+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s93 started at 16:57:28 on 09-Feb-2006 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s93 in I-4 CELL 0.71073 27.5929 27.5929 7.0313 90.000 90.000 90.000 ZERR 10.00 0.0020 0.0020 0.0005 0.000 0.000 0.000 LATT -2 SYMM - X, - Y, Z SYMM Y, - X, - Z SYMM - Y, X, - Z SFAC C H B P UNIT 240 280 30 10 V = 5353.41 F(000) = 2020.0 Mu = 0.14 mm-1 Cell Wt = 3798.64 Rho = 1.178 MERG 2 OMIT -3.00 55.00 OMIT 5 0 1 OMIT 0 5 1 OMIT 6 3 1 OMIT -4 3 1 EXTI 0.11751 SHEL 7 0.77 delu simu EQIV $1 -X+1, -Y+1, Z EQIV $2 Y, -X+1, -Z EQIV $3 -Y+1, X, -Z DFIX 21 0.04 B1 B2 B1 B3 B2 B3 B11 B12 B11 B11_$1 DFIX 21 0.04 B101 B102 B101 B103 B102 B103 FREE B11 B11_$2 FREE B11 B11_$3 FREE B11 B12_$2 FREE B12 B11_$2 FREE B12 B11_$3 DFIX 20.55 0.03 B11 H13A B12 H13A DFIX 20.55 0.03 B1 H4A B2 H4A B1 H5A B3 H5A DFIX 20.55 0.03 B101 H104 B102 H104 B101 H105 B103 H105 dfix 1.97 0.03 B102 H105 B2 H5A B103 H104 B3 H4A FMAP 2 PLAN 10 SIZE 0.08 0.10 0.42 ACTA BOND $H WGHT 0.20000 L.S. 40 TEMP -153.00 FVAR 0.36934 1.66726 0.44631 MOLE 1 C1 1 0.705694 0.655932 0.098527 11.00000 0.06522 0.01987 = 0.03378 -0.00051 -0.01340 0.02115 C2 1 0.742252 0.653672 -0.037120 11.00000 0.07158 0.04124 = 0.03545 -0.00537 -0.01078 0.03321 AFIX 43 H2 2 0.761984 0.625547 -0.045854 11.00000 -1.20000 AFIX 0 C3 1 0.750093 0.692199 -0.159704 11.00000 0.09498 0.03739 = 0.03082 -0.00707 -0.00377 0.01948 AFIX 43 H3 2 0.775888 0.691131 -0.249093 11.00000 -1.20000 AFIX 0 C4 1 0.719170 0.733340 -0.150439 11.00000 0.09618 0.03710 = 0.03450 0.00437 -0.01581 0.01573 AFIX 43 H4 2 0.723706 0.759333 -0.237233 11.00000 -1.20000 AFIX 0 C5 1 0.683058 0.735915 -0.018324 11.00000 0.07699 0.03252 = 0.04355 -0.00086 -0.01773 0.02316 AFIX 43 H5 2 0.663174 0.763966 -0.011346 11.00000 -1.20000 AFIX 0 C6 1 0.675209 0.696969 0.107949 11.00000 0.05815 0.03205 = 0.04393 0.00382 -0.01198 0.02627 AFIX 43 H6 2 0.649672 0.698335 0.198409 11.00000 -1.20000 AFIX 0 C7 1 0.645629 0.613009 0.401015 11.00000 0.04909 0.04526 = 0.03861 0.00685 -0.02203 0.01106 C8 1 0.646924 0.650671 0.533513 11.00000 0.04326 0.05742 = 0.04338 -0.00101 -0.01440 0.01824 AFIX 43 H8 2 0.674481 0.671223 0.540950 11.00000 -1.20000 AFIX 0 C9 1 0.607719 0.658013 0.654673 11.00000 0.04898 0.08647 = 0.04899 -0.00202 -0.01839 0.03132 AFIX 43 H9 2 0.608085 0.684248 0.742158 11.00000 -1.20000 AFIX 0 C10 1 0.567695 0.626779 0.647876 11.00000 0.05305 0.10728 = 0.05670 0.02348 -0.01411 0.01535 AFIX 43 H10 