+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2010src0795a started at 21:21:19 on 27-Mar-2011 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2010src0795a CELL 0.71073 19.6553 4.0406 32.6526 90.000 101.378 90.000 ZERR 8.00 0.0012 0.0002 0.0020 0.000 0.002 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O CL UNIT 120 96 8 16 8 V = 2542.28 F(000) = 1136.0 Mu = 0.30 mm-1 Cell Wt = 2189.65 Rho = 1.430 MERG 2 OMIT -3.00 55.00 OMIT 0 2 11 SHEL 7 0.77 DFIX 0.85 O1W H1W O1W H2WA O1W H2WB DANG 1.37 H1W H2WA H1W H2WB DFIX 1.90 O1W_$2 H2WA O1W_$3 H2WB EQIV $1 [ -x+1/2, -y+5/2, -z+1 ] EQIV $2 [ -x+1, -y+3, -z+1 ] EQIV $3 [ -x+1, -y+2, -z+1 ] HTAB N1 O1_$1 HTAB O1W O1 HTAB O1W O1W_$2 HTAB O1W O1W_$3 FMAP 2 PLAN 5 SIZE 0.08 0.14 0.16 ACTA BOND $H WGHT 0.06200 2.15010 L.S. 20 TEMP -153.00 FVAR 0.12222 MOLE 1 CL1 5 0.396320 0.333327 0.233887 11.00000 0.04335 0.03676 = 0.02557 -0.00529 0.01543 0.00028 O1 4 0.324760 1.158081 0.473980 11.00000 0.02746 0.04211 = 0.01904 -0.00399 0.00609 -0.00278 N1 3 0.211695 0.975118 0.459001 11.00000 0.02562 0.03429 = 0.01626 0.00051 0.00751 0.00171 AFIX 43 H1 2 0.197686 1.059782 0.480752 11.00000 -1.20000 AFIX 0 C1 1 0.277052 1.005873 0.451597 11.00000 0.02784 0.02948 = 0.01742 0.00441 0.00659 0.00201 C2 1 0.278279 0.827699 0.411338 11.00000 0.02669 0.02487 = 0.01715 0.00441 0.00498 0.00163 C3 1 0.207648 0.694770 0.397175 11.00000 0.02723 0.02141 = 0.01813 0.00519 0.00628 0.00195 C4 1 0.175164 0.503364 0.363531 11.00000 0.03055 0.02344 = 0.02401 0.00338 0.01003 0.00159 AFIX 43 H4 2 0.199839 0.434271 0.342769 11.00000 -1.20000 AFIX 0 C5 1 0.105819 0.414414 0.360740 11.00000 0.03392 0.02414 = 0.02541 0.00048 0.00501 -0.00224 AFIX 43 H5 2 0.082991 0.286207 0.337700 11.00000 -1.20000 AFIX 0 C6 1 0.069738 0.511630 0.391377 11.00000 0.02514 0.02762 = 0.03090 0.00691 0.00716 -0.00079 AFIX 43 H6 2 0.022561 0.447981 0.388834 11.00000 -1.20000 AFIX 0 C7 1 0.100997 0.699311 0.425557 11.00000 0.02712 0.02900 = 0.02255 0.00638 0.00788 0.00304 AFIX 43 H7 2 0.076525 0.762102 0.446683 11.00000 -1.20000 AFIX 0 C8 1 0.169521 0.790975 0.427477 11.00000 0.02824 0.02376 = 0.01746 0.00606 0.00670 0.00353 C9 1 0.338492 0.809823 0.397550 11.00000 0.02673 0.02543 = 0.01983 0.00244 0.00499 -0.00069 AFIX 43 H9 2 0.378318 0.891319 0.416151 11.00000 -1.20000 AFIX 0 C10 1 0.350575 0.680457 0.357420 11.00000 0.02546 0.02114 = 0.02173 0.00134 0.00799 -0.00260 C11 1 0.304734 0.749994 0.319663 11.00000 0.02597 0.02227 = 0.02475 0.00136 0.00849 -0.00002 AFIX 43 H11 2 0.263197 0.869123 0.320052 11.00000 -1.20000 AFIX 0 C12 1 0.319329 0.647087 0.281885 11.00000 0.03016 0.02435 = 0.02156 0.00128 0.00624 -0.00231 AFIX 43 H12 2 0.288201 0.696034 0.256455 11.00000 -1.20000 AFIX 0 C13 1 0.379934 0.471616 0.281562 11.00000 0.03197 0.02264 = 0.02425 -0.00251 0.01304 -0.00381 C14 1 0.426563 0.399472 0.318328 11.00000 0.02700 0.02435 = 0.03065 -0.00063 0.01047 -0.00123 AFIX 43 H14 2 0.467714 0.277822 0.317723 11.00000 -1.20000 AFIX 0 C15 1 0.411869 0.508449 0.355903 11.00000 0.02452 0.02400 = 0.02394 0.00015 0.00566 -0.00249 AFIX 43 H15 2 0.444034 0.465552 0.381124 11.00000 -1.20000 AFIX 0 MOLE 2 O1W 4 0.467302 1.249592 0.476128 11.00000 0.03772 0.22331 = 0.07314 -0.04418 0.02366 -0.02918 H1W 2 0.423504 1.231866 0.478031 11.00000 -1.50000 PART 1 H2WA 2 