+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2010src0792ra started at 15:50:42 on 27-Mar-2011 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2010src0792ra in C2/c CELL 0.71073 19.6228 4.0710 32.9795 90.000 101.698 90.000 ZERR 8.00 0.0026 0.0005 0.0044 0.000 0.003 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O BR UNIT 120 96 8 16 8 V = 2579.83 F(000) = 1280.0 Mu = 3.18 mm-1 Cell Wt = 2545.33 Rho = 1.638 MERG 2 OMIT -3.00 55.00 OMIT 8 0 6 SHEL 7 0.77 DFIX 0.85 O1W H1W O1W H2WA O1W H2WB DANG 1.37 H1W H2WA H1W H2WB DFIX 1.88 O1W_$2 H2WA O1W_$3 H2WB EQIV $1 [ -x+1/2, -y-3/2, -z+1 ] EQIV $2 [ -x+1, -y-2, -z+1 ] EQIV $3 [ -x+1, -y-1, -z+1 ] HTAB N1 O1_$1 HTAB O1W O1 HTAB O1W O1W_$2 HTAB O1W O1W_$3 FMAP 2 PLAN 10 SIZE 0.02 0.04 0.10 ACTA BOND $H WGHT 0.00000 55.12160 L.S. 20 TEMP -153.00 FVAR 0.27080 MOLE 1 C1 1 0.277195 -0.505792 0.452239 11.00000 0.02924 0.02611 = 0.01842 -0.00584 0.00458 -0.00556 C2 1 0.278520 -0.324094 0.412937 11.00000 0.02444 0.02671 = 0.02055 -0.00511 0.00768 -0.00237 C3 1 0.209022 -0.194827 0.399078 11.00000 0.02277 0.02401 = 0.02148 -0.01316 0.00502 -0.00804 C4 1 0.175497 0.003638 0.365964 11.00000 0.03575 0.01752 = 0.02237 -0.00635 0.01146 -0.00296 AFIX 43 H4 2 0.200143 0.075408 0.345591 11.00000 -1.20000 AFIX 0 C5 1 0.106440 0.094344 0.363104 11.00000 0.03212 0.02452 = 0.02725 -0.00210 0.00830 0.00260 AFIX 43 H5 2 0.084301 0.228440 0.340700 11.00000 -1.20000 AFIX 0 C6 1 0.069058 -0.008126 0.392568 11.00000 0.02596 0.03182 = 0.02866 -0.00498 0.00579 -0.00153 AFIX 43 H6 2 0.021440 0.050587 0.389567 11.00000 -1.20000 AFIX 0 C7 1 0.101142 -0.195947 0.426344 11.00000 0.02879 0.03317 = 0.02311 -0.00199 0.00719 0.00316 AFIX 43 H7 2 0.076738 -0.259104 0.447208 11.00000 -1.20000 AFIX 0 C8 1 0.169892 -0.288046 0.428585 11.00000 0.02277 0.02152 = 0.01838 -0.00497 0.00057 -0.00278 C9 1 0.339469 -0.306717 0.399445 11.00000 0.03118 0.01790 = 0.02823 -0.00272 0.00982 0.00553 AFIX 43 H9 2 0.379609 -0.388412 0.417746 11.00000 -1.20000 AFIX 0 C10 1 0.350193 -0.174292 0.359312 11.00000 0.02747 0.02436 = 0.02240 -0.00048 0.00636 0.00942 C11 1 0.303762 -0.244447 0.322643 11.00000 0.02348 0.02403 = 0.03101 0.00217 0.01081 0.00338 AFIX 43 H11 2 0.262695 -0.365748 0.323437 11.00000 -1.20000 AFIX 0 C12 1 0.316591 -0.139424 0.284750 11.00000 0.02866 0.02314 = 0.02056 0.00064 0.00350 -0.00300 AFIX 43 H12 2 0.284814 -0.187402 0.259659 11.00000 -1.20000 AFIX 0 C13 1 0.377016 0.037258 0.284550 11.00000 0.03046 0.02570 = 0.02323 0.00190 0.01624 0.00091 C14 1 0.425218 0.106424 0.320546 11.00000 0.02881 0.02192 = 0.03404 -0.00152 0.01637 0.00038 AFIX 43 H14 2 0.466532 0.225325 0.319622 11.00000 -1.20000 AFIX 0 C15 1 0.411328 -0.003346 0.358058 11.00000 0.02258 0.03284 = 0.03050 -0.00206 0.00817 0.00708 AFIX 43 H15 2 0.443847 0.038694 0.383049 11.00000 -1.20000 AFIX 0 N1 3 0.211357 -0.474466 0.459695 11.00000 0.01853 0.03791 = 0.01898 -0.00399 0.00595 0.00076 AFIX 43 H1 2 0.197160 -0.559718 0.481065 11.00000 -1.20000 AFIX 0 O1 4 0.324879 -0.656307 0.474593 11.00000 0.02525 0.04319 = 0.02084 0.00215 0.00186 -0.00054 BR1 5 0.393937 0.188890 0.232791 11.00000 0.03660 0.03172 = 0.02747 0.00524 0.01353 0.00050 MOLE 2 O1W 4 0.467822 -0.746419 0.476896 11.00000 0.03140 0.22287 = 0.07068 0.04259 0.01721 0.01607 H1W 2 0.426181 -0.790316 0.478922 11.00000 -1.50000 PART 1 H2WA 2 0.493630 -0.886591 0.492037 10.50000 -1.50000 PART 2 H2WB 2 0.477238 -0.556827 0.487607 10.50000 -1.50000 HKLF 4 Covalent radii and connectivity table for 2010src0792ra in C2/c C 0.770 H 0.320 N 0.700 O 0.660 BR 1.140 C1 - O1 N1 C2 C2 - C9 C3 C1 C3 - C8 C4 C2 C4 - C5 C3 C5 - C4 C6 C6 - C7 C5 C7 - C8 C6 C8 - C7 N1 C3 C9 - C2 C10 C10 - C11 C15 C9 C11 - C10 C12 C12 - C13 C11 C13 - C12 C14 Br1 C14 - C13 C15 C15 - C14 C10 N1 - C1 C8 O1 - C1 Br1 - C13 O1W - no bonds found Operators for generating equivalent atoms: $1 -x+1/2, -y-3/2, -z+1 $2 -x+1, -y-2, -z+1 $3 -x+1, -y-1, -z+1 10009 Reflections read, of which 916 rejected -24 =< h =< 24, -4 =< k =< 5, -42 =< l =< 41, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 2888 Unique reflections, of which 0 suppressed R(int) = 0.0715 R(sigma) = 0.0842 Friedel opposites merged Maximum memory for data reduction = 1924 / 35521 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 = 2408 / 225832 wR2 = 0.1671 before cycle 1 for 2888 data and 181 / 181 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 5. 2. 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 0.003 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.124 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 55.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27080 0.00077 0.006 OSF Mean shift/su = 0.001 Maximum = -0.008 for z Br1 Max. shift = 0.001 A for H2WA_a Max. dU = 0.000 for C12 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1671 before cycle 2 for 2888 data and 181 / 181 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 5. 2. 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 0.003 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.124 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 55.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27080 0.00077 -0.001 OSF Mean shift/su = 0.000 Maximum = 0.005 for z H2WA_a Max. shift = 0.002 A for H2WA_a Max. dU = 0.000 for O1W Least-squares cycle 3 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1671 before cycle 3 for 2888 data and 181 / 181 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 5. 2. 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 0.003 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.124 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 55.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27080 0.00077 0.000 OSF Mean shift/su = 0.000 Maximum = -0.006 for z H2WA_a Max. shift = 0.002 A for H2WA_a Max. dU = 0.000 for O1W Least-squares cycle 4 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1671 before cycle 4 for 2888 data and 181 / 181 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 5. 2. 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 0.003 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.124 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 55.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27080 0.00077 0.000 OSF Mean shift/su = 0.000 Maximum = 0.006 for z H2WA_a Max. shift = 0.002 A for H2WA_a Max. dU = 0.000 for O1W Least-squares cycle 5 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1671 before cycle 5 for 2888 data and 181 / 181 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 5. 2. 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 0.003 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.124 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 55.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27080 0.00077 0.000 OSF Mean shift/su = 0.000 Maximum = -0.005 for z H2WA_a Max. shift = 0.002 A for H2WA_a Max. dU = 0.000 for O1W Least-squares cycle 6 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1671 before cycle 6 for 2888 data and 181 / 181 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 5. 2. 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 0.003 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.124 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 55.