00116 0.00060 C5 0.99553 0.25584 0.03370 1.00000 0.02112 0.01870 0.02336 0.00039 -0.00747 -0.00632 0.02095 0.00402 0.00049 0.00042 0.00028 0.00000 0.00144 0.00142 0.00142 0.00112 0.00119 0.00116 0.00060 C10 0.82747 0.35269 0.38101 1.00000 0.01914 0.02782 0.02384 0.00181 -0.00582 -0.00847 0.02357 0.00426 0.00050 0.00045 0.00029 0.00000 0.00145 0.00165 0.00152 0.00120 0.00119 0.00121 0.00064 C7 0.83972 0.32708 0.24456 1.00000 0.01889 0.02423 0.02082 0.00025 -0.00386 -0.00832 0.02141 0.00415 0.00050 0.00043 0.00028 0.00000 0.00138 0.00152 0.00137 0.00114 0.00111 0.00116 0.00060 N11 0.81708 0.37151 0.49320 1.00000 0.02622 0.04649 0.02226 0.00085 -0.00436 -0.01476 0.03157 0.00392 0.00046 0.00044 0.00026 0.00000 0.00142 0.00175 0.00135 0.00118 0.00111 0.00125 0.00065 N12 0.42200 0.37339 0.24227 1.00000 0.01975 0.03901 0.02529 -0.00783 -0.00390 -0.01128 0.02797 0.00415 0.00046 0.00043 0.00028 0.00000 0.00133 0.00163 0.00143 0.00120 0.00115 0.00116 0.00061 N6 1.05407 0.27968 0.14062 1.00000 0.02242 0.02253 0.01805 -0.00075 -0.00442 -0.00785 0.02120 0.00336 0.00042 0.00035 0.00023 0.00000 0.00123 0.00130 0.00117 0.00096 0.00098 0.00100 0.00053 O9 0.75251 0.28611 0.05686 1.00000 0.02165 0.02781 0.01913 -0.00172 -0.00683 -0.00849 0.02258 0.00274 0.00034 0.00030 0.00019 0.00000 0.00105 0.00112 0.00100 0.00082 0.00082 0.00085 0.00046 H12B 0.33639 0.34845 0.19526 1.00000 0.03074 0.05329 0.00606 0.00500 0.00343 0.00000 0.00926 H12A 0.34834 0.43228 0.32575 1.00000 0.06177 0.06415 0.00761 0.00652 0.00459 0.00000 0.01305 Final Structure Factor Calculation for 2009src0461p-1 in P-1 Total number of l.s. parameters = 142 Maximum vector length = 511 Memory required = 1913 / 24017 wR2 = 0.1271 before cycle 26 for 1849 data and 0 / 142 parameters Summary of restraints applied in cycle 26 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 10. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.129; Restrained GooF = 1.127 for 10 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0642 for 1358 Fo > 4sig(Fo) and 0.0970 for all 1849 data wR2 = 0.1271, GooF = S = 1.129, Restrained GooF = 1.127 for all data Occupancy sum of asymmetric unit = 13.00 for non-hydrogen and 5.00 for hydrogen atoms Principal mean square atomic displacements U 0.0316 0.0273 0.0155 C1_a 0.0316 0.0273 0.0155 C2_a 0.0316 0.0273 0.0155 C3_a 0.0316 0.0273 0.0155 C4_a 0.0340 0.0244 0.0158 S1_a 0.0227 0.0110 0.0033 C1B_b 0.0363 0.0319 0.0124 C2B_b 0.0363 0.0319 0.0124 C3B_b 0.0363 0.0319 0.0124 C4B_b 0.0308 0.0263 0.0161 S1B_b 0.0256 0.0209 0.0180 C8 0.0243 0.0200 0.0186 C5 0.0281 0.0239 0.0187 C10 0.0248 0.0214 0.0180 C7 0.0467 0.0264 0.0215 N11 0.0448 0.0207 0.0183 N12 0.0236 0.0226 0.0174 N6 0.0294 0.0219 0.0165 O9 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.016 0.023 0.034 0.044 0.055 0.071 0.092 0.130 1.000 Number in group 194. 190. 175. 198. 178. 178. 184. 187. 181. 184. GooF 1.218 1.227 1.168 1.158 1.128 1.195 1.130 1.066 0.901 1.055 K 6.111 1.817 1.196 1.067 0.977 0.984 0.988 1.000 1.002 1.014 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.67 inf Number in group 189. 181. 190. 184. 182. 185. 191. 178. 