0.484710 1.378475 0.496402 10.50000 -1.50000 PART 2 H2WB 2 0.487006 1.069295 0.484930 10.50000 -1.50000 HKLF 4 Covalent radii and connectivity table for 2010src0795a C 0.770 H 0.320 N 0.700 O 0.660 CL 0.990 Cl1 - C13 O1 - C1 N1 - C1 C8 C1 - O1 N1 C2 C2 - C9 C3 C1 C3 - C4 C8 C2 C4 - C3 C5 C5 - C6 C4 C6 - C7 C5 C7 - C8 C6 C8 - C7 N1 C3 C9 - C2 C10 C10 - C15 C11 C9 C11 - C12 C10 C12 - C11 C13 C13 - C12 C14 Cl1 C14 - C15 C13 C15 - C14 C10 O1W - no bonds found Operators for generating equivalent atoms: $1 -x+1/2, -y+5/2, -z+1 $2 -x+1, -y+3, -z+1 $3 -x+1, -y+2, -z+1 14498 Reflections read, of which 1281 rejected -25 =< h =< 25, -5 =< k =< 5, -42 =< l =< 42, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 2890 Unique reflections, of which 0 suppressed R(int) = 0.0578 R(sigma) = 0.0522 Friedel opposites merged Maximum memory for data reduction = 1924 / 35744 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 = 0.1320 before cycle 1 for 2890 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 0.014 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.066 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0620 * P )^2 + 2.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.12221 0.00032 -0.017 OSF Mean shift/su = 0.004 Maximum = 0.020 for z Cl1 Max. shift = 0.001 A for H2WB_b Max. dU = 0.000 for O1W Least-squares cycle 2 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1320 before cycle 2 for 2890 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 0.014 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.066 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0620 * P )^2 + 2.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.12222 0.00032 0.001 OSF Mean shift/su = 0.001 Maximum = 0.007 for z Cl1 Max. shift = 0.000 A for H2WB_b Max. dU = 0.000 for O1W Least-squares cycle 3 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1320 before cycle 3 for 2890 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 0.014 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.066 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0620 * P )^2 + 2.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.12222 0.00032 0.000 OSF Mean shift/su = 0.000 Maximum = -0.002 for x H2WB_b Max. shift = 0.000 A for H2WB_b Max. dU = 0.000 for O1W Least-squares cycle 4 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1320 before cycle 4 for 2890 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 0.014 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.066 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0620 * P )^2 + 2.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.12222 0.00032 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for x H2WB_b Max. shift = 0.000 A for H2WB_b Max. dU = 0.000 for O1W Least-squares cycle 5 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1320 before cycle 5 for 2890 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 0.014 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.066 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0620 * P )^2 + 2.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.12222 0.00032 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for x H2WB_b Max. shift = 0.000 A for H2WB_b Max. dU = 0.000 for O1W Least-squares cycle 6 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1320 before cycle 6 for 2890 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 0.014 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.066 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0620 * P )^2 + 2.