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27080 0.00077 0.000 OSF Mean shift/su = 0.000 Maximum = 0.005 for z H2WA_a Max. shift = 0.002 A for H2WA_a Max. dU = 0.000 for O1W Least-squares cycle 7 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1671 before cycle 7 for 2888 data and 181 / 181 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 5. 2. 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 0.003 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.124 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 55.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27080 0.00077 0.000 OSF Mean shift/su = 0.000 Maximum = -0.004 for z H2WA_a Max. shift = 0.002 A for H2WA_a Max. dU = 0.000 for O1W Least-squares cycle 8 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1671 before cycle 8 for 2888 data and 181 / 181 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 5. 2. 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 0.003 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.124 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 55.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27080 0.00077 0.000 OSF Mean shift/su = 0.000 Maximum = 0.004 for z H2WA_a Max. shift = 0.001 A for H2WA_a Max. dU = 0.000 for O1W Least-squares cycle 9 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1671 before cycle 9 for 2888 data and 181 / 181 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 5. 2. 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 0.003 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.124 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 55.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27080 0.00077 0.000 OSF Mean shift/su = 0.000 Maximum = -0.003 for z H2WA_a Max. shift = 0.001 A for H2WA_a Max. dU = 0.000 for O1W Least-squares cycle 10 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1671 before cycle 10 for 2888 data and 181 / 181 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 5. 2. 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 0.003 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.124 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 55.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27080 0.00077 0.000 OSF Mean shift/su = 0.000 Maximum = 0.003 for z H2WA_a Max. shift = 0.001 A for H2WA_a Max. dU = 0.000 for O1W Least-squares cycle 11 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1671 before cycle 11 for 2888 data and 181 / 181 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 5. 2. 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 0.003 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.124 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 55.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27080 0.00077 0.000 OSF Mean shift/su = 0.000 Maximum = -0.002 for z H2WA_a Max. shift = 0.001 A for H2WA_a Max. dU = 0.000 for O1W Least-squares cycle 12 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1671 before cycle 12 for 2888 data and 181 / 181 parameters Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 5. 2. 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 0.003 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.124 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 55.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27080 0.00077 0.000 OSF Mean shift/su = 0.000 Maximum = 0.002 for z H2WA_a Max. shift = 0.001 A for H2WA_a Max. dU = 0.000 for O1W Least-squares cycle 13 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1671 before cycle 13 for 2888 data and 181 / 181 parameters Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 5. 