185. 184. GooF 1.207 1.110 1.144 1.255 1.210 1.178 1.007 0.949 1.007 1.180 K 1.028 1.103 1.072 1.042 1.013 0.984 0.992 0.995 1.021 1.011 R1 0.231 0.203 0.154 0.149 0.133 0.113 0.057 0.048 0.045 0.035 Recommended weighting scheme: WGHT 0.0000 0.7368 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) 3 2 10 10.60 0.31 3.16 0.005 0.99 -4 -2 8 25.97 8.64 3.07 0.027 0.85 -5 1 6 19.20 0.15 3.06 0.004 0.79 4 -1 9 35.23 1.48 2.94 0.011 0.97 0 0 9 7.47 0.11 2.89 0.003 1.11 1 4 7 11.48 28.16 2.87 0.049 1.12 -1 0 9 11.82 0.00 2.78 0.001 1.03 7 1 8 32.07 6.02 2.76 0.022 0.79 -4 -5 5 -0.23 13.85 2.76 0.034 0.95 -1 5 6 -1.86 31.38 2.73 0.051 0.92 -6 -2 2 -5.65 6.64 2.71 0.024 0.92 1 4 0 2941.04 2719.61 2.67 0.478 1.77 2 -5 5 10.46 0.68 2.67 0.008 1.00 7 3 0 17.81 1.69 2.66 0.012 0.85 -7 -6 1 -5.43 6.16 2.66 0.023 0.77 2 3 2 76.57 55.66 2.64 0.068 2.08 3 7 3 5.30 0.01 2.59 0.001 0.98 1 6 3 -1.73 3.57 2.58 0.017 1.10 6 7 4 59.04 31.94 2.52 0.052 0.83 3 0 6 12.53 24.48 2.49 0.045 1.45 1 -7 5 26.81 10.91 2.46 0.030 0.84 -6 2 2 12.21 29.52 2.41 0.050 0.78 0 1 5 740.72 667.59 2.41 0.237 1.87 -1 -7 7 25.36 51.31 2.40 0.066 0.82 1 -2 2 0.83 6.34 2.40 0.023 2.39 -2 -6 3 10.09 3.11 2.40 0.016 1.09 -1 7 1 11.25 1.50 2.39 0.011 0.87 0 6 6 4.31 18.87 2.38 0.040 0.89 -1 -2 5 -2.03 4.44 2.38 0.019 1.65 1 7 1 4.52 0.07 2.37 0.002 0.99 0 1 11 12.74 3.08 2.37 0.016 0.89 6 2 11 21.53 1.38 2.36 0.011 0.78 6 0 10 51.39 28.71 2.35 0.049 0.80 6 4 8 25.82 11.57 2.31 0.031 0.88 1 5 9 106.62 65.93 2.31 0.074 0.87 1 -7 2 52.40 34.18 2.30 0.054 0.88 4 -1 7 16.52 29.87 2.30 0.050 1.10 0 -1 6 629.68 554.33 2.30 0.216 1.63 -1 -1 10 4.97 0.00 2.29 0.000 0.94 0 5 9 16.68 4.46 2.29 0.019 0.82 4 4 9 7.19 0.76 2.29 0.008 0.95 -3 -9 2 20.14 0.59 2.27 0.007 0.77 2 -1 10 56.12 75.81 2.26 0.080 1.01 -3 2 8 9.12 0.72 2.22 0.008 0.84 -3 1 2 558.78 503.14 2.22 0.206 1.45 4 9 1 -0.59 9.27 2.22 0.028 0.78 2 6 5 7.25 1.07 2.22 0.010 1.04 1 1 4 569.13 513.78 2.21 0.208 2.46 -4 -7 6 19.92 4.03 2.20 0.018 0.79 -3 2 5 33.03 48.03 2.19 0.064 1.04 Bond lengths and angles C1_a - Distance Angles C2_a 1.4245 (0.0169) C5 1.4353 (0.0094) 121.90 (1.17) S1_a 1.6271 (0.0160) 113.92 (0.76) 124.12 (1.14) C1_a - C2_a C5 C2_a - Distance Angles C1_a 1.4245 (0.0169) C4_a 1.4577 (0.0123) 109.11 (1.07) H2_a 0.9500 125.45 125.45 C2_a - C1_a C4_a C3_a - Distance Angles C4_a 1.3644 (0.0083) S1_a 1.7134 (0.0074) 112.32 (1.19) H3_a 0.9500 123.84 123.84 C3_a - C4_a S1_a C4_a - Distance Angles C3_a 1.3644 (0.0083) C2_a 1.4577 (0.0123) 111.53 (1.31) H4_a 0.9500 124.24 124.24 C4_a - C3_a C2_a S1_a - Distance Angles C1_a 1.6271 (0.0160) C3_a 1.7134 (0.0074) 93.10 (0.65) S1_a - C1_a C1B_b - Distance Angles C2B_b 1.4471 (0.0215) C5 1.4494 (0.0130) 117.36 (1.50) S1B_b 1.6065 (0.0185) 113.41 (1.04) 129.16 (1.15) C1B_b - C2B_b C5 C2B_b - Distance Angles C1B_b 1.4471 (0.0215) C4B_b 1.4643 (0.0167) 108.58 (1.60) H2B_b 0.9500 125.71 125.71 C2B_b - C1B_b C4B_b C3B_b - Distance Angles C4B_b 1.3788 (0.0122) S1B_b 1.6939 (0.0105) 112.00 (1.79) H3B_b 0.9500 124.00 124.00 C3B_b - C4B_b S1B_b C4B_b - Distance Angles C3B_b 1.3788 (0.0123) C2B_b 1.4643 (0.0167) 111.29 (2.02) H4B_b 