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.12222 0.00032 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x Cl1 Max. shift = 0.000 A for H2WB_b Max. dU = 0.000 for O1W Least-squares cycle 7 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1320 before cycle 7 for 2890 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 0.014 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.066 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0620 * P )^2 + 2.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.12222 0.00032 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for x Cl1 Max. shift = 0.000 A for H2WB_b Max. dU = 0.000 for C6 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1320 before cycle 8 for 2890 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 0.014 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.066 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0620 * P )^2 + 2.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.12222 0.00032 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for x Cl1 Max. shift = 0.000 A for H2WB_b Max. dU = 0.000 for O1W Least-squares cycle 9 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1320 before cycle 9 for 2890 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 0.014 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.066 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0620 * P )^2 + 2.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.12222 0.00032 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for x Cl1 Max. shift = 0.000 A for H2WB_b Max. dU = 0.000 for C7 Least-squares cycle 10 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1320 before cycle 10 for 2890 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 0.014 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.066 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0620 * P )^2 + 2.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.12222 0.00032 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for x Cl1 Max. shift = 0.000 A for H2WB_b Max. dU = 0.000 for C15 Least-squares cycle 11 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1320 before cycle 11 for 2890 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 0.014 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.066 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0620 * P )^2 + 2.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.12222 0.00032 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for x Cl1 Max. shift = 0.000 A for H1W Max. dU = 0.000 for O1W Least-squares cycle 12 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1320 before cycle 12 for 2890 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 0.014 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.066 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0620 * P )^2 + 2.