+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2010src0035 started at 09:41:45 on 24-Feb-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2010src0035 in P2(1)/c CELL 0.71073 9.4446 13.9129 10.3330 90.000 92.517 90.000 ZERR 4.00 0.0004 0.0007 0.0003 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H B N O UNIT 20 64 20 4 40 V = 1356.46 F(000) = 632.0 Mu = 0.13 mm-1 Cell Wt = 1216.95 Rho = 1.490 MERG 2 OMIT -3.00 55.00 OMIT -1 1 1 OMIT 1 1 1 SHEL 7 0.77 eadp c1 c21 eadp c2 c22 eadp c3 c23 eadp c4 c24 eadp c5 c25 eadp n1 n21 size 0.42 0.38 0.18 EQIV $1 x-1, y, z EQIV $2 x, -y+1/2, z-1/2 EQIV $3 -x+2, -y, -z EQIV $4 x, -y+1/2, z+1/2 EQIV $5 -x+1, -y, -z+1 EQIV $6 x-1, -y+1/2, z+1/2 EQIV $7 x, y, z+1 HTAB O7 O9_$1 HTAB O8 O6_$2 HTAB O9 O4_$3 HTAB O10 O3_$4 HTAB N1 O1_$5 HTAB N1 O10_$6 HTAB N1 O8_$7 HTAB N1 O2_$7 HTAB N21 O1_$5 HTAB N21 O10_$6 HTAB N21 O8_$7 HTAB N21 O2_$7 FMAP 2 PLAN 5 ACTA HTAB BOND $H WGHT 0.06270 0.25710 L.S. 18 TEMP -153.00 FVAR 0.80583 0.74037 MOLE 1 B1 3 0.779622 0.124574 0.128626 11.00000 0.01315 0.02274 = 0.01625 -0.00095 0.00064 -0.00064 B2 3 0.528864 0.076251 0.119780 11.00000 0.01562 0.02081 = 0.01771 -0.00188 0.00013 0.00017 B3 3 0.605370 0.190218 -0.033733 11.00000 0.01687 0.02375 = 0.01863 -0.00287 0.00066 0.00184 B4 3 1.039097 0.099624 0.135034 11.00000 0.01417 0.02137 = 0.01797 0.00048 -0.00077 -0.00007 B5 3 0.942974 0.214730 0.277450 11.00000 0.01702 0.02321 = 0.01699 -0.00051 0.00129 -0.00074 O1 5 0.666196 0.058701 0.159028 11.00000 0.01253 0.02140 = 0.01977 0.00110 0.00084 -0.00013 O2 5 0.495784 0.147675 0.030255 11.00000 0.01318 0.02708 = 0.02087 0.00328 0.00014 0.00209 O3 5 0.741677 0.180179 0.010447 11.00000 0.01406 0.02535 = 0.01789 0.00264 0.00055 -0.00031 O4 5 0.906511 0.068108 0.101019 11.00000 0.01235 0.02231 = 0.02093 -0.00381 0.00054 0.00039 O5 5 1.059153 0.172965 0.223054 11.00000 0.01327 0.02730 = 0.02539 -0.00778 0.00093 -0.00219 O6 5 0.809177 0.190076 0.238141 11.00000 0.01449 0.02543 = 0.01760 -0.00340 0.00057 -0.00065 O7 5 0.426694 0.020065 0.166863 11.00000 0.01314 0.02871 = 0.03410 0.00788 -0.00126 -0.00138 AFIX 147 H7 2 0.346955 0.039459 0.138663 11.00000 -1.50000 AFIX 0 O8 5 0.566794 0.240667 -0.142109 11.00000 0.01745 0.03524 = 0.02329 0.00828 0.00045 0.00228 AFIX 147 H8 2 0.639562 0.262052 -0.176122 11.00000 -1.50000 AFIX 0 O9 5 1.155265 0.060043 0.084019 11.00000 0.01303 0.03033 = 0.02846 -0.01019 -0.00150 0.00074 AFIX 147 H9 2 1.129942 0.019362 0.027562 11.00000 -1.50000 AFIX 0 O10 5 0.973796 0.281466 0.370545 11.00000 0.01672 0.03272 = 0.02503 -0.01095 0.00196 -0.00288 AFIX 147 H10 2 0.899207 0.297125 0.406601 11.00000 -1.50000 AFIX 0 MOLE 2 PART 1 C1 1 0.258595 0.157821 0.662594 21.00000 0.01826 0.02493 = 0.02426 0.00442 0.01193 0.00689 AFIX 13 H1 2 0.247136 0.227531 0.641009 21.00000 -1.20000 AFIX 0 C2 1 0.130315 0.099615 0.605592 21.00000 0.03309 0.04163 = 0.02567 -0.00001 -0.00373 0.00134 AFIX 23 H2A 2 0.089893 0.058685 0.673106 21.00000 -1.20000 H2B 2 0.055448 0.143375 0.570429 21.00000 -1.20000 AFIX 0 C3 1 0.188678 0.037333 0.496981 21.00000 0.06439 0.04377 = 0.03081 -0.00157 0.00731 0.00246 AFIX 23 H3A 2 0.201892 -0.029937 0.526320 21.00000 -1.20000 H3B 2 0.123177 0.037989 0.419510 21.00000 -1.20000 AFIX 0 C4 1 0.327422 0.081632 0.467323 21.00000 0.06235 0.04707 = 0.03082 0.00043 0.01396 0.02011 AFIX 23 H4A 2 0.313794 0.135935 0.406125 21.00000 -1.20000 H4B 2 0.390846 0.033685 0.429156 21.00000 -1.20000 AFIX 0 C5 1 0.388622 0.116656 0.598214 21.00000 0.03462 0.02883 = 0.03777 0.00470 0.01863 0.01182 AFIX 23 H5A 2 0.461533 0.166770 0.587216 21.00000 -1.20000 H5B 2 0.430842 0.062933 0.649514 21.00000 -1.20000 AFIX 0 N1 4 0.272728 0.144320 0.806977 21.00000 0.01939 0.02782 = 0.02417 -0.00226 -0.00081 0.00255 AFIX 137 H1A 2 0.282358 0.080640 0.825443 21.00000 -1.50000 H1B 2 0.193973 0.167517 0.843923 21.00000 -1.50000 H1C 2 0.350405 0.176633 0.838936 21.00000 -1.50000 AFIX 0 PART 2 same c1 > n1 C21 1 0.285455 0.154695 0.644883 -21.00000 0.01826 0.02493 = 0.02426 0.00442 0.01193 0.00689 AFIX 13 H21 2 0.295847 0.224610 0.624956 -21.00000 -1.20000 AFIX 0 C22 1 0.139938 0.120864 0.588224 -21.00000 0.03309 0.04163 = 0.02567 -0.00001 -0.00373 0.00134 AFIX 23 H22A 2 0.070097 0.114902 0.656468 -21.00000 -1.20000 H22B 2 0.102391 0.165147 0.520017 -21.00000 -1.20000 AFIX 0 C23 1 0.176527 0.023349 