+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 14:28:31 on 09-Oct-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 03src0043r in P-1 CELL 0.71073 8.8931 9.0266 13.6881 72.225 77.234 77.122 ZERR 2.00 0.0003 0.0002 0.0006 0.002 0.002 0.002 LATT 1 SFAC C H BR N O UNIT 38 66 2 4 2 V = 1006.10 F(000) = 408.0 Mu = 2.05 mm-1 Cell Wt = 770.77 Rho = 1.272 MERG 2 OMIT -3.00 55.00 EXTI 0.00654 DFIX 0.84 H51 O1 H52 O1 DANG 1.37 H51 H52 HFIX 43 -1.20 C7 FMAP 2 PLAN 10 SIZE 0.01 0.20 0.24 ACTA BOND $H WGHT 0.04050 0.79770 L.S. 15 TEMP -153.00 FVAR 0.47921 BR1 3 0.165559 0.125644 0.577679 11.00000 0.02846 0.02838 = 0.06107 -0.01632 -0.00902 -0.00504 N1 4 0.389649 0.760333 0.363238 11.00000 0.02434 0.02112 = 0.02698 -0.00774 -0.00388 -0.00374 N2 4 0.249042 0.593000 0.359376 11.00000 0.02290 0.02384 = 0.02959 -0.00804 -0.00404 -0.00522 C1 1 0.417054 1.356508 -0.097979 11.00000 0.06489 0.04765 = 0.03569 -0.00516 -0.00506 0.00340 AFIX 137 H1A 2 0.447614 1.441816 -0.080376 11.00000 -1.50000 H1B 2 0.339622 1.401249 -0.144763 11.00000 -1.50000 H1C 2 0.509355 1.298366 -0.132493 11.00000 -1.50000 AFIX 0 C2 1 0.346734 1.245202 0.000616 11.00000 0.04605 0.03274 = 0.03745 -0.00752 -0.01048 -0.00043 AFIX 23 H2A 2 0.251866 1.304045 0.033942 11.00000 -1.20000 H2B 2 0.314473 1.160459 -0.017906 11.00000 -1.20000 AFIX 0 C3 1 0.458266 1.171537 0.077481 11.00000 0.03647 0.02970 = 0.03850 -0.00568 -0.00545 -0.00784 AFIX 23 H3A 2 0.493790 1.256829 0.093318 11.00000 -1.20000 H3B 2 0.551307 1.109938 0.044550 11.00000 -1.20000 AFIX 0 C4 1 0.390206 1.064454 0.178539 11.00000 0.03326 0.02794 = 0.03863 -0.00596 -0.00801 -0.00721 AFIX 23 H4A 2 0.356771 0.977439 0.163322 11.00000 -1.20000 H4B 2 0.296313 1.125103 0.211421 11.00000 -1.20000 AFIX 0 C5 1 0.505131 0.994874 0.254593 11.00000 0.02907 0.02246 = 0.03773 -0.00696 -0.00603 -0.00713 AFIX 23 H5A 2 0.591006 0.921400 0.225725 11.00000 -1.20000 H5B 2 0.551395 1.081309 0.260434 11.00000 -1.20000 AFIX 0 C6 1 0.435378 0.907545 0.362397 11.00000 0.03325 0.02090 = 0.03787 -0.01053 -0.00933 -0.00452 AFIX 23 H6A 2 0.512734 0.882818 0.409582 11.00000 -1.20000 H6B 2 0.342357 0.976509 0.388992 11.00000 -1.20000 AFIX 0 C7 1 0.248448 0.740460 0.359224 11.00000 0.02733 0.02536 = 0.02635 -0.00706 -0.00497 -0.00486 C8 1 0.490344 0.617601 0.366275 11.00000 0.02451 0.02118 = 0.02313 -0.00571 -0.00107 -0.00341 C9 1 0.648544 0.572995 0.372946 11.00000 0.02588 0.02745 = 0.02817 -0.00689 -0.00497 -0.00489 AFIX 43 H9 2 0.709910 0.645458 0.374886 11.00000 -1.20000 AFIX 0 C10 1 0.711125 0.418412 0.376574 11.00000 0.02495 0.03121 = 0.02849 -0.00747 -0.00190 -0.00115 AFIX 43 H10 2 0.819003 0.383074 0.380838 11.00000 -1.20000 AFIX 0 C11 1 0.620600 0.310926 0.374177 11.00000 0.03447 0.02095 = 0.03036 -0.00858 0.00029 0.00016 AFIX 43 H11 2 0.668823 0.204931 0.377040 11.00000 -1.20000 AFIX 0 C12 1 0.464224 0.354814 0.367806 11.00000 0.03274 0.02484 = 0.02718 -0.00899 -0.00168 -0.00746 AFIX 43 H12 2 0.402851 0.282135 0.366198 11.00000 -1.20000 AFIX 0 C13 1 0.400860 0.511033 0.363850 11.00000 0.02453 0.02505 = 0.02052 -0.00545 -0.00231 -0.00508 C14 1 0.117541 0.528384 0.349500 11.00000 0.02573 0.03041 = 0.03634 -0.00875 -0.00305 -0.01036 AFIX 23 H14A 2 0.018359 0.596822 0.368356 11.00000 -1.20000 H14B 2 0.116259 0.422210 0.398750 11.00000 -1.20000 AFIX 0 C15 1 0.127959 0.516578 0.240192 11.00000 0.03184 0.03216 = 0.03582 -0.01226 -0.00571 -0.01119 AFIX 23 H15A 2 0.049901 0.453210 0.240865 11.00000 -1.20000 H15B 2 0.232808 0.459170 0.218830 11.00000 -1.20000 AFIX 0 C16 1 0.100883 0.673858 0.159673 11.00000 0.03356 0.03215 = 0.03827 -0.01463 -0.00536 -0.00727 AFIX 23 H16A 2 0.177044 0.738856 0.159672 11.00000 -1.20000 H16B 2 -0.005346 0.730274 0.179162 11.00000 -1.20000 AFIX 0 C17 1 0.117173 0.656048 0.051016 11.00000 0.03947 0.03554 = 0.03654 -0.01389 -0.00491 -0.00867 AFIX 23 H17A 2 0.223561 0.599431 0.032145 11.00000 -1.20000 