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.12222 0.00032 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for x Cl1 Max. shift = 0.000 A for H1W Max. dU = 0.000 for O1W Least-squares cycle 13 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1320 before cycle 13 for 2890 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 0.014 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.066 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0620 * P )^2 + 2.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.12222 0.00032 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for x Cl1 Max. shift = 0.000 A for H2WA_a Max. dU = 0.000 for O1W Least-squares cycle 14 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1320 before cycle 14 for 2890 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 0.014 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.066 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0620 * P )^2 + 2.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.12222 0.00032 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for x Cl1 Max. shift = 0.000 A for H1W Max. dU = 0.000 for O1W Least-squares cycle 15 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1320 before cycle 15 for 2890 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 0.014 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.066 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0620 * P )^2 + 2.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.12222 0.00032 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for x Cl1 Max. shift = 0.000 A for H2WA_a Max. dU = 0.000 for O1W Least-squares cycle 16 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1320 before cycle 16 for 2890 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 0.014 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.066 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0620 * P )^2 + 2.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.12222 0.00032 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for x Cl1 Max. shift = 0.000 A for H1W Max. dU = 0.000 for O1W Least-squares cycle 17 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1320 before cycle 17 for 2890 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 0.014 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.066 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0620 * P )^2 + 2.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.12222 0.00032 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for x Cl1 Max. shift = 0.000 A for H2WA_a Max. dU = 0.000 for C10 Least-squares cycle 18 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1320 before cycle 18 for 2890 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 0.014 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.066 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0620 * P )^2 + 2.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.12222 0.00032 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for x Cl1 Max. shift = 0.000 A for H1W Max. dU = 0.000 for C9 Least-squares cycle 19 Maximum vector length = 511 Memory required = 2408 / 225832 wR2 = 0.1320 before cycle 19 for 2890 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 0.014 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.066 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0620 * P )^2 + 2.