0.532359 -21.00000 0.06439 0.04377 = 0.03081 -0.00157 0.00731 0.00246 AFIX 23 H23A 2 0.138182 -0.028146 0.586909 -21.00000 -1.20000 H23B 2 0.132331 0.017081 0.444101 -21.00000 -1.20000 AFIX 0 C24 1 0.327833 0.012582 0.527063 -21.00000 0.06235 0.04707 = 0.03082 0.00043 0.01396 0.02011 AFIX 23 H24A 2 0.354102 0.003054 0.436251 -21.00000 -1.20000 H24B 2 0.359519 -0.044358 0.577979 -21.00000 -1.20000 AFIX 0 C25 1 0.398959 0.102153 0.582054 -21.00000 0.03462 0.02883 = 0.03777 0.00470 0.01863 0.01182 AFIX 23 H25A 2 0.476241 0.085169 0.645790 -21.00000 -1.20000 H25B 2 0.438714 0.141249 0.512301 -21.00000 -1.20000 AFIX 0 N21 4 0.287425 0.143208 0.787998 -21.00000 0.01939 0.02782 = 0.02417 -0.00226 -0.00081 0.00255 AFIX 137 H21A 2 0.288298 0.079556 0.808284 -21.00000 -1.50000 H21B 2 0.208853 0.171171 0.819347 -21.00000 -1.50000 H21C 2 0.366332 0.171864 0.823960 -21.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 2010src0035 in P2(1)/c C 0.770 H 0.320 B 0.820 N 0.700 O 0.660 B1 - O1 O6 O4 O3 B2 - O7 O1 O2 B3 - O3 O8 O2 B4 - O9 O4 O5 B5 - O6 O10 O5 O1 - B2 B1 O2 - B2 B3 O3 - B3 B1 O4 - B4 B1 O5 - B4 B5 O6 - B5 B1 O7 - B2 O8 - B3 O9 - B4 O10 - B5 C1_a - N1_a C5_a C2_a C2_a - C3_a C1_a C3_a - C4_a C2_a C4_a - C3_a C5_a C5_a - C4_a C1_a N1_a - C1_a C21_b - C25_b N21_b C22_b C22_b - C23_b C21_b C23_b - C24_b C22_b C24_b - C23_b C25_b C25_b - C21_b C24_b N21_b - C21_b Operators for generating equivalent atoms: $1 x-1, y, z $2 x, -y+1/2, z-1/2 $3 -x+2, -y, -z $4 x, -y+1/2, z+1/2 $5 -x+1, -y, -z+1 $6 x-1, -y+1/2, z+1/2 $7 x, y, z+1 16516 Reflections read, of which 526 rejected -12 =< h =< 12, -18 =< k =< 16, -13 =< l =< 13, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 3110 Unique reflections, of which 0 suppressed R(int) = 0.0500 R(sigma) = 0.0447 Friedel opposites merged Maximum memory for data reduction = 3275 / 31168 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 = 3976 / 267397 wR2 = 0.1205 before cycle 1 for 3110 data and 215 / 215 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.0613 0.0200 SAME/SADI C1_a C5_a C21_b C25_b Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 13. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.039 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.026; Restrained GooF = 1.028 for 13 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80574 0.00189 -0.049 OSF 2 0.74085 0.00349 0.137 FVAR 2 Mean shift/esd = 0.048 Maximum = -0.162 for U33 O5 Max. shift = 0.007 A for H21C_b Max. dU = 0.000 for B5 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3976 / 267397 wR2 = 0.1205 before cycle 2 for 3110 data and 215 / 215 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.0611 0.0200 SAME/SADI C1_a C5_a C21_b C25_b Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 13. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.027; Restrained GooF = 1.029 for 13 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80552 0.00189 -0.115 OSF 2 0.74097 0.00349 0.035 FVAR 2 Mean shift/esd = 0.020 Maximum = -0.115 for OSF Max. shift = 0.003 A for C25_b Max. dU = 0.000 for N1_a Least-squares cycle 3 Maximum vector length = 511 Memory required = 3976 / 267397 wR2 = 0.1205 before cycle 3 for 3110 data and 215 / 215 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 0.0608 0.0200 SAME/SADI C1_a C5_a C21_b C25_b Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 13. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.027; Restrained GooF = 1.029 for 13 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80552 0.00189 0.000 OSF 2 0.74096 0.00349 -0.003 FVAR 2 Mean shift/esd = 0.004 Maximum = 0.051 for y C25_b Max. shift = 0.002 A for H21B_b Max. dU = 0.000 for C1_a Least-squares cycle 4 Maximum vector length = 511 Memory required = 3976 / 267397 wR2 = 0.1205 before cycle 4 for 3110 data and 215 / 215 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.0608 0.0200 SAME/SADI C1_a C5_a C21_b C25_b Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 13. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.027; Restrained GooF = 1.029 for 13 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80552 0.00189 0.004 OSF 2 0.74094 0.00349 -0.005 FVAR 2 Mean shift/esd = 0.003 Maximum = 0.029 for y C25_b Max. shift = 0.001 A for H21B_b Max. dU = 0.000 for C1_a Least-squares cycle 5 Maximum vector length = 511 Memory required = 3976 / 267397 wR2 = 0.1205 before cycle 5 for 3110 data and 215 / 215 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 0.0608 0.0200 SAME/SADI C1_a C5_a C21_b C25_b Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 13. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.027; Restrained GooF = 1.029 for 13 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80553 0.00189 0.001 OSF 2 0.74094 0.00349 -0.002 FVAR 2 Mean shift/esd = 0.001 Maximum = 0.017 for z C5_a Max. shift = 0.001 A for H25B_b Max. dU = 0.000 for C1_a Least-squares cycle 6 Maximum vector length = 511 Memory required = 3976 / 267397 wR2 = 0.1205 before cycle 6 for 3110 data and 215 / 215 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint 0.0608 0.0200 SAME/SADI C1_a C5_a C21_b C25_b Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 13. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.027; Restrained GooF = 1.029 for 13 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80553 0.00189 0.001 OSF 2 0.74094 0.00349 -0.001 FVAR 2 Mean shift/esd = 0.001 Maximum = 0.010 for z C5_a Max. shift = 0.000 A for C25_b Max. dU = 0.000 for C1_a Least-squares cycle 7 Maximum vector length = 511 Memory required = 3976 / 267397 wR2 = 0.1204 before cycle 7 for 3110 data and 215 / 215 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint 0.0608 0.0200 SAME/SADI C1_a C5_a C21_b C25_b Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 13. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.027; Restrained GooF = 1.029 for 13 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80553 0.00189 0.001 OSF 2 0.74093 0.00349 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.006 for z C5_a Max. shift = 0.000 A for C25_b Max. dU = 0.000 for N1_a Least-squares cycle 8 Maximum vector length = 511 Memory required = 3976 / 267397 wR2 = 0.1204 before cycle 8 for 3110 data and 215 / 215 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint 0.0608 0.0200 SAME/SADI C1_a C5_a C21_b C25_b Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 13. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.027; Restrained GooF = 1.029 for 13 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80553 0.00189 0.001 OSF 2 0.74093 0.00349 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.004 for z C5_a Max. shift = 0.000 A for C25_b Max. dU = 0.000 for N1_a Least-squares cycle 9 Maximum vector length = 511 Memory required = 3976 / 267397 wR2 = 0.1204 before cycle 9 for 3110 data and 215 / 215 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint 0.0608 0.0200 SAME/SADI C1_a C5_a C21_b C25_b Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 13. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.027; Restrained GooF = 1.029 for 13 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80553 0.00189 0.001 OSF 2 0.74093 0.00349 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.002 for z C5_a Max. shift = 0.000 A for H25B_b Max. dU = 0.000 for N1_a Least-squares cycle 10 Maximum vector length = 511 Memory required = 3976 / 267397 wR2 = 0.1204 before cycle 10 for 3110 data and 215 / 215 parameters Disagreeable restraints before cycle 10 Observed Target Error Sigma Restraint 0.0608 0.0200 SAME/SADI C1_a C5_a C21_b C25_b Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 13. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.027; Restrained GooF = 1.029 for 13 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80553 0.00189 0.000 OSF 2 0.74093 0.00349 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.001 for z C5_a Max. shift = 0.000 A for H25B_b Max. dU = 0.000 for N1_a Least-squares cycle 11 Maximum vector length = 511 Memory required = 3976 / 267397 wR2 = 0.1204 before cycle 11 for 3110 data and 215 / 215 parameters Disagreeable restraints before cycle 11 Observed Target Error Sigma Restraint 0.0608 0.0200 SAME/SADI C1_a C5_a C21_b C25_b Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 13. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.027; Restrained GooF = 1.029 for 13 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80553 0.00189 0.000 OSF 2 0.74093 0.00349 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.001 for z C5_a Max. shift = 0.000 A for C25_b Max. dU = 0.000 for N1_a Least-squares cycle 12 Maximum vector length = 511 Memory required = 3976 / 267397 wR2 = 0.1204 before cycle 12 for 3110 data and 215 / 215 parameters Disagreeable restraints before cycle 12 Observed Target Error Sigma Restraint 0.0608 0.0200 SAME/SADI C1_a C5_a C21_b C25_b Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 13. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.027; Restrained GooF = 1.029 for 13 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80553 0.00189 0.000 OSF 2 0.74093 0.00349 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z C5_a Max. shift = 0.000 A for H21A_b Max. dU = 0.000 for N1_a Least-squares cycle 13 Maximum vector length = 511 Memory required = 3976 / 267397 wR2 = 0.1204 before cycle 13 for 3110 data and 215 / 215 parameters Disagreeable restraints before cycle 13 Observed Target Error Sigma Restraint 0.0608 0.0200 SAME/SADI C1_a C5_a C21_b C25_b Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 13. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.027; Restrained GooF = 1.029 for 13 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80553 0.00189 0.000 OSF 2 0.74093 0.00349 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x O6 Max. shift = 0.000 A for H21B_b Max. dU = 0.000 for C3_a Least-squares cycle 14 Maximum vector length = 511 Memory required = 3976 / 267397 wR2 = 0.1204 before cycle 14 for 3110 data and 215 / 215 parameters Disagreeable restraints before cycle 14 Observed Target Error Sigma Restraint 0.0608 0.0200 SAME/SADI C1_a C5_a C21_b C25_b Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 13. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.027; Restrained GooF = 1.029 for 13 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80553 0.00189 0.000 OSF 2 0.74093 0.00349 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x O6 Max. shift = 0.000 A for C25_b Max. dU = 0.000 for N1_a Least-squares cycle 15 Maximum vector length = 511 Memory required = 3976 / 267397 wR2 = 0.1204 before cycle 15 for 3110 data and 215 / 215 parameters Disagreeable restraints before cycle 15 Observed Target Error Sigma Restraint 0.0608 0.0200 SAME/SADI C1_a C5_a C21_b C25_b Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 13. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.027; Restrained GooF = 1.029 for 13 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80553 0.00189 0.000 OSF 2 0.74093 0.00349 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x O6 Max. shift = 0.000 A for H25B_b Max. dU = 0.000 for C2_a Least-squares cycle 16 Maximum vector length = 511 Memory required = 3976 / 267397 wR2 = 0.1204 before cycle 16 for 3110 data and 215 / 215 parameters Disagreeable restraints before cycle 16 Observed Target Error Sigma Restraint 0.0608 0.0200 SAME/SADI C1_a C5_a C21_b C25_b Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 13. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.027; Restrained GooF = 1.029 for 13 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80553 0.00189 0.000 OSF 2 0.74093 0.00349 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x B4 Max. shift = 0.000 A for H21B_b Max. dU = 0.000 for C5_a Least-squares cycle 17 Maximum vector length = 511 Memory required = 3976 / 267397 wR2 = 0.1204 before cycle 17 for 3110 data and 215 / 215 parameters Disagreeable restraints before cycle 17 Observed Target Error Sigma Restraint 0.0608 0.0200 SAME/SADI C1_a C5_a C21_b C25_b Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 13. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.027; Restrained GooF = 1.029 for 13 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80553 0.00189 0.000 OSF 2 0.74093 0.00349 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x O6 Max. shift = 0.000 A for C25_b Max. dU = 0.000 for C2_a Least-squares cycle 18 Maximum vector length = 511 Memory required = 3976 / 267397 wR2 = 0.1204 before cycle 18 for 3110 data and 215 / 215 parameters Disagreeable restraints before cycle 18 Observed Target Error Sigma Restraint 0.0608 0.0200 SAME/SADI C1_a C5_a C21_b C25_b Summary of restraints applied in cycle 18 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 13. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.027; Restrained GooF = 1.029 for 13 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80553 0.00189 0.000 OSF 2 0.74093 0.00349 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x O6 Max. shift = 0.000 A for H21A_b Max. dU = 0.000 for C2_a Largest correlation matrix elements -0.987 y N21_b / y N1_a -0.912 y C21_b / y C1_a -0.873 x C21_b / U11 C1_a -0.973 x N21_b / x N1_a 0.910 z N21_b / U33 N1_a -0.869 x C25_b / x C5_a 0.949 y N21_b / U23 N1_a -0.907 y C25_b / y C5_a -0.868 z C21_b / z C1_a -0.943 U23 N1_a / y N1_a -0.904 y N21_b / U12 N1_a -0.861 U12 N1_a / U23 N1_a -0.930 z C25_b / z C5_a 0.896 U12 N1_a / y N1_a 0.860 z C21_b / U33 C1_a -0.929 z N21_b / z N1_a -0.888 U33 N1_a / z N1_a -0.858 z C22_b / z C2_a -0.926 x N21_b / U11 N1_a 0.883 z C25_b / U33 C5_a -0.853 U33 C5_a / z C5_a 0.912 U11 N1_a / x N1_a 0.882 y C25_b / U22 C5_a -0.850 tors H21A_b / tors H1A_a Idealized hydrogen atom generation before cycle 19 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H7 0.3469 0.0396 0.1389 147 0.840 0.000 O7 B2 H7 H8 0.6396 0.2619 -0.1763 147 0.840 0.000 O8 B3 H8 H9 1.1300 0.0194 0.0275 147 0.840 0.000 O9 B4 H9 H10 0.8993 0.2970 0.4068 147 0.840 0.000 O10 B5 H10 H1 0.2472 0.2275 0.6409 13 1.000 0.000 C1_a N1_a C5_a C2_a H2A 0.0899 0.0587 0.6731 23 0.990 0.000 C2_a C3_a C1_a H2B 0.0555 0.1434 0.5704 23 0.990 0.000 C2_a C3_a C1_a H3A 0.2019 -0.0299 0.5263 23 0.990 0.000 C3_a C4_a C2_a H3B 0.1232 0.0380 0.4195 23 0.990 0.000 C3_a C4_a C2_a H4A 0.3138 0.1360 0.4062 23 0.990 0.000 C4_a C3_a C5_a H4B 0.3908 0.0337 0.4291 23 0.990 0.000 C4_a C3_a C5_a H5A 0.4618 0.1666 0.5875 23 0.990 0.000 C5_a C4_a C1_a H5B 0.4307 0.0627 0.6497 23 0.990 0.000 C5_a C4_a C1_a H1A 0.2827 0.0807 0.8255 137 0.910 0.000 N1_a C1_a H1A_a H1B 0.1938 0.1673 0.8438 137 0.910 0.000 N1_a C1_a H1A_a H1C 0.3501 0.1769 0.8389 137 0.910 0.000 N1_a C1_a H1A_a H21 0.2953 0.2248 0.6253 13 1.000 0.000 C21_b C25_b N21_b C22_b H22A 0.0700 0.1149 0.6565 23 0.990 0.000 C22_b C23_b C21_b H22B 0.1023 0.1652 0.5201 23 0.990 0.000 C22_b C23_b C21_b H23A 0.1382 -0.0281 0.5870 23 0.990 0.000 C23_b C24_b C22_b H23B 0.1322 0.0171 0.4442 23 0.990 0.000 C23_b C24_b C22_b H24A 0.3540 0.0028 0.4362 23 0.990 0.000 C24_b C23_b C25_b H24B 0.3597 -0.0441 0.5783 23 0.990 0.000 C24_b C23_b C25_b H25A 0.4766 0.0860 0.6448 23 0.990 0.000 C25_b C21_b C24_b H25B 0.4376 0.1418 0.5114 23 0.990 0.000 C25_b C21_b C24_b H21A 0.2874 0.0795 0.8081 137 0.910 0.000 N21_b C21_b H21A_b H21B 0.2095 0.1716 0.8197 137 0.910 0.000 N21_b C21_b H21A_b H21C 0.3670 0.1712 0.8238 137 0.910 0.000 N21_b C21_b H21A_b 2010src0035 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq B1 0.77962 0.12458 0.12862 1.00000 0.01304 0.02270 0.01617 -0.00095 0.00065 -0.00065 0.01730 0.00288 0.00016 0.00014 0.00015 0.00000 0.00080 0.00096 0.00076 0.00066 0.00059 0.00068 0.00036 B2 0.52885 0.07624 0.11978 1.00000 0.01550 0.02080 0.01757 -0.00187 0.00015 0.00017 0.01797 0.00297 0.00018 0.00013 0.00015 0.00000 0.00081 0.00092 0.00076 0.00066 0.00060 0.00071 0.00036 B3 0.60536 0.19021 -0.03373 1.00000 0.01676 0.02368 0.01853 -0.00285 0.00061 0.00185 0.01966 0.00303 0.00018 0.00014 0.00016 0.00000 0.00083 0.00097 0.00077 0.00069 0.00061 0.00073 0.00037 B4 1.03908 0.09963 0.13504 1.00000 0.01407 0.02125 0.01793 0.00043 -0.00076 -0.00009 0.01779 0.00293 0.00017 0.00013 0.00015 0.00000 0.00079 0.00095 0.00078 0.00066 0.00060 0.00070 0.00036 B5 0.94297 0.21472 0.27745 1.00000 0.01696 0.02307 0.01684 -0.00053 0.00123 -0.00073 0.01894 0.00303 0.00018 0.00014 0.00015 0.00000 0.00084 0.00097 0.00076 0.00066 0.00061 0.00072 0.00037 O1 0.66619 0.05871 0.15903 1.00000 0.01242 0.02134 0.01970 0.00112 0.00081 -0.00017 0.01782 0.00172 0.00010 0.00008 0.00009 0.00000 0.00052 0.00061 0.00050 0.00042 0.00038 0.00043 0.00025 O2 0.49579 0.14768 0.03025 1.00000 0.01308 0.02703 0.02081 0.00328 0.00015 0.00207 0.02033 0.00183 0.00010 0.00008 0.00009 0.00000 0.00052 0.00065 0.00052 0.00044 0.00039 0.00045 0.00026 O3 0.74168 0.18018 0.01045 1.00000 0.01397 0.02528 0.01784 0.00264 0.00053 -0.00029 0.01903 0.00179 0.00010 0.00008 0.00009 0.00000 0.00051 0.00062 0.00049 0.00042 0.00037 0.00045 0.00025 O4 0.90652 0.06810 0.10102 1.00000 0.01227 0.02222 0.02084 -0.00379 0.00052 0.00041 0.01845 0.00170 0.00010 0.00008 0.00009 0.00000 0.00052 0.00062 0.00052 0.00043 0.00039 0.00044 0.00025 O5 1.05916 0.17296 0.22305 1.00000 0.01319 0.02720 0.02527 -0.00780 0.00092 -0.00220 0.02189 0.00175 0.00010 0.00008 0.00010 0.00000 0.00053 0.00066 0.00054 0.00046 0.00040 0.00046 0.00027 O6 0.80916 0.19007 0.23814 1.00000 0.01441 0.02534 0.01753 -0.00342 0.00056 -0.00065 0.01909 0.00174 0.00010 0.00008 0.00009 0.00000 0.00052 0.00063 0.00049 0.00043 0.00038 0.00045 0.00025 O7 0.42670 0.02006 0.16686 1.00000 0.01309 0.02865 0.03401 0.00786 -0.00129 -0.00134 0.02532 0.00197 0.00011 0.00009 0.00011 0.00000 0.00054 0.00069 0.00060 0.00050 0.00045 0.00048 0.00028 H7 0.34694 0.03960 0.13891 1.00000 0.03797 0.00000 0.00000 O8 0.56678 0.24067 -0.14211 1.00000 0.01736 0.03518 0.02323 0.00828 0.00044 0.00230 0.02527 0.00203 0.00011 0.00009 0.00010 0.00000 0.00056 0.00073 0.00055 0.00048 0.00042 0.00051 0.00028 H8 0.63956 0.26191 -0.17625 1.00000 0.03790 0.00000 0.00000 O9 1.15528 0.06005 0.08402 1.00000 0.01297 0.03026 0.02838 -0.01020 -0.00148 0.00074 0.02394 0.00186 0.00011 0.00009 0.00010 0.00000 0.00054 0.00071 0.00058 0.00048 0.00042 0.00047 0.00028 H9 1.12996 0.01940 0.02752 1.00000 0.03591 0.00000 0.00000 O10 0.97380 0.28146 0.37054 1.00000 0.01664 0.03266 0.02496 -0.01096 0.00196 -0.00286 0.02472 0.00179 0.00011 0.00009 0.00010 0.00000 0.00055 0.00070 0.00056 0.00048 0.00042 0.00050 0.00028 H10 0.89925 0.29699 0.40676 1.00000 0.03708 0.00000 0.00000 C1_a 0.25862 0.15777 0.66257 0.74093 0.01850 0.02493 0.02428 0.00458 0.01175 0.00674 0.02225 0.00872 0.00044 0.00041 0.00046 0.00349 0.00204 0.00102 0.00169 0.00108 0.00114 0.00138 0.00072 H1_a 0.24725 0.22748 0.64091 0.74093 0.02670 0.00349 0.00000 C2_a 0.13036 0.09961 0.60559 0.74093 0.03314 0.04144 0.02573 -0.00001 -0.00378 0.00141 0.03359 0.00935 0.00053 0.00033 0.00047 0.00349 0.00123 0.00272 0.00177 0.00160 0.00109 0.00156 0.00103 H2A_a 0.08994 0.05868 0.67311 0.74093 0.04030 0.00349 0.00000 H2B_a 0.05550 0.14338 0.57045 0.74093 0.04030 0.00349 0.00000 C3_a 0.18868 0.03733 0.49697 0.74093 0.06433 0.04388 0.03069 -0.00170 0.00725 0.00249 0.04615 0.00766 0.00045 0.00034 0.00031 0.00349 0.00185 0.00209 0.00218 0.00171 0.00155 0.00144 0.00093 H3A_a 0.20187 -0.02995 0.52629 0.74093 0.05538 0.00349 0.00000 H3B_a 0.12317 0.03801 0.41950 0.74093 0.05538 0.00349 0.00000 C4_a 0.32743 0.08161 0.46732 0.74093 0.06208 0.04711 0.03069 0.00040 0.01382 0.02008 0.04628 0.00534 0.00032 0.00022 0.00024 0.00349 0.00178 0.00170 0.00131 0.00108 0.00116 0.00145 0.00072 H4A_a 0.31383 0.13598 0.40622 0.74093 0.05554 0.00349 0.00000 H4B_a 0.39082 0.03368 0.42906 0.74093 0.05554 0.00349 0.00000 C5_a 0.38871 0.11651 0.59841 0.74093 0.03457 0.02943 0.03713 0.00463 0.01862 0.01149 0.03321 0.00864 0.00054 0.00051 0.00069 0.00349 0.00127 0.00245 0.00226 0.00129 0.00113 0.00136 0.00080 H5A_a 0.46176 0.16655 0.58755 0.74093 0.03985 0.00349 0.00000 H5B_a 0.43071 0.06271 0.64971 0.74093 0.03985 0.00349 0.00000 N1_a 0.27269 0.14434 0.80695 0.74093 0.01921 0.02774 0.02420 -0.00231 -0.00075 0.00265 0.02377 0.01729 0.00087 0.00088 0.00052 0.00349 0.00200 0.00089 0.00183 0.00197 0.00136 0.00151 0.00077 H1A_a 0.28269 0.08069 0.82546 0.74093 0.03565 0.00349 0.00000 H1B_a 0.19376 0.16733 0.84382 0.74093 0.03565 0.00349 0.00000 H1C_a 0.35015 0.17687 0.83894 0.74093 0.03565 0.00349 0.00000 C21_b 0.28525 0.15482 0.64497 0.25907 0.01850 0.02493 0.02428 0.00458 0.01175 0.00674 0.02225 0.02828 0.00158 0.00137 0.00158 0.00349 0.00204 0.00102 0.00169 0.00108 0.00114 0.00138 0.00072 H21_b 0.29534 0.22480 0.62527 0.25907 0.02670 0.00349 0.00000 C22_b 0.13987 0.12092 0.58830 0.25907 0.03314 0.04144 0.02573 -0.00001 -0.00378 0.00141 0.03359 0.02931 0.00165 0.00117 0.00173 0.00349 0.00123 0.00272 0.00177 0.00160 0.00109 0.00156 0.00103 H22A_b 0.07002 0.11494 0.65653 0.25907 0.04030 0.00349 0.00000 H22B_b 0.10230 0.16519 0.52008 0.25907 0.04030 0.00349 0.00000 C23_b 0.17648 0.02340 0.53243 0.25907 0.06433 0.04388 0.03069 -0.00170 0.00725 0.00249 0.04615 0.02574 0.00144 0.00112 0.00122 0.00349 0.00185 0.00209 0.00218 0.00171 0.00155 0.00144 0.00093 H23A_b 0.13819 -0.02809 0.58702 0.25907 0.05538 0.00349 0.00000 H23B_b 0.13221 0.01712 0.44421 0.25907 0.05538 0.00349 0.00000 C24_b 0.32781 0.01263 0.52702 0.25907 0.06208 0.04711 0.03069 0.00040 0.01382 0.02008 0.04628 0.01497 0.00089 0.00061 0.00069 0.00349 0.00178 0.00170 0.00131 0.00108 0.00116 0.00145 0.00072 H24A_b 0.35401 0.00281 0.43624 0.25907 0.05554 0.00349 0.00000 H24B_b 0.35967 -0.04409 0.57830 0.25907 0.05554 0.00349 0.00000 C25_b 0.39869 0.10264 0.58147 0.25907 0.03457 0.02943 0.03713 0.00463 0.01862 0.01149 0.03321 0.02652 0.00171 0.00159 0.00228 0.00349 