H17B 2 0.041713 0.589737 0.051867 11.00000 -1.20000 AFIX 0 C18 1 0.090293 0.809702 -0.032208 11.00000 0.04190 0.03787 = 0.04232 -0.01022 -0.00974 -0.01052 AFIX 23 H18A 2 -0.017386 0.865012 -0.015136 11.00000 -1.20000 H18B 2 0.163624 0.877680 -0.032214 11.00000 -1.20000 AFIX 0 C19 1 0.112455 0.787221 -0.139612 11.00000 0.07106 0.06121 = 0.03624 -0.00753 -0.00974 -0.01981 AFIX 137 H19A 2 0.218969 0.732824 -0.157203 11.00000 -1.50000 H19B 2 0.095699 0.890386 -0.190321 11.00000 -1.50000 H19C 2 0.037090 0.723855 -0.141055 11.00000 -1.50000 AFIX 0 O1 5 1.055604 0.151873 0.361896 11.00000 0.05822 0.05937 = 0.06314 -0.01003 -0.01281 -0.02152 H51 2 0.987575 0.084798 0.375632 11.00000 -1.50000 H52 2 1.077227 0.143970 0.425800 11.00000 -1.50000 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 Covalent radii and connectivity table for 03src0043r in P-1 C 0.770 H 0.320 BR 1.140 N 0.700 O 0.660 Br1 - no bonds found N1 - C7 C8 C6 N2 - C7 C13 C14 C1 - C2 C2 - C3 C1 C3 - C2 C4 C4 - C3 C5 C5 - C6 C4 C6 - N1 C5 C7 - N1 N2 C8 - C9 C13 N1 C9 - C10 C8 C10 - C9 C11 C11 - C12 C10 C12 - C11 C13 C13 - C12 C8 N2 C14 - N2 C15 C15 - C14 C16 C16 - C15 C17 C17 - C18 C16 C18 - C19 C17 C19 - C18 O1 - no bonds found 20601 Reflections read, of which 18 rejected -11 =< h =< 11, -11 =< k =< 11, -17 =< l =< 17, Max. 2-theta = 55.00 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 1 10 4 16.85 4.73 2 28.71 6 -5 5 10.03 1.32 5 10.54 6 -4 6 32.79 1.69 7 8.68 -5 5 6 3.16 0.79 7 4.52 -6 3 10 6.18 1.48 5 11.77 -2 7 10 4.44 0.97 6 8.53 -3 8 11 11.98 2.76 2 13.90 7 Inconsistent equivalents 4615 Unique reflections, of which 0 suppressed R(int) = 0.0727 R(sigma) = 0.0500 Friedel opposites merged Maximum memory for data reduction = 2702 / 45906 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 = 3393 / 269878 wR2 = 0.0952 before cycle 1 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.9008 0.8400 0.0608 0.0200 DFIX H51 O1 0.9151 0.8400 0.0751 0.0200 DFIX H52 O1 Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.068 0.061 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.976; Restrained GooF = 0.979 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47905 0.00083 -0.197 OSF 2 0.00632 0.00133 -0.164 EXTI Mean shift/su = 0.139 Maximum = 2.132 for U12 C7 Max. shift = 0.015 A for H19A Max. dU = 0.000 for C7 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0950 before cycle 2 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.9089 0.8400 0.0689 0.0200 DFIX H52 O1 Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.064 0.054 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.975; Restrained GooF = 0.977 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47897 0.00083 -0.093 OSF 2 0.00624 0.00132 -0.066 EXTI Mean shift/su = 0.048 Maximum = 0.690 for U12 C7 Max. shift = 0.006 A for H19A Max. dU = 0.000 for O1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0950 before cycle 3 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 0.9069 0.8400 0.0669 0.0200 DFIX H52 O1 Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.062 0.052 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.975; Restrained GooF = 0.977 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47897 0.00083 -0.002 OSF 2 0.00623 0.00131 -0.004 EXTI Mean shift/su = 0.002 Maximum = -0.019 for U33 C14 Max. shift = 0.001 A for H52 Max. dU = 0.000 for C14 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0950 before cycle 4 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.9067 0.8400 0.0667 0.0200 DFIX H52 O1 Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.062 0.052 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.975; Restrained GooF = 0.977 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47897 0.00083 0.000 OSF 2 0.00623 0.00131 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.004 for tors H1A Max. shift = 0.000 A for H52 Max. dU = 