2. 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 0.003 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.124 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 55.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27080 0.00077 0.000 OSF Mean shift/su = 0.000 Maximum = -0.002 for z H2WA_a Max. shift = 0.001 A for H2WA_a Max. dU = 0.000 for O1W Least-squares cycle 14 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1671 before cycle 14 for 2888 data and 181 / 181 parameters Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 5. 2. 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 0.003 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.124 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 55.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27080 0.00077 0.000 OSF Mean shift/su = 0.000 Maximum = 0.002 for z H2WA_a Max. shift = 0.001 A for H2WA_a Max. dU = 0.000 for O1W Least-squares cycle 15 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1671 before cycle 15 for 2888 data and 181 / 181 parameters Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 5. 2. 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 0.003 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.124 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 55.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27080 0.00077 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for z H2WA_a Max. shift = 0.001 A for H2WA_a Max. dU = 0.000 for O1W Least-squares cycle 16 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1671 before cycle 16 for 2888 data and 181 / 181 parameters Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 5. 2. 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 0.003 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.124 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 55.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27080 0.00077 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for z H2WA_a Max. shift = 0.001 A for H2WA_a Max. dU = 0.000 for O1W Least-squares cycle 17 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1671 before cycle 17 for 2888 data and 181 / 181 parameters Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 5. 2. 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 0.003 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.124 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 55.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27080 0.00077 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for z H2WA_a Max. shift = 0.000 A for H2WA_a Max. dU = 0.000 for O1W Least-squares cycle 18 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1671 before cycle 18 for 2888 data and 181 / 181 parameters Summary of restraints applied in cycle 18 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 5. 2. 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 0.003 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.124 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 55.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27080 0.00077 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for z H2WA_a Max. shift = 0.000 A for H2WA_a Max. dU = 0.000 for O1W Least-squares cycle 19 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1671 before cycle 19 for 2888 data and 181 / 181 parameters Summary of restraints applied in cycle 19 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 5. 2. 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 0.003 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.124 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 55.