0.9500 124.35 124.35 C4B_b - C3B_b C2B_b S1B_b - Distance Angles C1B_b 1.6065 (0.0185) C3B_b 1.6939 (0.0105) 94.69 (0.81) S1B_b - C1B_b C8 - Distance Angles N12 1.3229 (0.0038) O9 1.3645 (0.0033) 118.29 (0.25) C7 1.3751 (0.0040) 134.45 (0.28) 107.23 (0.24) C8 - N12 O9 C5 - Distance Angles N6 1.2870 (0.0035) O9 1.3914 (0.0033) 113.51 (0.24) C1_a 1.4353 (0.0094) 126.69 (0.78) 119.80 (0.77) C1B_b 1.4494 (0.0130) 132.90 (0.84) 113.57 (0.83) 6.27 (1.48) C5 - N6 O9 C1_a C10 - Distance Angles N11 1.1562 (0.0037) C7 1.4094 (0.0040) 179.19 (0.33) C10 - N11 C7 - Distance Angles C8 1.3751 (0.0040) N6 1.4033 (0.0035) 109.19 (0.25) C10 1.4094 (0.0040) 127.31 (0.27) 123.40 (0.25) C7 - C8 N6 N11 - Distance Angles C10 1.1562 (0.0037) N11 - N12 - Distance Angles C8 1.3229 (0.0038) H12B 0.8701 (0.0355) 121.20 (2.23) H12A 0.9000 (0.0454) 119.75 (2.69) 119.02 (3.42) N12 - C8 H12B N6 - Distance Angles C5 1.2870 (0.0035) C7 1.4033 (0.0035) 104.95 (0.23) N6 - C5 O9 - Distance Angles C8 1.3645 (0.0033) C5 1.3914 (0.0033) 105.11 (0.20) O9 - C8 Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.87(4) 2.18(4) 3.016(4) 162(3) N12-H12B...N6_$1 0.90(5) 2.16(5) 3.044(4) 168(4) N12-H12A...N11_$2 FMAP and GRID set by program FMAP 2 1 18 GRID -3.333 -2 -2 3.333 2 2 R1 = 0.0960 for 1849 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.31 at 0.4053 0.0733 0.6857 [ 0.68 A from C3 ] Deepest hole -0.36 at 0.2673 0.2607 0.7615 [ 1.30 A from C4B ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 1940 / 15597 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.4053 0.0733 -0.3143 1.00000 0.05 0.31 0.68 C3 0.79 C3B 0.88 C4B 0.93 C4 Q2 1 0.7836 0.3408 0.3128 1.00000 0.05 0.29 0.69 C7 0.84 C10 1.66 C8 1.96 N11 Q3 1 1.5400 0.2511 -0.1363 1.00000 0.05 0.26 1.00 H2B 1.03 S1 1.29 C2B 1.93 C4B Q4 1 0.8371 0.1361 -0.1805 1.00000 0.05 0.25 0.82 H2 1.45 S1B 1.56 C2 2.15 H2B Q5 1 0.9565 0.5041 0.3971 1.00000 0.05 0.25 1.58 C10 1.63 N11 2.20 H12A 2.40 H4 Q6 1 0.6987 0.2703 0.1179 1.00000 0.05 0.25 0.66 O9 0.82 C8 1.77 N12 1.77 C5 Q7 1 0.3617 0.4130 0.2030 1.00000 0.05 0.24 0.55 H12B 0.62 N12 1.26 H12A 1.67 C8 Q8 1 0.6457 0.2938 0.0179 1.00000 0.05 0.24 0.85 O9 1.85 C8 2.07 H2B 2.13 C5 Q9 1 1.0549 0.1774 -0.0254 1.00000 0.05 0.23 0.76 C5 0.90 C1B 0.91 C1 1.73 O9 Q10 1 1.0653 0.2637 -0.1442 1.00000 0.05 0.23 0.66 C1B 0.79 C1 0.87 C2 1.13 S1B Shortest distances between peaks (including symmetry equivalents) 6 8 1.16 9 10 1.35 3 4 1.66 6 7 1.93 3 8 1.95 4 10 2.04 2 5 2.16 7 8 2.18 6 9 2.18 4 8 2.19 8 9 2.28 5 5 2.33 2 6 2.33 1 10 2.35 4 9 2.44 8 10 2.62 5 7 2.64 3 7 2.68 1 3 2.72 9 9 2.82 8 8 2.92 3 10 2.92 2 7 2.99 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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. 0.31: 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 1.14: Structure factors and derivatives 1.73: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.09: Apply other restraints 0.41: Solve l.s. equations 0.00: Generate HTAB table 0.09: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0461p-1 finished at 12:19:56 Total CPU time: 4.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++