0.000 for C19 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0950 before cycle 5 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 0.9067 0.8400 0.0667 0.0200 DFIX H52 O1 Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.062 0.052 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.975; Restrained GooF = 0.977 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47897 0.00083 0.000 OSF 2 0.00623 0.00131 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for z Br1 Max. shift = 0.000 A for H52 Max. dU = 0.000 for O1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0950 before cycle 6 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint 0.9067 0.8400 0.0667 0.0200 DFIX H52 O1 Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.062 0.052 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.975; Restrained GooF = 0.977 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47897 0.00083 0.000 OSF 2 0.00623 0.00131 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H52 Max. dU = 0.000 for C8 Least-squares cycle 7 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0950 before cycle 7 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint 0.9067 0.8400 0.0667 0.0200 DFIX H52 O1 Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.062 0.052 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.975; Restrained GooF = 0.977 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47897 0.00083 0.000 OSF 2 0.00623 0.00131 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H52 Max. dU = 0.000 for C1 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0950 before cycle 8 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint 0.9067 0.8400 0.0667 0.0200 DFIX H52 O1 Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.062 0.052 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.975; Restrained GooF = 0.977 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47897 0.00083 0.000 OSF 2 0.00623 0.00131 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for z Br1 Max. shift = 0.000 A for H52 Max. dU = 0.000 for C1 Least-squares cycle 9 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0950 before cycle 9 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint 0.9067 0.8400 0.0667 0.0200 DFIX H52 O1 Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.062 0.052 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.975; Restrained GooF = 0.977 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47897 0.00083 0.000 OSF 2 0.00623 0.00131 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for z Br1 Max. shift = 0.000 A for H51 Max. dU = 0.000 for O1 Least-squares cycle 10 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0950 before cycle 10 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 10 Observed Target Error Sigma Restraint 0.9067 0.8400 0.0667 0.0200 DFIX H52 O1 Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.062 0.052 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.975; Restrained GooF = 0.977 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47897 0.00083 0.000 OSF 2 0.00623 0.00131 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for z Br1 Max. shift = 0.000 A for H52 Max. dU = 0.000 for O1 Least-squares cycle 11 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0950 before cycle 11 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 11 Observed Target Error Sigma Restraint 0.9067 0.8400 0.0667 0.0200 DFIX H52 O1 Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.062 0.052 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.975; Restrained GooF = 0.977 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47897 0.00083 0.000 OSF 2 0.00623 0.00131 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for z Br1 Max. shift = 0.000 A for H51 Max. dU = 0.000 for C2 Least-squares cycle 12 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0950 before