2 0.540844 0.631878 0.730039 11.00000 -1.20000 AFIX 0 C11 1 0.567504 0.588459 0.520791 11.00000 0.05261 0.09152 = 0.07628 0.03632 -0.01858 -0.00187 AFIX 43 H11 2 0.541084 0.566382 0.520951 11.00000 -1.20000 AFIX 0 C12 1 0.605016 0.581819 0.394062 11.00000 0.06516 0.05563 = 0.05953 0.02458 -0.02814 0.00253 AFIX 43 H12 2 0.603598 0.556484 0.302744 11.00000 -1.20000 AFIX 0 C13 1 0.690793 0.552747 0.100887 11.00000 0.08522 0.02061 = 0.03753 -0.00413 -0.03158 0.00510 C14 1 0.653057 0.553719 -0.032858 11.00000 0.11447 0.04016 = 0.05370 -0.00062 -0.05379 0.01308 AFIX 43 H14 2 0.632317 0.581093 -0.042385 11.00000 -1.20000 AFIX 0 C15 1 0.646677 0.514360 -0.149695 11.00000 0.14434 0.03649 = 0.05560 0.00363 -0.05859 -0.00943 AFIX 43 H15 2 0.620306 0.514116 -0.236550 11.00000 -1.20000 AFIX 0 C16 1 0.678728 0.473829 -0.143682 11.00000 0.12965 0.02721 = 0.04909 0.00047 -0.03512 -0.02401 AFIX 43 H16 2 0.674785 0.447462 -0.229172 11.00000 -1.20000 AFIX 0 C17 1 0.715537 0.473740 -0.011189 11.00000 0.10624 0.02064 = 0.03683 0.00162 -0.02199 -0.00563 AFIX 43 H17 2 0.736437 0.446450 -0.003520 11.00000 -1.20000 AFIX 0 C18 1 0.722857 0.512502 0.111344 11.00000 0.07840 0.01853 = 0.03925 -0.00049 -0.01310 -0.00017 AFIX 43 H18 2 0.748757 0.512145 0.200349 11.00000 -1.20000 AFIX 0 C19 1 0.749868 0.596445 0.399275 11.00000 0.05646 0.02654 = 0.03173 -0.00775 -0.02070 0.02041 C20 1 0.748760 0.560061 0.536453 11.00000 0.05982 0.03181 = 0.03008 -0.00048 -0.01646 0.01594 AFIX 43 H20 2 0.721055 0.539864 0.548786 11.00000 -1.20000 AFIX 0 C21 1 0.788785 0.553474 0.656054 11.00000 0.07263 0.04180 = 0.02527 0.00090 -0.01307 0.02437 AFIX 43 H21 2 0.788598 0.528146 0.747568 11.00000 -1.20000 AFIX 0 C22 1 0.828646 0.583735 0.641471 11.00000 0.06656 0.03983 = 0.03375 -0.00774 -0.01823 0.02120 AFIX 43 H22 2 0.855497 0.579386 0.724301 11.00000 -1.20000 AFIX 0 C23 1 0.829522 0.619769 0.508648 11.00000 0.05876 0.04174 = 0.04040 -0.01470 -0.01487 0.01141 AFIX 43 H23 2 0.857139 0.640203 0.499836 11.00000 -1.20000 AFIX 0 C24 1 0.790879 0.627062 0.386565 11.00000 0.07382 0.02212 = 0.03925 -0.00630 -0.01795 0.01402 AFIX 43 H24 2 0.791870 0.652381 0.295090 11.00000 -1.20000 AFIX 0 P1 4 0.697793 0.604646 0.250246 11.00000 0.06201 0.02172 = 0.03370 0.00028 -0.02065 0.01496 MOLE 2 C31 1 0.948118 0.513030 0.901217 11.00000 0.05920 0.03215 = 0.03858 0.00113 0.00128 -0.00236 C32 1 0.951902 0.551545 1.030913 11.00000 0.05270 0.05435 = 0.04293 -0.00355 0.00055 -0.02724 AFIX 43 H32 2 