0.00127 0.00245 0.00226 0.00129 0.00113 0.00136 0.00080 H25A_b 0.47658 0.08600 0.64476 0.25907 0.03985 0.00349 0.00000 H25B_b 0.43757 0.14182 0.51137 0.25907 0.03985 0.00349 0.00000 N21_b 0.28752 0.14313 0.78800 0.25907 0.01921 0.02774 0.02420 -0.00231 -0.00075 0.00265 0.02377 0.05270 0.00281 0.00273 0.00164 0.00349 0.00200 0.00089 0.00183 0.00197 0.00136 0.00151 0.00077 H21A_b 0.28743 0.07945 0.80810 0.25907 0.03565 0.00349 0.00000 H21B_b 0.20952 0.17163 0.81967 0.25907 0.03565 0.00349 0.00000 H21C_b 0.36699 0.17116 0.82383 0.25907 0.03565 0.00349 0.00000 Final Structure Factor Calculation for 2010src0035 in P2(1)/c Total number of l.s. parameters = 215 Maximum vector length = 511 Memory required = 3761 / 24017 wR2 = 0.1204 before cycle 19 for 3110 data and 0 / 215 parameters Disagreeable restraints before cycle 19 Observed Target Error Sigma Restraint 0.0608 0.0200 SAME/SADI C1_a C5_a C21_b C25_b Summary of restraints applied in cycle 19 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 13. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.027; Restrained GooF = 1.029 for 13 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0447 for 2319 Fo > 4sig(Fo) and 0.0665 for all 3110 data wR2 = 0.1204, GooF = S = 1.027, Restrained GooF = 1.029 for all data Occupancy sum of asymmetric unit = 21.00 for non-hydrogen and 16.00 for hydrogen atoms Principal mean square atomic displacements U 0.0229 0.0160 0.0130 B1 0.0217 0.0169 0.0154 B2 0.0254 0.0176 0.0161 B3 0.0213 0.0184 0.0136 B4 0.0232 0.0172 0.0164 B5 0.0219 0.0191 0.0124 O1 0.0286 0.0197 0.0127 O2 0.0261 0.0170 0.0140 O3 0.0254 0.0177 0.0123 O4 0.0342 0.0187 0.0128 O5 0.0266 0.0163 0.0143 O6 0.0400 0.0230 0.0129 O7 0.0395 0.0198 0.0165 O8 0.0398 0.0193 0.0127 O9 0.0407 0.0175 0.0159 O10 0.0370 0.0206 0.0092 C1_a 0.0417 0.0357 0.0233 C2_a 0.0651 0.0440 0.0294 C3_a 0.0777 0.0377 0.0235 C4_a 0.0568 0.0276 0.0153 C5_a 0.0299 0.0231 0.0183 N1_a 0.0370 0.0206 0.0092 C21_b 0.0417 0.0357 0.0233 C22_b 0.0651 0.0440 0.0294 C23_b 0.0777 0.0377 0.0235 C24_b 0.0568 0.0276 0.0153 C25_b 0.0299 0.0231 0.0183 N21_b Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.022 0.032 0.044 0.057 0.072 0.093 0.123 0.189 1.000 Number in group 323. 321. 298. 302. 336. 308. 296. 304. 312. 310. GooF 0.853 0.947 1.047 1.081 1.091 1.121 1.148 1.003 0.980 0.975 K 2.375 1.032 0.918 0.916 0.938 0.983 0.988 1.018 1.035 1.005 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 319. 312. 315. 298. 312. 310. 310. 311. 310. 313. GooF 0.979 0.978 0.989 0.989 0.983 1.026 1.041 0.882 1.038 1.308 K 1.005 1.051 1.025 1.000 1.024 1.038 1.039 1.037 1.025 0.979 R1 0.186 0.147 0.139 0.101 0.074 0.062 0.046 0.035 0.033 0.034 Recommended weighting scheme: WGHT 0.0612 0.2699 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) -7 6 4 31.03 63.70 4.77 0.062 1.08 -2 2 1 85.33 128.34 4.62 0.088 3.70 4 6 9 16.85 38.74 3.84 0.049 0.93 3 1 0 115.13 158.49 3.83 0.098 3.07 1 4 2 209.45 158.01 3.73 0.098 2.74 1 7 0 140.84 102.12 3.68 0.079 1.94 2 2 6 22.63 12.39 3.50 0.027 1.55 -4 1 1 16.08 8.75 3.41 0.023 2.29 -7 4 4 42.17 64.46 3.24 0.063 1.15 2 6 5 1.90 7.87 3.23 0.022 1.45 -1 0 4 610.94 762.94 3.21 0.216 2.52 -2 0 2 36.10 24.65 3.18 0.039 3.56 7 3 8 29.93 57.79 3.09 0.059 0.90 9 6 1 65.82 91.06 3.07 0.075 0.95 2 2 4 1.60 6.14 3.06 0.019 2.12 -5 3 3 130.27 98.77 3.05 0.078 1.58 4 4 3 129.15 100.50 3.03 0.078 1.67 7 8 2 666.09 530.48 2.99 0.180 1.04 2 0 10 25.96 50.12 2.97 0.055 1.00 3 9 7 -3.14 3.41 2.96 0.014 1.00 -4 2 5 44.59 31.64 2.91 0.044 1.55 -6 2 7 118.93 155.16 2.91 0.097 1.09 -7 9 8 134.46 93.81 2.85 0.076 0.81 -7 6 5 28.02 43.27 2.85 0.051 1.03 1 12 2 37.08 57.89 2.82 0.059 1.12 1 12 0 70.57 102.37 2.81 0.079 1.15 -8 10 3 71.42 103.80 2.80 0.080 0.88 -8 5 3 84.62 58.57 2.77 0.060 1.05 -6 9 1 162.21 206.89 2.77 0.112 1.10 0 6 10 0.68 11.87 2.76 0.027 0.94 5 1 5 368.77 304.21 2.75 0.136 1.36 -2 1 3 34.51 46.76 2.75 0.053 2.78 0 13 3 3.30 18.31 2.74 0.033 1.02 6 1 2 203.78 166.15 2.72 0.101 1.48 -1 1 3 17.24 25.27 2.71 0.039 3.19 4 0 0 214.65 173.76 2.70 0.103 2.36 -11 5 5 27.66 55.14 2.69 0.058 0.77 0 16 5 60.13 4.01 2.68 0.016 0.80 3 16 5 42.28 0.98 2.68 0.008 0.77 -3 13 2 365.06 291.47 2.67 0.133 1.00 2 2 1 2654.61 3161.52 2.65 0.439 3.61 10 1 6 99.44 67.85 2.64 0.064 0.81 0 8 12 66.84 99.40 2.62 0.078 0.77 1 6 5 60.93 81.05 2.62 0.070 1.51 -4 11 7 