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27080 0.00077 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for z H2WA_a Max. shift = 0.000 A for H2WA_a Max. dU = 0.000 for O1W Least-squares cycle 20 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1671 before cycle 20 for 2888 data and 181 / 181 parameters Summary of restraints applied in cycle 20 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 5. 2. 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 0.003 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.124 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 55.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.27080 0.00077 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for z H2WA_a Max. shift = 0.000 A for H2WA_a Max. dU = 0.000 for O1W Largest correlation matrix elements 0.968 z H2WA_a / y H2WA_a -0.724 z H2WB_b / y H1W -0.566 y H2WA_a / y O1W -0.818 z H2WB_b / y H2WB_b -0.708 z H2WB_b / x H2WB_b -0.548 z H2WA_a / x H1W 0.808 x H2WA_a / x H1W 0.703 z H1W / x H1W -0.532 z H2WA_a / y O1W 0.794 x H2WB_b / y H1W -0.582 x H2WA_a / y H1W Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H4 0.2001 0.0754 0.3456 43 0.950 0.000 C4 C5 C3 H5 0.0843 0.2284 0.3407 43 0.950 0.000 C5 C4 C6 H6 0.0214 0.0506 0.3896 43 0.950 0.000 C6 C7 C5 H7 0.0767 -0.2591 0.4472 43 0.950 0.000 C7 C8 C6 H9 0.3796 -0.3884 0.4177 43 0.950 0.000 C9 C2 C10 H11 0.2627 -0.3657 0.3234 43 0.950 0.000 C11 C10 C12 H12 0.2848 -0.1874 0.2597 43 0.950 0.000 C12 C13 C11 H14 0.4665 0.2253 0.3196 43 0.950 0.000 C14 C13 C15 H15 0.4438 0.0387 0.3830 43 0.950 0.000 C15 C14 C10 H1 0.1972 -0.5597 0.4811 43 0.880 0.000 N1 C1 C8 2010src0792ra in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.27720 -0.50579 0.45224 1.00000 0.02924 0.02611 0.01842 -0.00584 0.00458 -0.00556 0.02462 0.01256 0.00038 0.00178 0.00019 0.00000 0.00393 0.00408 0.00296 0.00282 0.00282 0.00327 0.00154 C2 0.27852 -0.32409 0.41294 1.00000 0.02444 0.02671 0.02055 -0.00511 0.00768 -0.00237 0.02346 0.01250 0.00035 0.00185 0.00018 0.00000 0.00353 0.00372 0.00290 0.00292 0.00263 0.00327 0.00143 C3 0.20902 -0.19483 0.39908 1.00000 0.02277 0.02400 0.02148 -0.01316 0.00502 -0.00804 0.02268 0.01157 0.00034 0.00179 0.00018 0.00000 0.00341 0.00354 0.00286 0.00291 0.00256 0.00318 0.00140 C4 0.17550 0.00364 0.36596 1.00000 0.03575 0.01752 0.02237 -0.00635 0.01146 -0.00296 0.02443 0.01262 0.00038 0.00166 0.00020 0.00000 0.00426 0.00368 0.00308 0.00271 0.00298 0.00312 0.00155 H4 0.20014 0.07541 0.34559 1.00000 0.02931 0.00000 0.00000 C5 0.10644 0.09434 0.36310 1.00000 0.03212 0.02452 0.02725 -0.00210 0.00830 0.00260 0.02764 0.01353 0.00038 0.00180 0.00021 0.00000 0.00413 0.00400 0.00337 0.00291 0.00308 0.00322 0.00162 H5 0.08430 0.22844 0.34070 1.00000 0.03317 0.00000 0.00000 C6 0.06906 -0.00813 0.39257 1.00000 0.02596 0.03182 0.02866 -0.00498 0.00579 -0.00153 0.02878 0.01330 0.00039 0.00185 0.00020 0.00000 0.00389 0.00444 0.00349 0.00317 0.00301 0.00339 0.00165 H6 0.02144 0.05059 0.38957 1.00000 0.03453 0.00000 0.00000 C7 0.10114 -0.19595 0.42634 1.00000 0.02879 0.03317 0.02311 -0.00199 0.00719 0.00316 0.02808 0.01345 0.00037 0.00194 0.00019 0.00000 0.00383 0.00404 0.00306 0.00313 0.00282 0.00356 0.00155 H7 0.07674 -0.25910 0.44721 1.00000 0.03370 0.00000 0.00000 C8 0.16989 -0.28805 0.42859 1.00000 0.02277 0.02152 0.01838 -0.00497 0.00057 -0.00278 0.02140 0.01179 0.00034 0.00172 0.00018 0.00000 0.00344 0.00355 0.00272 0.00271 0.00246 0.00300 0.00139 C9 0.33947 -0.30672 0.39945 1.00000 0.03118 0.01790 0.02823 -0.00272 0.00982 0.00553 0.02523 0.01329 0.00037 0.00177 0.00020 0.00000 0.00391 0.00332 0.00320 0.00298 0.00292 0.00329 0.00147 