cycle 12 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 12 Observed Target Error Sigma Restraint 0.9067 0.8400 0.0667 0.0200 DFIX H52 O1 Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.062 0.052 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.975; Restrained GooF = 0.977 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47897 0.00083 0.000 OSF 2 0.00623 0.00131 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for z Br1 Max. shift = 0.000 A for H52 Max. dU = 0.000 for O1 Least-squares cycle 13 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0950 before cycle 13 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 13 Observed Target Error Sigma Restraint 0.9067 0.8400 0.0667 0.0200 DFIX H52 O1 Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.062 0.052 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.975; Restrained GooF = 0.977 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47897 0.00083 0.000 OSF 2 0.00623 0.00131 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for z Br1 Max. shift = 0.000 A for H51 Max. dU = 0.000 for C19 Least-squares cycle 14 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0950 before cycle 14 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 14 Observed Target Error Sigma Restraint 0.9067 0.8400 0.0667 0.0200 DFIX H52 O1 Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.062 0.052 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.975; Restrained GooF = 0.977 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47897 0.00083 0.000 OSF 2 0.00623 0.00131 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for z Br1 Max. shift = 0.000 A for H52 Max. dU = 0.000 for C13 Least-squares cycle 15 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0950 before cycle 15 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 15 Observed Target Error Sigma Restraint 0.9067 0.8400 0.0667 0.0200 DFIX H52 O1 Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.062 0.052 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.975; Restrained GooF = 0.977 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47897 0.00083 0.000 OSF 2 0.00623 0.00131 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for z Br1 Max. shift = 0.000 A for C3 Max. dU = 0.000 for O1 Largest correlation matrix elements -0.726 y H51 / x H51 0.607 U11 Br1 / OSF 0.545 U33 Br1 / OSF 0.610 U22 Br1 / OSF -0.551 z H52 / x H52 0.541 EXTI / OSF Idealized hydrogen atom generation before cycle 16 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.4468 1.4422 -0.0802 137 0.980 0.000 C1 C2 H1A H1B 0.3403 1.4004 -0.1450 137 0.980 0.000 C1 C2 H1A H1C 0.5102 1.2985 -0.1319 137 0.980 0.000 C1 C2 H1A H2A 0.2517 1.3038 0.0339 23 0.990 0.000 C2 C3 C1 H2B 0.3146 1.1603 -0.0180 23 0.990 0.000 C2 C3 C1 H3A 0.4938 1.2568 0.0933 23 0.990 0.000 C3 C2 C4 H3B 0.5514 1.1098 0.0446 23 0.990 0.000 C3 C2 C4 H4A 0.3565 0.9776 0.1633 23 0.990 0.000 C4 C3 C5 H4B 0.2963 1.1253 0.2114 23 0.990 0.000 C4 C3 C5 H5A 0.5911 0.9210 0.2258 23 0.990 0.000 C5 C6 C4 H5B 0.5519 1.0810 0.2604 23 0.990 0.000 C5 C6 C4 H6A 0.5125 0.8829 0.4097 23 0.990 0.000 C6 N1 C5 H6B 0.3423 0.9767 0.3889 23 0.990 0.000 C6 N1 C5 H7 0.1587 0.8208 0.3566 43 0.950 0.000 C7 N1 N2 H9 0.7098 0.6455 0.3752 43 0.950 0.000 C9 C10 C8 H10 0.8192 0.3831 0.3807 43 0.950 0.000 C10 C9 C11 H11 0.6688 0.2048 0.3771 43 0.950 0.000 C11 C12 C10 H12 0.4028 0.2821 0.3661 43 0.950 0.000 C12 C11 C13 H14A 0.0183 0.5968 0.3686 23 0.990 0.000 C14 N2 C15 H14B 0.1163 0.4222 0.3990 23 0.990 0.000 C14 N2 C15 H15A 0.0501 0.4531 0.2408 23 0.990 0.000 C15 C14 C16 H15B 0.2330 0.4592 0.2188 23 0.990 0.000 C15 C14 C16 H16A 0.1771 0.7389 0.1597 23 0.990 0.000 C16 C15 C17 H16B -0.0053 0.7302 0.1792 23 0.990 0.000 C16 C15 C17 H17A 0.2237 0.5994 0.0321 23 0.990 0.000 C17 C18 C16 H17B 0.0419 0.5895 0.0518 23 0.990 0.000 C17 C18 C16 H18A -0.0175 0.8650 -0.0152 23 0.990 0.000 