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.12222 0.00032 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for x Cl1 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 = 0.1320 before cycle 20 for 2890 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 0.014 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.066 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0620 * P )^2 + 2.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.12222 0.00032 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for x Cl1 Max. shift = 0.000 A for H1W Max. dU = 0.000 for O1W Largest correlation matrix elements 0.779 y H2WB_b / x H2WB_b -0.724 y H2WA_a / x H2WA_a -0.575 x H2WB_b / y H1W -0.731 z H2WA_a / y H2WA_a 0.639 z H2WB_b / y H2WB_b 0.564 z H1W / x H1W Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.1977 1.0598 0.4808 43 0.880 0.000 N1 C1 C8 H4 0.1998 0.4343 0.3428 43 0.950 0.000 C4 C3 C5 H5 0.0830 0.2862 0.3377 43 0.950 0.000 C5 C6 C4 H6 0.0226 0.4480 0.3888 43 0.950 0.000 C6 C7 C5 H7 0.0765 0.7621 0.4467 43 0.950 0.000 C7 C8 C6 H9 0.3783 0.8913 0.4162 43 0.950 0.000 C9 C2 C10 H11 0.2632 0.8691 0.3201 43 0.950 0.000 C11 C12 C10 H12 0.2882 0.6960 0.2565 43 0.950 0.000 C12 C11 C13 H14 0.4677 0.2778 0.3177 43 0.950 0.000 C14 C15 C13 H15 0.4440 0.4655 0.3811 43 0.950 0.000 C15 C14 C10 2010src0795a ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Cl1 0.39632 0.33333 0.23389 1.00000 0.04335 0.03676 0.02557 -0.00529 0.01543 0.00028 0.03404 0.00103 0.00003 0.00014 0.00002 0.00000 0.00033 0.00034 0.00027 0.00021 0.00023 0.00024 0.00018 O1 0.32476 1.15808 0.47398 1.00000 0.02746 0.04212 0.01904 -0.00399 0.00610 -0.00278 0.02933 0.00264 0.00007 0.00038 0.00004 0.00000 0.00075 0.00095 0.00067 0.00063 0.00059 0.00066 0.00036 N1 0.21169 0.97512 0.45900 1.00000 0.02562 0.03429 0.01626 0.00051 0.00751 0.00171 0.02493 0.00312 0.00008 0.00043 0.00005 0.00000 0.00085 0.00099 0.00077 0.00067 0.00067 0.00072 0.00038 H1 0.19768 1.05978 0.48075 1.00000 0.02992 0.00000 0.00000 C1 0.27705 1.00588 0.45160 1.00000 0.02783 0.02950 0.01742 0.00441 0.00660 0.00201 0.02462 0.00391 0.00010 0.00051 0.00006 0.00000 0.00102 0.00109 0.00089 0.00079 0.00080 0.00084 0.00043 C2 0.27828 0.82770 0.41134 1.00000 0.02669 0.02487 0.01715 0.00441 0.00497 0.00163 0.02282 0.00368 0.00010 0.00049 0.00006 0.00000 0.00098 0.00104 0.00087 0.00075 0.00076 0.00080 0.00042 C3 0.20765 0.69477 0.39717 1.00000 0.02724 0.02142 0.01812 0.00519 0.00628 0.00195 0.02201 0.00369 0.00010 0.00048 0.00006 0.00000 0.00099 0.00099 0.00087 0.00074 0.00077 0.00078 0.00041 C4 0.17516 0.50336 0.36353 1.00000 0.03056 0.02344 0.02402 0.00337 0.01003 0.00159 0.02537 0.00390 0.00011 0.00049 0.00006 0.00000 0.00104 0.00104 0.00095 0.00079 0.00084 0.00083 0.00044 H4 0.19984 0.43427 0.34277 1.00000 0.03044 0.00000 0.00000 C5 0.10582 0.41442 0.36074 1.00000 0.03393 0.02414 0.02541 0.00048 0.00502 -0.00224 0.02794 0.00400 0.00011 0.00053 0.00006 0.00000 0.00113 0.00104 0.00099 0.00083 0.00088 0.00088 0.00045 H5 0.08299 0.28622 0.33770 1.00000 0.03353 0.00000 0.00000 C6 0.06974 0.51163 0.39138 1.00000 0.02514 0.02763 0.03090 0.00692 0.00716 -0.00079 0.02767 0.00406 0.00011 0.00053 0.00006 0.00000 0.00101 0.00114 0.00109 0.00086 0.00087 0.00084 0.00046 H6 0.02256 0.44798 0.38883 1.00000 0.03320 0.00000 0.00000 C7 0.10100 0.69931 0.42556 1.00000 0.02713 0.02900 0.02255 0.00637 0.00788 0.00305 0.02582 0.00396 0.00010 0.00052 0.00006 0.00000 0.00101 