17.57 0.12 2.61 0.003 0.90 -7 7 4 85.42 112.35 2.60 0.083 1.04 0 10 2 3.08 11.18 2.58 0.026 1.34 -5 15 2 54.46 91.77 2.56 0.075 0.82 -4 11 8 1.98 19.39 2.55 0.034 0.85 10 9 1 12.00 49.14 2.52 0.055 0.80 Bond lengths and angles B1 - Distance Angles O1 1.4545 (0.0020) O6 1.4701 (0.0019) 109.93 (0.11) O4 1.4715 (0.0019) 108.62 (0.13) 110.58 (0.11) O3 1.4763 (0.0019) 110.76 (0.11) 110.05 (0.13) 106.84 (0.11) B1 - O1 O6 O4 B2 - Distance Angles O7 1.3489 (0.0020) O1 1.3639 (0.0019) 118.37 (0.14) O2 1.3841 (0.0020) 120.87 (0.13) 120.72 (0.14) B2 - O7 O1 B3 - Distance Angles O3 1.3542 (0.0020) O8 1.3579 (0.0020) 123.23 (0.14) O2 1.3850 (0.0020) 120.95 (0.14) 115.81 (0.13) B3 - O3 O8 B4 - Distance Angles O9 1.3551 (0.0020) O4 1.3581 (0.0019) 121.41 (0.14) O5 1.3744 (0.0020) 117.94 (0.13) 120.65 (0.14) B4 - O9 O4 B5 - Distance Angles O6 1.3544 (0.0020) O10 1.3593 (0.0020) 123.59 (0.14) O5 1.3827 (0.0020) 121.22 (0.14) 115.18 (0.13) B5 - O6 O10 O1 - Distance Angles B2 1.3639 (0.0019) B1 1.4545 (0.0020) 121.53 (0.13) O1 - B2 O2 - Distance Angles B2 1.3841 (0.0020) B3 1.3850 (0.0020) 118.32 (0.12) O2 - B2 O3 - Distance Angles B3 1.3542 (0.0020) B1 1.4763 (0.0019) 121.70 (0.12) O3 - B3 O4 - Distance Angles B4 1.3581 (0.0019) B1 1.4715 (0.0019) 121.79 (0.12) O4 - B4 O5 - Distance Angles B4 1.3744 (0.0020) B5 1.3827 (0.0020) 119.47 (0.12) O5 - B4 O6 - Distance Angles B5 1.3544 (0.0020) B1 1.4701 (0.0019) 122.06 (0.12) O6 - B5 O7 - Distance Angles B2 1.3489 (0.0020) H7 0.8400 109.47 O7 - B2 O8 - Distance Angles B3 1.3579 (0.0020) H8 0.8400 109.47 O8 - B3 O9 - Distance Angles B4 1.3551 (0.0020) H9 0.8400 109.47 O9 - B4 O10 - Distance Angles B5 1.3593 (0.0020) H10 0.8400 109.47 O10 - B5 C1_a - Distance Angles N1_a 1.5036 (0.0048) C5_a 1.5330 (0.0040) 110.18 (0.46) C2_a 1.5512 (0.0048) 110.20 (0.47) 105.54 (0.35) H1_a 1.0000 110.28 110.28 110.28 C1_a - N1_a C5_a C2_a C2_a - Distance Angles C3_a 1.5389 (0.0051) C1_a 1.5512 (0.0048) 105.78 (0.33) H2A_a 0.9900 110.58 110.58 H2B_a 0.9900 110.58 110.58 108.73 C2_a - C3_a C1_a H2A_a C3_a - Distance Angles C4_a 1.4920 (0.0047) C2_a 1.5389 (0.0051) 105.25 (0.31) H3A_a 0.9900 110.69 110.69 H3B_a 0.9900 110.69 110.69 108.80 C3_a - C4_a C2_a H3A_a C4_a - Distance Angles C3_a 1.4920 (0.0047) C5_a 1.5287 (0.0063) 104.53 (0.29) H4A_a 0.9900 110.84 110.84 H4B_a 0.9900 110.84 110.84 108.89 C4_a - C3_a C5_a H4A_a C5_a - Distance Angles C4_a 1.5287 (0.0063) C1_a 1.5330 (0.0039) 102.87 (0.39) H5A_a 0.9900 111.19 111.19 H5B_a 0.9900 111.19 111.19 109.12 C5_a - C4_a C1_a H5A_a N1_a - Distance Angles C1_a 1.5036 (0.0048) H1A_a 0.9100 109.47 H1B_a 0.9100 109.47 109.47 H1C_a 0.9100 109.47 109.47 109.47 N1_a - C1_a H1A_a H1B_a C21_b - Distance Angles C25_b 1.4722 (0.0135) N21_b 1.4861 (0.0139) 114.22 (1.65) C22_b 1.5427 (0.0139) 109.45 (1.15) 108.53 (1.45) H21_b 1.0000 108.16 108.16 108.16 C21_b - C25_b N21_b C22_b C22_b - Distance Angles C23_b 1.5202 (0.0146) C21_b 1.5427 (0.0139) 101.75 (1.14) H22A_b 0.9900 111.42 111.42 H22B_b 0.9900 111.42 111.42 109.27 C22_b - C23_b C21_b H22A_b C23_b - Distance Angles C24_b 1.4407 (0.0135) C22_b 1.5202 (0.0146) 110.50 (1.08) H23A_b 0.9900 109.55 109.55 H23B_b 0.9900 109.55 109.55 108.10 C23_b - C24_b C22_b H23A_b C24_b - Distance Angles C23_b 1.4407 (0.0135) C25_b 1.5165 (0.0150) 108.79 (0.96) H24A_b 0.9900 109.93 109.93 H24B_b 0.9900 109.93 109.93 108.32 C24_b - C23_b C25_b H24A_b C25_b - Distance Angles C21_b 1.4722 (0.0135) C24_b 1.5165 (0.0150) 104.75 (1.13) H25A_b 0.9900 110.80 110.80 H25B_b 0.9900 110.80 110.80 108.87 C25_b - C21_b C24_b H25A_b N21_b - Distance Angles C21_b 1.4861 (0.0139) H21A_b 0.9100 109.47 H21B_b 0.9100 109.47 109.47 H21C_b 0.9100 109.47 109.47 109.47 N21_b - C21_b H21A_b H21B_b Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.89 2.7241(15) 169.2 O7-H7...O9_$1 0.84 1.98 2.8194(15) 178.2 O8-H8...O6_$2 0.84 1.82 2.6603(15) 174.1 O9-H9...O4_$3 0.84 1.90 2.7311(14) 171.0 O10-H10...O3_$4 0.91 2.00 2.902(12) 168.9 N1_a-H1A_a...O1_$5 0.91 2.22 3.103(8) 162.0 N1_a-H1B_a...O10_$6 0.91 2.23 3.108(10) 161.7 N1_a-H1C_a...O8_$7 0.91 2.39 3.056(8) 129.8 N1_a-H1C_a...O2_$7 0.91 2.00 2.89(4) 166.8 N21_b-H21A_b...O1_$5 0.91 2.40 3.29(2) 166.0 N21_b-H21B_b...O10_$6 0.91 2.14 3.03(3) 165.5 N21_b-H21C_b...O8_$7 0.91 2.43 3.12(2) 132.2 N21_b-H21C_b...O2_$7 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)