C18 C19 C17 H18B 0.1635 0.8778 -0.0323 23 0.990 0.000 C18 C19 C17 H19A 0.2181 0.7308 -0.1566 137 0.980 0.000 C19 C18 H19A H19B 0.0977 0.8904 -0.1905 137 0.980 0.000 C19 C18 H19A H19C 0.0354 0.7257 -0.1414 137 0.980 0.000 C19 C18 H19A 03src0043r in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Br1 0.16555 0.12565 0.57768 1.00000 0.02843 0.02835 0.06104 -0.01631 -0.00900 -0.00505 0.03797 0.00036 0.00003 0.00003 0.00002 0.00000 0.00015 0.00015 0.00021 0.00012 0.00011 0.00009 0.00011 N1 0.38964 0.76031 0.36326 1.00000 0.02415 0.02108 0.02680 -0.00767 -0.00386 -0.00367 0.02380 0.00260 0.00021 0.00021 0.00015 0.00000 0.00094 0.00090 0.00106 0.00075 0.00078 0.00070 0.00040 N2 0.24911 0.59304 0.35934 1.00000 0.02285 0.02384 0.02935 -0.00780 -0.00405 -0.00531 0.02501 0.00266 0.00022 0.00021 0.00016 0.00000 0.00092 0.00094 0.00111 0.00078 0.00079 0.00072 0.00041 C1 0.41721 1.35638 -0.09783 1.00000 0.06492 0.04755 0.03563 -0.00516 -0.00505 0.00337 0.05339 0.00529 0.00041 0.00037 0.00024 0.00000 0.00209 0.00175 0.00173 0.00132 0.00148 0.00144 0.00081 H1A 0.44677 1.44216 -0.08016 1.00000 0.08009 0.00000 0.00000 H1B 0.34027 1.40044 -0.14500 1.00000 0.08009 0.00000 0.00000 H1C 0.51017 1.29848 -0.13194 1.00000 0.08009 0.00000 0.00000 C2 0.34667 1.24502 0.00061 1.00000 0.04595 0.03282 0.03757 -0.00777 -0.01071 -0.00031 0.03959 0.00410 0.00033 0.00031 0.00022 0.00000 0.00156 0.00135 0.00158 0.00112 0.00124 0.00111 0.00062 H2A 0.25172 1.30379 0.03392 1.00000 0.04750 0.00000 0.00000 H2B 0.31458 1.16026 -0.01799 1.00000 0.04750 0.00000 0.00000 C3 0.45832 1.17147 0.07749 1.00000 0.03669 0.02950 0.03847 -0.00562 -0.00548 -0.00798 0.03542 0.00380 0.00031 0.00029 0.00021 0.00000 0.00137 0.00126 0.00156 0.00106 0.00115 0.00101 0.00057 H3A 0.49381 1.25681 0.09330 1.00000 0.04250 0.00000 0.00000 H3B 0.55137 1.10983 0.04460 1.00000 0.04250 0.00000 0.00000 C4 0.39011 1.06451 0.17852 1.00000 0.03298 0.02790 0.03869 -0.00586 -0.00804 -0.00728 0.03320 0.00360 0.00029 0.00028 0.00021 0.00000 0.00129 0.00122 0.00153 0.00103 0.00111 0.00097 0.00055 H4A 0.35651 0.97757 0.16331 1.00000 0.03984 0.00000 0.00000 H4B 0.29632 1.12526 0.21142 1.00000 0.03984 0.00000 0.00000 C5 0.50539 0.99466 0.25465 1.00000 0.02907 0.02255 0.03762 -0.00701 -0.00607 -0.00730 0.02941 0.00334 0.00028 0.00026 0.00020 0.00000 0.00119 0.00111 0.00146 0.00096 0.00104 0.00089 0.00052 H5A 0.59108 0.92098 0.22582 1.00000 0.03530 0.00000 0.00000 H5B 0.55189 1.08097 0.26043 1.00000 0.03530 0.00000 0.00000 C6 0.43534 0.90761 0.36244 1.00000 0.03300 0.02089 0.03760 -0.01059 -0.00912 -0.00448 0.02934 0.00328 0.00029 0.00026 0.00020 0.00000 0.00124 0.00110 0.00146 0.00096 0.00107 0.00090 0.00052 H6A 0.51252 0.88294 0.40974 1.00000 0.03520 0.00000 0.00000 H6B 0.34225 0.97668 0.38887 1.00000 0.03520 0.00000 0.00000 C7 0.24850 0.74047 0.35921 1.00000 0.02610 0.02396 0.02778 -0.00743 -0.00538 -0.00242 0.02598 0.00321 0.00027 0.00026 0.00019 0.00000 0.00112 0.00111 0.00129 0.00090 0.00094 0.00085 0.00048 H7 0.15874 0.82075 0.35657 1.00000 0.03117 0.00000 0.00000 C8 0.49032 0.61762 0.36627 1.00000 0.02453 0.02120 0.02290 -0.00554 -0.00135 -0.00335 0.02346 0.00318 0.00026 0.00025 0.00018 0.00000 0.00109 0.00105 0.00122 0.00086 0.00089 0.00082 0.00046 C9 0.64857 0.57304 0.37308 1.00000 0.02577 0.02779 0.02800 -0.00702 -0.00491 -0.00492 0.02715 0.00334 0.00027 0.00027 0.00019 0.00000 0.00113 0.00116 0.00132 0.00094 0.00096 0.00088 0.00049 H9 0.70983 0.64547 0.37521 1.00000 0.03258 0.00000 0.00000 C10 0.71130 0.41838 0.37657 1.00000 0.02489 0.03086 0.02839 -0.00735 -0.00200 -0.00105 0.02918 0.00352 0.00027 0.00027 0.00019 0.00000 0.00115 0.00123 0.00134 0.00097 0.00097 0.00091 0.00051 H10 0.81922 0.38309 0.38071 1.00000 0.03502 0.00000 0.00000 C11 0.62064 0.31077 0.37420 1.00000 0.03450 0.02091 0.02984 -0.00826 0.00017 -0.00002 0.02974 0.00358 0.00028 0.00026 0.00019 0.00000 0.00127 0.00111 0.00137 