0.00110 0.00093 0.00082 0.00082 0.00084 0.00044 H7 0.07652 0.76210 0.44668 1.00000 0.03098 0.00000 0.00000 C8 0.16952 0.79097 0.42748 1.00000 0.02824 0.02377 0.01746 0.00607 0.00670 0.00353 0.02285 0.00377 0.00010 0.00048 0.00006 0.00000 0.00102 0.00101 0.00087 0.00075 0.00078 0.00081 0.00042 C9 0.33849 0.80983 0.39755 1.00000 0.02673 0.02543 0.01983 0.00244 0.00499 -0.00070 0.02394 0.00381 0.00010 0.00050 0.00006 0.00000 0.00100 0.00106 0.00091 0.00078 0.00079 0.00081 0.00043 H9 0.37832 0.89133 0.41615 1.00000 0.02873 0.00000 0.00000 C10 0.35058 0.68046 0.35742 1.00000 0.02546 0.02114 0.02172 0.00135 0.00799 -0.00260 0.02232 0.00364 0.00010 0.00048 0.00006 0.00000 0.00097 0.00099 0.00091 0.00075 0.00078 0.00079 0.00041 C11 0.30473 0.74999 0.31966 1.00000 0.02597 0.02227 0.02475 0.00136 0.00849 -0.00002 0.02386 0.00374 0.00010 0.00050 0.00006 0.00000 0.00099 0.00100 0.00097 0.00078 0.00081 0.00079 0.00043 H11 0.26320 0.86912 0.32005 1.00000 0.02863 0.00000 0.00000 C12 0.31933 0.64709 0.28189 1.00000 0.03016 0.02436 0.02156 0.00129 0.00624 -0.00230 0.02521 0.00381 0.00011 0.00049 0.00006 0.00000 0.00103 0.00107 0.00091 0.00080 0.00082 0.00084 0.00043 H12 0.28820 0.69604 0.25646 1.00000 0.03025 0.00000 0.00000 C13 0.37993 0.47162 0.28156 1.00000 0.03198 0.02264 0.02425 -0.00251 0.01304 -0.00381 0.02526 0.00384 0.00011 0.00050 0.00006 0.00000 0.00108 0.00103 0.00096 0.00079 0.00086 0.00083 0.00044 C14 0.42656 0.39948 0.31833 1.00000 0.02700 0.02434 0.03066 -0.00064 0.01048 -0.00123 0.02668 0.00390 0.00011 0.00052 0.00006 0.00000 0.00100 0.00103 0.00103 0.00085 0.00085 0.00085 0.00044 H14 0.46771 0.27783 0.31772 1.00000 0.03201 0.00000 0.00000 C15 0.41187 0.50845 0.35590 1.00000 0.02452 0.02401 0.02394 0.00015 0.00566 -0.00249 0.02404 0.00369 0.00010 0.00048 0.00006 0.00000 0.00098 0.00107 0.00097 0.00078 0.00081 0.00079 0.00043 H15 0.44403 0.46554 0.38112 1.00000 0.02884 0.00000 0.00000 O1W 0.46730 1.24958 0.47613 1.00000 0.03773 0.22323 0.07315 -0.04416 0.02366 -0.02916 0.10963 0.00515 0.00012 0.00100 0.00009 0.00000 0.00118 0.00377 0.00170 0.00202 0.00121 0.00167 0.00121 H1W 0.42349 1.23201 0.47801 1.00000 0.16444 0.09039 0.00120 0.01491 0.00166 0.00000 0.00000 H2WA_a 0.48472 1.37846 0.49640 0.50000 0.16444 0.05191 0.00421 0.01636 0.00180 0.00000 0.00000 H2WB_b 0.48694 1.06912 0.48493 0.50000 0.16444 0.16054 0.00401 0.01383 0.00189 0.00000 0.00000 Final Structure Factor Calculation for 2010src0795a Total number of l.s. parameters = 181 Maximum vector length = 511 Memory required = 2227 / 24017 wR2 = 0.1320 before cycle 21 for 2890 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 0.014 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.067; Restrained GooF = 1.066 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0620 * P )^2 + 2.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0470 for 2207 Fo > 4sig(Fo) and 0.0657 for all 2890 data wR2 = 0.1320, GooF = S = 1.067, Restrained GooF = 1.066 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 0.0457 0.0381 0.0184 Cl1 0.0432 0.0269 0.0179 O1 0.0346 0.0258 0.0143 N1 0.0319 0.0266 0.0153 C1 0.0281 0.0253 0.0150 C2 0.0285 0.0235 0.0141 C3 0.0330 0.0241 0.0191 C4 0.0348 0.0255 0.0235 C5 0.0364 0.0260 0.0206 C6 0.0343 0.0251 0.0181 C7 0.0312 0.0238 0.0136 C8 0.0274 0.0258 0.0186 C9 0.0273 0.0227 0.0169 C10 0.0284 0.0229 0.0203 C11 0.0310 0.0245 0.0202 C12 0.0366 0.0214 0.0178 C13 0.0333 0.0244 0.0223 C14 0.0268 0.0240 0.0213 C15 0.2377 0.0615 0.0296 O1W may be split into 0.4651 1.2994 0.4746 and 0.4695 1.1998 0.4777 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.023 0.036 0.049 0.065 0.084 0.109 0.141 0.204 1.000 Number in group 294. 