H9 0.37961 -0.38841 0.41775 1.00000 0.03028 0.00000 0.00000 C10 0.35019 -0.17429 0.35931 1.00000 0.02747 0.02436 0.02240 -0.00048 0.00636 0.00942 0.02456 0.01332 0.00036 0.00183 0.00019 0.00000 0.00368 0.00366 0.00299 0.00296 0.00272 0.00334 0.00146 C11 0.30376 -0.24445 0.32264 1.00000 0.02348 0.02403 0.03101 0.00217 0.01081 0.00338 0.02543 0.01338 0.00036 0.00171 0.00020 0.00000 0.00359 0.00432 0.00332 0.00288 0.00287 0.00297 0.00159 H11 0.26269 -0.36575 0.32344 1.00000 0.03051 0.00000 0.00000 C12 0.31659 -0.13942 0.28475 1.00000 0.02866 0.02314 0.02056 0.00064 0.00350 -0.00300 0.02433 0.01282 0.00037 0.00169 0.00019 0.00000 0.00378 0.00406 0.00297 0.00276 0.00273 0.00317 0.00152 H12 0.28481 -0.18740 0.25966 1.00000 0.02919 0.00000 0.00000 C13 0.37702 0.03726 0.28455 1.00000 0.03046 0.02570 0.02323 0.00190 0.01624 0.00091 0.02494 0.01370 0.00038 0.00177 0.00020 0.00000 0.00394 0.00388 0.00316 0.00289 0.00295 0.00322 0.00154 C14 0.42522 0.10642 0.32055 1.00000 0.02881 0.02192 0.03404 -0.00152 0.01637 0.00038 0.02685 0.01404 0.00038 0.00174 0.00021 0.00000 0.00397 0.00398 0.00354 0.00295 0.00313 0.00305 0.00162 H14 0.46653 0.22532 0.31962 1.00000 0.03221 0.00000 0.00000 C15 0.41133 -0.00335 0.35806 1.00000 0.02258 0.03284 0.03050 -0.00206 0.00817 0.00708 0.02825 0.01414 0.00037 0.00186 0.00021 0.00000 0.00384 0.00446 0.00349 0.00318 0.00299 0.00333 0.00165 H15 0.44385 0.03869 0.38305 1.00000 0.03390 0.00000 0.00000 N1 0.21136 -0.47447 0.45969 1.00000 0.01853 0.03791 0.01898 -0.00399 0.00595 0.00076 0.02484 0.01049 0.00029 0.00153 0.00016 0.00000 0.00293 0.00373 0.00254 0.00251 0.00224 0.00270 0.00132 H1 0.19716 -0.55972 0.48107 1.00000 0.02980 0.00000 0.00000 O1 0.32488 -0.65631 0.47459 1.00000 0.02525 0.04319 0.02084 0.00215 0.00186 -0.00054 0.03015 0.00909 0.00025 0.00134 0.00013 0.00000 0.00267 0.00328 0.00216 0.00230 0.00198 0.00258 0.00117 Br1 0.39394 0.18889 0.23279 1.00000 0.03660 0.03172 0.02747 0.00524 0.01353 0.00050 0.03094 0.00148 0.00004 0.00019 0.00002 0.00000 0.00043 0.00041 0.00034 0.00034 0.00028 0.00038 0.00023 O1W 0.46782 -0.74642 0.47690 1.00000 0.03140 0.22287 0.07069 0.04259 0.01721 0.01607 0.10735 0.02182 0.00037 0.00336 0.00025 0.00000 0.00387 0.01223 0.00496 0.00655 0.00387 0.00585 0.00383 H1W 0.42618 -0.79033 0.47892 1.00000 0.16103 0.25522 0.00267 0.03536 0.00494 0.00000 0.00000 H2WA_a 0.49363 -0.88662 0.49203 0.50000 0.16103 0.52066 0.00508 0.05004 0.01052 0.00000 0.00000 H2WB_b 0.47724 -0.55683 0.48761 0.50000 0.16103 0.06525 0.00681 0.01654 0.00504 0.00000 0.00000 Final Structure Factor Calculation for 2010src0792ra in C2/c Total number of l.s. parameters = 181 Maximum vector length = 511 Memory required = 2227 / 24017 wR2 = 0.1671 before cycle 21 for 2888 data and 0 / 181 parameters Summary of restraints applied in cycle 21 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 5. 2. 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 0.003 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.124 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 55.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0785 for 2064 Fo > 4sig(Fo) and 0.1198 for all 2888 data wR2 = 0.1671, GooF = S = 1.125, Restrained GooF = 1.124 for all data Occupancy sum of asymmetric unit = 19.00 for non-hydrogen and 12.00 for hydrogen atoms Principal mean square atomic displacements U 0.0337 0.0250 0.0151 C1 0.0308 0.0230 0.0166 C2 0.0374 0.0219 0.0087 C3 0.0378 0.0227 0.0128 C4 0.0331 0.0282 0.0216 C5 0.0355 0.0260 0.0249 C6 0.0351 0.0281 0.0211 C7 0.0258 0.0249 0.0135 C8 0.0339 0.0279 0.0140 C9 0.0355 0.0227 0.0155 C10 0.0339 0.0238 0.0186 C11 0.0307 0.0219 0.0204 C12 0.0367 0.0255 0.0126 C13 0.0401 0.0224 0.0180 C14 0.0368 0.0309 0.0170 C15 0.0388 0.0203 0.0154 N1 0.0435 0.0272 0.0198 O1 0.0401 0.0327 0.0200 Br1 0.2343 0.0596 0.0282 O1W may be split into 0.4693 -0.6968 0.4784 and 0.4663 -0.7960 0.4753 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.018 0.035 0.052 0.069 0.091 0.117 0.145 0.187 0.259 1.000 Number in group 297. 