0.00093 0.00103 0.00090 0.00052 H11 0.66882 0.20475 0.37712 1.00000 0.03569 0.00000 0.00000 C12 0.46418 0.35477 0.36776 1.00000 0.03284 0.02460 0.02695 -0.00902 -0.00150 -0.00755 0.02776 0.00334 0.00028 0.00026 0.00019 0.00000 0.00124 0.00114 0.00131 0.00093 0.00099 0.00092 0.00050 H12 0.40278 0.28214 0.36613 1.00000 0.03331 0.00000 0.00000 C13 0.40091 0.51095 0.36378 1.00000 0.02433 0.02497 0.02060 -0.00529 -0.00237 -0.00510 0.02355 0.00316 0.00026 0.00025 0.00018 0.00000 0.00108 0.00109 0.00118 0.00085 0.00089 0.00083 0.00045 C14 0.11751 0.52832 0.34970 1.00000 0.02559 0.03046 0.03633 -0.00879 -0.00297 -0.01045 0.03024 0.00332 0.00027 0.00028 0.00020 0.00000 0.00115 0.00122 0.00146 0.00101 0.00102 0.00092 0.00052 H14A 0.01833 0.59676 0.36856 1.00000 0.03629 0.00000 0.00000 H14B 0.11630 0.42215 0.39898 1.00000 0.03629 0.00000 0.00000 C15 0.12807 0.51649 0.24018 1.00000 0.03179 0.03198 0.03585 -0.01219 -0.00573 -0.01104 0.03154 0.00334 0.00029 0.00028 0.00020 0.00000 0.00126 0.00125 0.00149 0.00104 0.00108 0.00098 0.00054 H15A 0.05007 0.45308 0.24081 1.00000 0.03785 0.00000 0.00000 H15B 0.23296 0.45915 0.21883 1.00000 0.03785 0.00000 0.00000 C16 0.10093 0.67385 0.15971 1.00000 0.03338 0.03230 0.03844 -0.01469 -0.00539 -0.00725 0.03331 0.00350 0.00030 0.00029 0.00021 0.00000 0.00129 0.00128 0.00154 0.00108 0.00111 0.00099 0.00055 H16A 0.17708 0.73886 0.15970 1.00000 0.03997 0.00000 0.00000 H16B -0.00531 0.73024 0.17920 1.00000 0.03997 0.00000 0.00000 C17 0.11725 0.65593 0.05095 1.00000 0.03946 0.03562 0.03643 -0.01375 -0.00481 -0.00891 0.03604 0.00369 0.00032 0.00030 0.00021 0.00000 0.00140 0.00137 0.00154 0.00111 0.00116 0.00107 0.00058 H17A 0.22367 0.59940 0.03205 1.00000 0.04325 0.00000 0.00000 H17B 0.04185 0.58954 0.05182 1.00000 0.04325 0.00000 0.00000 C18 0.09019 0.80972 -0.03228 1.00000 0.04167 0.03769 0.04241 -0.01021 -0.00953 -0.01035 0.03969 0.00389 0.00034 0.00031 0.00022 0.00000 0.00149 0.00143 0.00168 0.00118 0.00125 0.00113 0.00062 H18A -0.01750 0.86497 -0.01516 1.00000 0.04763 0.00000 0.00000 H18B 0.16350 0.87775 -0.03233 1.00000 0.04763 0.00000 0.00000 C19 0.11228 0.78719 -0.13960 1.00000 0.07128 0.06118 0.03620 -0.00736 -0.01010 -0.01952 0.05596 0.00483 0.00044 0.00041 0.00025 0.00000 0.00225 0.00201 0.00178 0.00145 0.00159 0.00167 0.00083 H19A 0.21805 0.73077 -0.15660 1.00000 0.08393 0.00000 0.00000 H19B 0.09772 0.89042 -0.19052 1.00000 0.08393 0.00000 0.00000 H19C 0.03542 0.72573 -0.14140 1.00000 0.08393 0.00000 0.00000 O1 1.05563 0.15188 0.36187 1.00000 0.05823 0.05974 0.06326 -0.00993 -0.01305 -0.02156 0.05952 0.00345 0.00029 0.00028 0.00020 0.00000 0.00145 0.00144 0.00163 0.00118 0.00124 0.00110 0.00061 H51 0.98769 0.08536 0.37530 1.00000 0.08928 0.03830 0.00406 0.00415 0.00317 0.00000 0.00000 H52 1.07785 0.14273 0.42521 1.00000 0.08928 0.03961 0.00491 0.00485 0.00203 0.00000 0.00000 Final Structure Factor Calculation for 03src0043r in P-1 Total number of l.s. parameters = 217 Maximum vector length = 511 Memory required = 3176 / 24017 wR2 = 0.0950 before cycle 16 for 4615 data and 0 / 217 parameters Disagreeable restraints before cycle 16 Observed Target Error Sigma Restraint 0.9067 0.8400 0.0667 0.0200 DFIX H52 O1 Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.062 0.052 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.975; Restrained GooF = 0.977 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0405 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0397 for 3747 Fo > 4sig(Fo) and 0.0563 for all 4615 data wR2 = 0.0950, GooF = S = 0.975, Restrained GooF = 0.977 for all data Occupancy sum of asymmetric unit = 23.00 for non-hydrogen and 33.00 for hydrogen atoms Principal mean square atomic displacements U 0.0611 0.0286 0.0242 Br1 0.0269 0.0242 0.0203 N1 0.0295 0.0245 0.0211 N2 0.0810 0.0450 0.0342 C1 0.0497 0.0386 0.0304 C2 0.0412 0.0371 0.0280 C3 0.0410 0.0320 0.0266 C4 0.0383 0.0296 0.0204 C5 0.0389 0.0307 0.0184 C6 0.0282 0.0265 0.0232 C7 0.0278 0.0214 0.0212 C8 0.0286 0.0275 0.0253 C9 0.0358 0.0287 0.0230 C10 0.0424 0.0280 0.0189 C11 0.0353 0.0260 0.0220 C12 0.0256 0.0248 0.0203 C13 0.0372 0.0331 0.0204 C14 0.0380 0.0347 0.0219 C15 0.0405 0.0336 0.0258 C16 0.0419 0.0370 0.0292 C17 0.0455 0.0403 0.0332 C18 0.0753 0.0569 0.0357 C19 0.0746 0.0595 0.0444 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.028 0.041 0.056 0.070 0.086 0.106 0.137 0.191 1.000 Number in group 462. 