0.980299 0.570963 1.036413 11.00000 -1.20000 AFIX 0 C33 1 0.912968 0.560409 1.150760 11.00000 0.05650 0.03876 = 0.03644 -0.00441 0.00186 -0.01193 AFIX 43 H33 2 0.913937 0.586999 1.236504 11.00000 -1.20000 AFIX 0 C34 1 0.871786 0.529837 1.145321 11.00000 0.05280 0.01992 = 0.03626 0.00389 -0.00502 -0.01170 AFIX 43 H34 2 0.845726 0.535488 1.230787 11.00000 -1.20000 AFIX 0 C35 1 0.868962 0.492223 1.018622 11.00000 0.05049 0.01982 = 0.03655 -0.00070 -0.00591 0.00194 AFIX 43 H35 2 0.840964 0.472203 1.015403 11.00000 -1.20000 AFIX 0 C36 1 0.907056 0.483528 0.895423 11.00000 0.06872 0.02706 = 0.03551 -0.00076 -0.00460 0.00624 AFIX 43 H36 2 0.905279 0.457540 0.807075 11.00000 -1.20000 AFIX 0 P31 4 1.000000 0.500000 0.750000 10.25000 0.07136 0.07136 = 0.03687 0.00000 0.00000 0.00000 MOLE 3 PART 1 B1 3 0.899119 0.711177 -0.171163 31.00000 0.02761 0.13497 = 0.01560 0.00128 0.00081 0.00906 AFIX 23 H1A 2 0.898414 0.742640 -0.238783 31.00000 -1.20000 H1B 2 0.901427 0.682620 -0.255917 31.00000 -1.20000 AFIX 0 B2 3 0.865572 0.706038 0.015210 31.00000 0.03708 0.14250 = 0.05998 0.02715 0.01689 0.05965 AFIX 23 H2A 2 0.849820 0.674394 0.039339 31.00000 -1.20000 H2B 2 0.846791 0.734735 0.056565 31.00000 -1.20000 AFIX 0 B3 3 0.928979 0.708972 0.028655 31.00000 0.03738 0.05710 = 0.01992 0.02513 -0.00086 0.00734 AFIX 23 H3A 2 0.943859 0.739259 0.076483 31.00000 -1.20000 H3B 2 0.946890 0.678877 0.059245 31.00000 -1.20000 AFIX 0 H4A 2 0.868611 0.710952 -0.117143 31.00000 -1.50000 H5A 2 0.928905 0.713571 -0.100402 31.00000 -1.50000 PART 2 B101 3 0.872389 0.689409 0.049554 -31.00000 0.04283 0.15465 = 0.04834 0.05515 -0.02310 -0.00251 AFIX 23 H10A 2 0.858106 0.658985 0.098835 -31.00000 -1.20000 H10B 2 0.850212 0.717541 0.057418 -31.00000 -1.20000 AFIX 0 B102 3 0.903271 0.685205 -0.132625 -31.00000 0.04436 0.06943 = 0.07402 -0.01643 -0.01035 0.02870 AFIX 23 H10C 2 0.901248 0.711665 -0.227386 -31.00000 -1.20000 H10D 2 0.909226 0.652493 -0.185533 -31.00000 -1.20000 AFIX 0 B103 3 0.927695 0.699221 0.100854 -31.00000 0.06417 0.03763 = 0.12108 0.03647 -0.07589 -0.02076 AFIX 23 H10E 2 0.945904 0.673684 0.169225 -31.00000 -1.20000 H10F 2 0.937914 0.732947 0.127308 -31.00000 -1.20000 AFIX 0 H104 2 0.875242 0.696902 -0.082493 -31.00000 -1.50000 H105 2 0.900527 0.686675 0.144005 -31.00000 -1.50000 MOLE 4 PART 0 B11 3 0.530521 0.505260 0.015200 10.50000 0.06603 0.05125 = 0.05144 -0.00426 -0.01143 0.00165 AFIX 23 H11A 2 0.552409 0.478244 -0.019535 10.50000 -1.20000 H11B 