293. 291. 276. 286. 293. 286. 293. 282. 291. GooF 1.164 1.184 1.141 1.270 1.121 1.181 1.102 1.078 0.898 1.074 K 5.867 1.645 1.213 1.172 1.045 1.019 1.005 0.999 1.014 1.010 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.31 1.67 inf Number in group 291. 291. 289. 287. 288. 291. 287. 286. 291. 287. GooF 1.226 1.153 1.150 1.266 1.258 1.121 1.147 1.068 0.908 0.885 K 1.105 1.067 1.062 1.042 1.030 1.039 1.010 1.023 0.994 1.011 R1 0.326 0.244 0.206 0.198 0.159 0.118 0.098 0.065 0.044 0.031 Recommended weighting scheme: WGHT 0.0000 55.1288 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) -12 2 15 7927.01 13235.28 4.72 0.318 1.17 12 0 2 2976.49 6234.77 4.63 0.218 1.56 13 3 10 1116.25 3538.96 4.37 0.164 0.92 -22 2 19 -57.27 1310.38 3.95 0.100 0.78 -14 0 24 8364.52 12795.39 3.90 0.312 1.08 -21 1 19 1674.78 4283.83 3.87 0.181 0.86 7 1 13 8737.91 13363.68 3.82 0.319 1.55 -15 1 25 1296.96 3064.53 3.64 0.153 0.99 10 2 6 2108.42 4125.55 3.62 0.177 1.31 -14 0 20 6641.32 11671.08 3.57 0.298 1.17 9 3 4 7800.66 12759.38 3.12 0.312 1.12 13 3 13 -252.40 648.15 3.11 0.070 0.89 -14 2 30 5471.49 3419.64 3.09 0.161 0.86 17 1 15 484.08 1803.22 3.07 0.117 0.90 -7 3 3 1235.05 417.97 3.06 0.056 1.22 15 1 14 -90.78 516.70 3.04 0.063 1.00 -3 3 33 940.22 5.22 3.04 0.006 0.80 -21 1 3 1534.79 514.54 2.96 0.063 0.90 0 4 20 1361.39 270.37 2.87 0.045 0.86 19 3 5 1538.15 64.85 2.86 0.022 0.79 -16 2 23 1233.71 410.61 2.81 0.056 0.91 -7 5 3 1651.33 88.14 2.81 0.026 0.78 -16 0 20 10503.06 13799.32 2.74 0.324 1.07 18 2 4 1853.96 622.29 2.73 0.069 0.92 -22 0 26 480.57 1566.38 2.70 0.109 0.79 1 3 31 2114.33 931.45 2.69 0.084 0.82 -16 0 32 8027.62 5543.21 2.68 0.206 0.86 -16 0 18 28785.08 35178.69 2.67 0.518 1.11 -10 4 21 1432.24 386.07 2.65 0.054 0.81 3 3 30 1021.77 77.51 2.62 0.024 0.82 9 3 17 33.73 601.29 2.57 0.068 0.94 20 2 6 1064.71 37.10 2.56 0.017 0.83 13 1 24 1236.27 432.21 2.54 0.057 0.89 13 3 14 -41.74 616.23 2.54 0.069 0.87 20 0 0 1507.88 241.39 2.53 0.043 0.96 -3 3 17 1392.25 605.38 2.51 0.068 1.11 19 1 11 1676.77 671.75 2.49 0.072 0.88 12 4 9 5070.58 3261.03 2.49 0.158 0.82 6 2 25 11.07 536.89 2.48 0.064 0.98 4 2 28 245.89 944.74 2.48 0.085 0.95 -10 4 18 877.97 12.44 2.47 0.010 0.84 -1 1 35 3113.90 1915.41 2.47 0.121 0.91 7 1 34 608.62 3.24 2.47 0.005 0.83 -10 2 31 1651.65 2755.37 2.47 0.145 0.90 17 1 12 -238.63 612.49 2.47 0.068 0.95 5 5 6 207.62 1163.50 2.46 0.094 0.78 11 1 12 647.64 12.10 2.44 0.010 1.28 -13 1 32 955.42 274.85 2.43 0.046 0.90 12 4 0 538.21 15.68 2.43 0.011 0.86 -8 4 11 310.63 1029.69 2.42 0.089 0.91 Bond lengths and angles C1 - Distance Angles O1 1.2308 (0.0084) N1 1.3692 (0.0086) 124.70 (0.61) C2 1.4972 (0.0090) 128.32 (0.63) 106.98 (0.60) C1 - O1 N1 C2 - Distance Angles C9 1.3598 (0.0090) C3 1.4467 (0.0095) 135.48 (0.65) C1 1.4972 (0.0090) 118.67 (0.65) 105.81 (0.54) C2 - C9 C3 C3 - Distance Angles C8 1.4084 (0.0086) C4 1.4096 (0.0097) 117.10 (0.61) C2 1.4467 (0.0096) 107.14 (0.57) 135.67 (0.60) C3 - C8 C4 C4 - Distance Angles C5 1.3891 (0.0098) C3 1.4096 (0.0097) 120.04 (0.61) H4 0.9500 119.98 119.98 C4 - C5 C3 C5 - Distance Angles C4 1.3891 (0.0098) C6 1.3948 (0.0093) 121.12 (0.67) H5 0.9500 119.44 119.44 C5 - C4 C6 C6 - Distance Angles C7 1.3919 (0.0099) C5 1.3948 (0.0093) 120.36 (0.69) H6 0.9500 