486. 438. 483. 459. 456. 455. 458. 453. 465. GooF 0.933 0.995 1.049 0.974 1.019 0.997 0.943 1.000 0.908 0.922 K 1.989 1.267 1.037 1.021 1.010 1.003 0.995 1.003 1.004 1.006 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.66 inf Number in group 476. 460. 452. 465. 455. 464. 457. 460. 462. 464. GooF 0.894 0.871 0.929 0.965 0.930 0.956 0.957 0.881 0.891 1.370 K 1.022 1.007 0.999 1.004 1.005 1.017 1.017 1.019 1.008 1.000 R1 0.169 0.132 0.107 0.087 0.063 0.050 0.039 0.029 0.025 0.030 Recommended weighting scheme: WGHT 0.0338 0.7173 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 1 2 145.77 87.58 5.64 0.061 4.03 2 -2 2 250.49 166.48 5.26 0.084 2.49 4 4 3 48.98 91.60 4.96 0.063 1.75 0 0 3 6851.17 8227.43 4.23 0.594 4.29 1 1 2 666.44 524.05 4.22 0.150 5.65 -3 -5 12 122.16 0.29 4.16 0.004 0.77 -4 0 1 154.47 217.10 4.10 0.096 2.05 -2 2 2 320.92 411.04 3.92 0.133 2.62 3 1 2 290.47 374.86 3.77 0.127 2.89 3 -2 3 129.13 178.71 3.74 0.087 1.95 -1 -3 3 809.55 664.92 3.72 0.169 2.07 6 -3 9 63.73 32.17 3.71 0.037 0.93 5 3 1 42.32 17.91 3.68 0.028 1.63 -1 -1 4 340.92 267.77 3.58 0.107 2.57 0 -3 4 293.37 387.61 3.56 0.129 1.88 1 0 4 605.07 742.89 3.44 0.178 3.19 2 3 0 17.25 35.29 3.44 0.039 2.56 2 5 4 433.47 358.21 3.20 0.124 1.74 0 4 5 303.51 374.75 3.19 0.127 1.91 6 1 9 225.71 171.11 3.18 0.086 1.15 3 4 15 39.55 71.96 3.16 0.056 0.91 1 -7 9 34.09 64.98 3.14 0.053 0.82 0 9 10 67.14 102.62 3.12 0.066 0.88 -4 -3 3 39.71 17.07 3.08 0.027 1.54 -2 -4 3 157.97 120.80 3.08 0.072 1.64 1 -1 3 134.80 182.97 3.05 0.089 3.29 1 -1 4 233.17 292.18 3.04 0.112 2.70 -2 -2 12 55.00 24.18 2.99 0.032 0.93 -4 6 1 18.76 2.73 2.99 0.011 1.10 5 3 14 41.29 17.79 2.95 0.028 0.93 4 0 3 231.96 286.62 2.95 0.111 2.05 -1 2 1 2448.28 2786.49 2.94 0.345 3.59 4 -1 11 87.36 56.50 2.93 0.049 1.05 6 -3 8 120.97 162.02 2.93 0.083 0.97 4 3 11 179.83 135.37 2.90 0.076 1.17 8 4 13 64.06 17.20 2.85 0.027 0.84 6 -8 2 47.63 92.52 2.83 0.063 0.77 4 4 1 330.96 274.35 2.81 0.108 1.71 1 1 1 32.79 10.90 2.81 0.022 6.89 6 -4 11 37.03 11.48 2.79 0.022 0.80 4 -1 15 -2.14 12.89 2.78 0.023 0.81 -1 1 7 1353.67 1554.86 2.77 0.258 1.78 5 -1 2 222.83 271.55 2.77 0.108 1.62 7 -3 8 110.48 80.70 2.75 0.059 0.90 6 -3 1 -2.60 8.05 2.74 0.019 1.19 2 -5 6 35.43 20.86 2.74 0.030 1.13 -8 3 4 94.58 64.60 2.73 0.053 0.90 3 -2 12 -3.01 18.57 2.71 0.028 0.96 7 -2 10 21.67 8.80 2.70 0.019 0.88 -5 4 3 432.63 367.33 2.68 0.125 1.20 Bond lengths and angles N1 - Distance Angles C7 1.3219 (0.0029) C8 1.3900 (0.0028) 108.19 (0.18) C6 1.4707 (0.0028) 126.61 (0.19) 125.18 (0.19) N1 - C7 C8 N2 - Distance Angles C7 1.3290 (0.0028) C13 1.3922 (0.0028) 107.88 (0.18) C14 1.4658 (0.0029) 126.91 (0.19) 125.10 (0.18) N2 - C7 C13 C1 - Distance Angles C2 1.5166 (0.0041) H1A 0.9800 109.47 H1B 0.9800 109.47 109.47 H1C 0.9800 109.47 109.47 109.47 C1 - C2 H1A H1B C2 - Distance Angles C3 1.5084 (0.0037) C1 1.5166 (0.0041) 112.80 (0.25) H2A 0.9900 109.03 109.03 H2B 0.9900 109.03 109.03 107.80 C2 - C3 C1 H2A C3 - Distance Angles C2 1.5084 (0.0037) C4 1.5125 (0.0036) 114.38 (0.22) H3A 0.9900 108.66 108.66 H3B 0.9900 108.66 108.66 107.60 C3 - C2 C4 H3A C4 - Distance Angles C3 1.5125 (0.0036) C5 1.5223 (0.0034) 112.81 (0.21) H4A 0.9900 109.03 109.03 H4B 0.9900 109.03 109.03 107.80 C4 - C3 C5 H4A C5 - Distance Angles C6 1.5122 (0.0035) C4 1.5223 (0.0034) 114.62 (0.20) H5A 0.9900 108.61 108.61 H5B 0.9900 108.61 108.61 