285. 312. 267. 295. 287. 292. 283. 285. 290. GooF 0.942 0.876 0.956 1.066 1.346 1.136 1.091 1.034 1.181 0.961 K 2.667 1.282 1.253 0.975 0.965 0.996 1.008 1.012 1.013 1.008 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.65 inf Number in group 295. 288. 291. 288. 283. 289. 289. 290. 286. 291. GooF 1.089 1.021 0.942 0.983 0.971 1.033 1.042 1.132 1.054 1.342 K 0.996 1.012 1.023 1.001 1.035 1.023 1.021 1.026 1.009 1.000 R1 0.181 0.134 0.101 0.097 0.081 0.066 0.049 0.052 0.038 0.031 Recommended weighting scheme: WGHT 0.0620 2.1579 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) 5 1 22 764.24 1693.63 6.62 0.164 1.22 1 1 16 2994.67 6379.22 5.75 0.318 1.76 7 1 27 52.34 253.89 5.70 0.064 0.99 9 3 5 71.11 200.09 4.90 0.056 1.10 -10 0 8 327.60 165.08 4.89 0.051 1.89 10 0 22 1500.53 2642.65 4.86 0.205 1.06 -12 4 15 721.05 1391.84 4.55 0.149 0.82 -6 2 22 588.23 1256.14 4.29 0.141 1.17 -1 3 8 2328.81 3496.74 4.24 0.236 1.28 1 1 17 95.66 181.74 3.74 0.054 1.67 3 3 6 268.89 607.66 3.73 0.098 1.27 -18 2 2 4.80 67.97 3.68 0.033 0.95 3 1 39 74.52 207.25 3.65 0.057 0.78 -2 0 14 298.86 190.83 3.65 0.055 2.33 -7 1 28 50.69 123.47 3.63 0.044 1.10 2 0 10 44.13 102.87 3.61 0.040 2.87 0 2 2 86.12 158.61 3.58 0.050 2.00 1 3 3 1393.34 1955.36 3.52 0.176 1.33 -1 3 26 699.12 467.14 3.31 0.086 0.91 -12 0 6 1715.28 1314.32 3.28 0.145 1.63 3 5 4 366.89 730.29 3.21 0.108 0.80 -12 0 34 741.52 1086.03 3.19 0.131 0.89 -4 0 6 1076.05 1413.86 3.16 0.150 3.99 -14 2 33 492.20 328.88 3.13 0.072 0.81 -17 3 18 608.85 927.02 3.12 0.121 0.83 -6 0 16 1613.48 2269.64 3.11 0.190 1.87 1 3 13 295.53 427.48 3.07 0.082 1.17 -4 0 8 282.94 400.44 3.02 0.080 3.43 -22 0 14 29.72 115.27 2.99 0.043 0.88 7 1 9 65.91 122.17 2.96 0.044 1.79 3 1 15 153.75 239.57 2.94 0.062 1.73 -7 1 11 865.47 1110.73 2.88 0.133 1.95 -6 2 5 33.67 70.56 2.88 0.033 1.70 -19 1 18 181.40 281.40 2.79 0.067 0.94 7 1 29 85.74 183.95 2.75 0.054 0.94 -10 4 9 908.06 1244.20 2.74 0.141 0.89 -24 0 22 13.39 182.98 2.72 0.054 0.77 10 0 4 35.85 2.72 2.68 0.007 1.79 -13 1 19 4491.00 44.48 2.67 0.027 1.19 -14 0 16 533.12 397.21 2.66 0.079 1.26 7 3 12 3397.40 2734.40 2.61 0.208 1.07 -14 4 12 412.54 603.91 2.60 0.098 0.81 -17 1 20 641.90 855.08 2.58 0.117 0.99 11 3 22 432.68 278.27 2.56 0.066 0.82 -24 0 10 453.71 642.78 2.55 0.101 0.82 8 2 33 130.50 305.54 2.55 0.070 0.78 3 1 12 19.33 48.22 2.52 0.028 2.00 -5 1 22 142.24 217.62 2.51 0.059 1.37 -22 2 10 82.04 19.92 2.51 0.018 0.82 -4 0 4 1193.68 1485.07 2.50 0.154 4.54 Bond lengths and angles Cl1 - Distance Angles C13 1.7427 (0.0019) Cl1 - O1 - Distance Angles C1 1.2334 (0.0025) O1 - N1 - Distance Angles C1 1.3589 (0.0025) C8 1.4013 (0.0026) 111.15 (0.15) H1 0.8800 124.42 124.42 N1 - C1 C8 C1 - Distance Angles O1 1.2334 (0.0025) N1 1.3589 (0.0025) 125.11 (0.17) C2 1.5032 (0.0026) 127.99 (0.17) 106.89 (0.17) C1 - O1 N1 C2 - Distance Angles C9 1.3486 (0.0026) C3 1.4752 (0.0027) 135.18 (0.18) C1 1.5032 (0.0026) 118.96 (0.18) 105.79 (0.15) C2 - C9 C3 C3 - Distance Angles C4 1.3913 (0.0028) C8 1.4086 (0.0025) 118.89 (0.18) C2 1.4752 (0.0027) 134.97 (0.18) 106.11 (0.17) C3 - C4 C8 C4 - Distance Angles C3 1.3913 (0.0028) C5 1.3951 (0.0028) 119.02 (0.18) H4 0.9500 120.49 120.49 C4 - C3 C5 C5 - Distance Angles C6 1.3921 (0.0028) C4 1.3951 (0.0028) 120.67 (0.20) H5 0.9500 119.67 119.67 C5 - C6 C4 C6 - Distance Angles C7 1.3884 (0.0029) C5 1.3921 (0.0028) 121.63 (0.19) H6 0.9500 119.19 119.19 C6 - C7 C5 C7 - Distance Angles C8 1.3863 (0.0028) C6 1.3884 (0.0029) 117.01 (0.18) H7 0.9500 121.49 121.49 C7 - C8 C6 C8 - Distance Angles C7 1.3863 (0.0028) N1 1.4013 (0.0026) 127.13 (0.17) C3 1.4086 (0.0025) 122.77 (0.19) 110.05 (0.17) C8 - C7 N1 C9 - Distance Angles C2 1.3486 (0.0026) C10 1.4729 (0.0025) 128.47 (0.19) H9 0.9500 115.76 115.76 C9 - C2 C10 C10 - Distance Angles C15 1.4002 (0.0027) C11 1.4045 (0.0027) 118.41 (0.18) C9 1.4729 (0.0025) 119.90 (0.17) 121.46 (0.17) C10 - C15 C11 C11 - Distance Angles C12 1.3843 (0.0026) C10 1.4045 (0.0027) 120.82 (0.18) H11 0.9500 119.59 119.59 C11 - C12 C10 C12 - Distance Angles C11 1.3843 (0.0026) C13 1.3881 (0.0028) 119.29 (0.19) H12 0.9500 120.36 120.36 C12 - C11 C13 C13 - Distance Angles C12 1.3881 (0.0028) C14 1.3900 (0.0030) 121.41 (0.18) Cl1 1.7427 (0.0019) 118.73 (0.16) 119.85 (0.15) C13 - C12 C14 C14 - Distance Angles C15 1.3865 (0.0027) C13 1.3900 (0.0030) 118.73 (0.19) H14 0.9500 120.63 120.63 C14 - C15 C13 C15 - Distance Angles C14 1.3865 (0.0027) C10 1.4002 (0.0027) 121.32 (0.19) H15 0.9500 119.34 119.34 C15 - C14 C10 O1W - Distance Angles H1W 0.8782 (0.0190) H2WA_a 0.8586 (0.0193) 104.02 (4.39) H2WB_b 0.8482 (0.0194) 107.08 (4.81) 100.06 (7.96) 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 2.849(2) 167.3 N1-H1...O1_$1 0.878(19) 1.94(2) 2.813(3) 171(5) O1W-H1W...O1 0.859(19) 1.902(19) 2.718(6) 158(7) O1W-H2WA_a...O1W_$2 0.848(19) 1.906(19) 2.713(8) 158(7) O1W-H2WB_b...O1W_$3 FMAP and GRID set by program FMAP 2 3 38 GRID -0.714 -1 -2 0.714 1 2 R1 = 0.0652 for 2890 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.31 at 0.2258 0.4200 0.0723 [ 0.67 A from C2 ] Deepest hole -0.35 at 0.3905 0.5071 0.2344 [ 0.71 A from CL1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2236 / 16655 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2742 0.9200 0.4277 1.00000 0.05 0.31 0.67 C2 0.84 C1 1.74 C3 1.76 N1 Q2 1 0.3184 0.6273 0.3378 1.00000 0.05 0.26 0.78 C11 0.83 C10 1.49 H11 1.83 C12 Q3 1 0.1921 0.7178 0.4121 1.00000 0.05 0.24 0.63 C3 0.79 C8 1.76 C2 1.78 C4 Q4 1 0.3980 0.3441 0.3010 1.00000 0.05 0.24 0.75 C14 0.84 C13 1.40 H14 1.88 C15 Q5 1 0.4207 0.4946 0.3353 1.00000 0.05 0.23 0.70 C14 0.73 C15 1.47 H14 1.48 H15 Shortest distances between peaks (including symmetry equivalents) 4 5 1.28 1 3 1.79 2 5 2.10 2 4 2.44 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 0.02: 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. 0.81: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.31: Structure factors and derivatives 1.91: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.13: Apply other restraints 0.47: Solve l.s. equations 0.00: Generate HTAB table 0.14: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010src0795a finished at 21:21:24 Total CPU time: 4.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++