119.82 119.82 C6 - C7 C5 C7 - Distance Angles C8 1.3877 (0.0093) C6 1.3919 (0.0099) 117.91 (0.62) H7 0.9500 121.04 121.04 C7 - C8 C6 C8 - Distance Angles C7 1.3877 (0.0093) N1 1.3972 (0.0085) 126.94 (0.58) C3 1.4084 (0.0086) 123.42 (0.62) 109.62 (0.57) C8 - C7 N1 C9 - Distance Angles C2 1.3598 (0.0090) C10 1.4831 (0.0088) 127.17 (0.66) H9 0.9500 116.41 116.41 C9 - C2 C10 C10 - Distance Angles C11 1.3883 (0.0094) C15 1.3947 (0.0100) 119.56 (0.60) C9 1.4831 (0.0088) 121.05 (0.66) 119.10 (0.62) C10 - C11 C15 C11 - Distance Angles C10 1.3883 (0.0094) C12 1.3912 (0.0086) 120.86 (0.65) H11 0.9500 119.57 119.57 C11 - C10 C12 C12 - Distance Angles C13 1.3880 (0.0097) C11 1.3912 (0.0086) 118.29 (0.63) H12 0.9500 120.86 120.86 C12 - C13 C11 C13 - Distance Angles C12 1.3880 (0.0097) C14 1.3885 (0.0099) 122.38 (0.59) Br1 1.9066 (0.0061) 118.43 (0.51) 119.19 (0.51) C13 - C12 C14 C14 - Distance Angles C13 1.3885 (0.0099) C15 1.3933 (0.0092) 118.17 (0.66) H14 0.9500 120.91 120.91 C14 - C13 C15 C15 - Distance Angles C14 1.3933 (0.0092) C10 1.3947 (0.0100) 120.71 (0.67) H15 0.9500 119.65 119.65 C15 - C14 C10 N1 - Distance Angles C1 1.3692 (0.0086) C8 1.3972 (0.0085) 110.42 (0.54) H1 0.8800 124.79 124.79 N1 - C1 C8 O1 - Distance Angles C1 1.2308 (0.0084) O1 - Br1 - Distance Angles C13 1.9066 (0.0061) Br1 - O1W - Distance Angles H1W 0.8522 (0.0206) H2WA_a 0.8537 (0.0194) 106.17 (4.96) H2WB_b 0.8533 (0.0208) 106.73 (5.24) 108.04 (9.99) O1W - H1W H2WA_a Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.88 1.98 2.844(7) 166.9 N1-H1...O1_$1 0.85(2) 2.04(7) 2.815(9) 151(13) O1W-H1W...O1 0.854(19) 1.88(2) 2.720(19) 167(12) O1W-H2WA_a...O1W_$2 0.85(2) 1.88(2) 2.68(3) 154(8) O1W-H2WB_b...O1W_$3 FMAP and GRID set by program FMAP 2 3 39 GRID -0.694 -1 -2 0.694 1 2 R1 = 0.1158 for 2888 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.65 at 0.3974 0.4633 0.2306 [ 1.12 A from BR1 ] Deepest hole -0.81 at 0.3605 0.2001 0.2461 [ 0.86 A from BR1 ] Mean = 0.00, Rms deviation from mean = 0.16 e/A^3, Highest memory used = 2225 / 16713 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3974 0.4633 0.2306 1.00000 0.05 0.65 1.12 BR1 2.57 C13 2.68 H5 2.87 H4 Q2 1 0.2783 0.1710 0.3400 1.00000 0.05 0.63 1.63 H4 1.88 C11 1.97 H11 2.00 C10 Q3 1 0.1307 0.1003 0.3220 1.00000 0.05 0.58 1.31 H5 1.43 H4 1.53 C5 1.58 C4 Q4 1 0.3977 0.1013 0.2627 1.00000 0.05 0.58 0.93 C13 1.04 BR1 1.87 C14 2.12 C12 Q5 1 0.1821 -0.1252 0.4115 1.00000 0.05 0.57 0.78 C3 0.93 C8 1.57 C4 1.78 C7 Q6 1 0.2286 -0.1870 0.4639 1.00000 0.05 0.55 1.22 N1 1.52 C8 1.70 C1 1.77 H1 Q7 1 0.2064 -0.4745 0.3370 1.00000 0.05 0.55 1.35 H11 1.86 H4 2.26 C11 2.30 C4 Q8 1 0.3195 -0.6560 0.3536 1.00000 0.05 0.54 1.78 H11 1.95 C11 2.05 C10 2.05 C9 Q9 1 0.2085 -0.0323 0.3886 1.00000 0.05 0.54 0.75 C3 0.90 C4 1.46 H4 1.87 C2 Q10 1 0.1576 0.1968 0.2913 1.00000 0.05 0.53 1.88 H4 2.26 H12 2.31 BR1 2.39 H5 Shortest distances between peaks (including symmetry equivalents) 5 9 1.07 2 8 1.10 3 10 1.29 1 10 1.51 1 3 1.80 5 6 1.80 1 4 1.81 2 7 2.01 7 10 2.10 3 7 2.27 7 8 2.30 6 6 2.42 2 9 2.45 3 9 2.47 7 9 2.47 4 10 2.51 6 9 2.51 2 10 2.58 2 3 2.85 5 7 2.96 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.02: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.55: 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 1.23: Structure factors and derivatives 1.95: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.20: Apply other restraints 0.38: Solve l.s. equations 0.00: Generate HTAB table 0.16: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010src0792ra finished at 15:50:47 Total CPU time: 4.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++