107.57 C5 - C6 C4 H5A C6 - Distance Angles N1 1.4707 (0.0028) C5 1.5122 (0.0035) 112.04 (0.20) H6A 0.9900 109.20 109.20 H6B 0.9900 109.20 109.20 107.90 C6 - N1 C5 H6A C7 - Distance Angles N1 1.3219 (0.0029) N2 1.3290 (0.0028) 110.85 (0.19) H7 0.9500 124.58 124.58 C7 - N1 N2 C8 - Distance Angles C9 1.3907 (0.0031) C13 1.3906 (0.0031) 121.68 (0.20) N1 1.3900 (0.0028) 131.76 (0.20) 106.54 (0.19) C8 - C9 C13 C9 - Distance Angles C10 1.3735 (0.0033) C8 1.3907 (0.0031) 116.23 (0.21) H9 0.9500 121.89 121.89 C9 - C10 C8 C10 - Distance Angles C9 1.3735 (0.0033) C11 1.4052 (0.0034) 121.97 (0.22) H10 0.9500 119.01 119.01 C10 - C9 C11 C11 - Distance Angles C12 1.3740 (0.0034) C10 1.4052 (0.0034) 121.77 (0.21) H11 0.9500 119.11 119.11 C11 - C12 C10 C12 - Distance Angles C11 1.3740 (0.0034) C13 1.3856 (0.0031) 116.31 (0.21) H12 0.9500 121.85 121.85 C12 - C11 C13 C13 - Distance Angles C12 1.3856 (0.0031) C8 1.3906 (0.0031) 122.04 (0.21) N2 1.3922 (0.0028) 131.41 (0.21) 106.54 (0.18) C13 - C12 C8 C14 - Distance Angles N2 1.4658 (0.0029) C15 1.5161 (0.0036) 111.72 (0.20) H14A 0.9900 109.27 109.27 H14B 0.9900 109.27 109.27 107.94 C14 - N2 C15 H14A C15 - Distance Angles C14 1.5161 (0.0036) C16 1.5162 (0.0035) 114.56 (0.20) H15A 0.9900 108.62 108.62 H15B 0.9900 108.62 108.62 107.58 C15 - C14 C16 H15A C16 - Distance Angles C15 1.5162 (0.0035) C17 1.5180 (0.0037) 112.55 (0.20) H16A 0.9900 109.09 109.09 H16B 0.9900 109.09 109.09 107.83 C16 - C15 C17 H16A C17 - Distance Angles C18 1.5132 (0.0037) C16 1.5180 (0.0037) 114.65 (0.21) H17A 0.9900 108.60 108.60 H17B 0.9900 108.60 108.60 107.57 C17 - C18 C16 H17A C18 - Distance Angles C19 1.5083 (0.0043) C17 1.5132 (0.0037) 113.02 (0.24) H18A 0.9900 108.98 108.98 H18B 0.9900 108.98 108.98 107.77 C18 - C19 C17 H18A C19 - Distance Angles C18 1.5083 (0.0043) H19A 0.9800 109.47 H19B 0.9800 109.47 109.47 H19C 0.9800 109.47 109.47 109.47 C19 - C18 H19A H19B O1 - Distance Angles H51 0.8970 (0.0183) H52 0.9067 (0.0183) 104.02 (3.06) O1 - H51 FMAP and GRID set by program FMAP 2 3 35 GRID -1.563 -2 -2 1.563 2 2 R1 = 0.0540 for 4615 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.12 at 0.8627 0.8486 0.4818 [ 0.85 A from BR1 ] Deepest hole -0.71 at 0.8022 0.9263 0.3754 [ 0.74 A from BR1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 3001 / 23155 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1373 0.1514 0.5182 1.00000 0.05 1.12 0.85 BR1 1.51 H52 2.41 O1 2.48 H14B Q2 1 0.0355 0.2147 0.5748 1.00000 0.05 0.32 1.25 BR1 1.82 H7 2.00 H14A 2.26 H52 Q3 1 0.1232 0.0974 0.6123 1.00000 0.05 0.31 0.57 BR1 2.05 H51 2.43 H7 2.57 H52 Q4 1 0.2053 0.1199 0.5791 1.00000 0.05 0.30 0.35 BR1 2.54 H52 2.54 H6A 2.65 H51 Q5 1 0.1756 0.2587 0.5294 1.00000 0.05 0.28 1.19 BR1 2.03 H14B 2.27 H9 2.38 H14A Q6 1 0.6585 0.3741 0.3708 1.00000 0.05 0.28 0.71 C10 0.71 C11 1.49 H10 1.49 H11 Q7 1 0.2253 0.1123 0.6575 1.00000 0.05 0.28 1.28 BR1 2.27 H9 2.31 H6A 2.44 H5A Q8 1 0.1473 0.5185 0.2961 1.00000 0.05 0.26 0.75 C14 0.83 C15 1.34 H15B 1.41 H14B Q9 1 0.2604 0.2037 0.4870 1.00000 0.05 0.26 1.42 BR1 1.90 H12 2.22 H52 2.26 H14B Q10 1 0.1458 -0.0270 0.6575 1.00000 0.05 0.25 1.49 BR1 1.60 H51 1.97 H19B 2.11 H11 Shortest distances between peaks (including symmetry equivalents) 3 4 0.80 5 9 0.98 1 4 1.07 3 10 1.10 4 7 1.11 1 5 1.16 2 3 1.21 1 2 1.21 1 3 1.22 1 9 1.23 4 5 1.23 3 7 1.26 4 9 1.31 2 5 1.35 4 10 1.54 2 4 1.56 7 10 1.57 3 5 1.64 5 7 1.92 3 9 1.99 1 10 2.09 2 9 2.09 2 7 2.12 1 7 2.12 7 9 2.20 2 10 2.24 5 10 2.67 9 10 2.78 Time profile in seconds ----------------------- 0.03: 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. 0.77: 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 2.34: Structure factors and derivatives 4.16: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.38: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 14:28:39 Total CPU time: 7.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++