2 0.542103 0.538044 -0.019535 10.50000 -1.20000 AFIX 0 B12 3 0.500000 0.500000 0.189153 10.25000 0.21862 0.03011 = 0.01817 0.00000 0.00000 -0.01322 AFIX 23 H12A 2 0.505100 0.470405 0.266195 10.25000 -1.20000 H12B 2 0.494900 0.529595 0.266196 10.25000 -1.20000 AFIX 0 H13A 2 0.530697 0.507520 0.147311 10.50000 -1.50000 HKLF 4 Covalent radii and connectivity table for s93 in I-4 C 0.770 H 0.320 B 0.820 P 1.100 C1 - C2 C6 P1 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 - C8 C12 P1 C8 - C9 C7 C9 - C8 C10 C10 - C11 C9 C11 - C12 C10 C12 - C11 C7 C13 - C14 C18 P1 C14 - C15 C13 C15 - C14 C16 C16 - C17 C15 C17 - C16 C18 C18 - C17 C13 C19 - C20 C24 P1 C20 - C19 C21 C21 - C22 C20 C22 - C23 C21 C23 - C22 C24 C24 - C23 C19 P1 - C1 C13 C19 C7 C31 - C36 C32 P31 C32 - C33 C31 C33 - C32 C34 C34 - C35 C33 C35 - C34 C36 C36 - C35 C31 P31 - C31_$6 C31_$4 C31 C31_$5 B1_a - B2_a B3_a B2_a - B1_a B3_a B3_a - B1_a B2_a B101_b - B102_b B103_b B102_b - B101_b B103_b B103_b - B101_b B102_b B11 - B12 B11_$1 B12 - B11_$1 B11 Operators for generating equivalent atoms: $1 -x+1, -y+1, z $2 y, -x+1, -z $3 -y+1, x, -z $4 -x+2, -y+1, z $5 y+1/2, -x+3/2, -z+3/2 $6 -y+3/2, x-1/2, -z+3/2 15089 Reflections read, of which 77 rejected -35 =< h =< 35, -33 =< k =< 35, -9 =< l =< 8, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 20 20 0 283.25 11.36 3 61.25 17 25 0 75.91 6.23 2 34.88 -10 28 0 106.70 7.91 2 64.96 -11 29 0 40.87 4.60 2 31.11 -9 29 0 35.35 4.81 2 25.90 10 30 0 27.81 3.79 2 19.51 5 31 0 153.63 9.65 2 87.71 7 31 0 113.41 8.30 2 73.85 6 32 0 178.21 9.96 2 54.60 -3 6 1 2256.51 45.82 2 4547.04 -1 7 2 175.88 2.87 3 1886.19 1 21 2 1.21 0.29 3 3.03 -8 26 2 149.66 7.95 2 115.79 8 28 2 144.52 9.78 2 58.96 15 0 3 436.41 13.82 2 447.15 7 6 3 2669.20 94.79 2 1857.43 -6 7 3 3215.78 69.01 3 1275.52 18 19 3 42.53 3.77 2 19.99 -2 25 3 38.89 4.61 2 24.04 0 31 3 24.29 4.22 2 22.30 13 9 4 518.49 11.11 3 1097.90 -15 11 4 35.54 2.95 2 17.32 -16 12 4 305.24 12.70 2 75.84 -9 23 4 107.57 8.14 2 47.17 2 21 5 177.43 9.64 2 66.33 10 15 7 144.70 9.40 2 49.73 26 Inconsistent equivalents 5893 Unique reflections, of which 0 suppressed R(int) = 0.0862 R(sigma) = 0.1024 Friedel opposites not merged Maximum memory for data reduction = 5013 / 70541 Special position constraints for P31 x = 1.0000 y = 0.5000 z = 0.7500 U22 = 1.0 * U11 U23 = 0 U13 = 0 U12 = 0 sof = 0.25000 Input constraints retained (at least in part) for sof Special position constraints for B12 x = 0.5000 y = 0.5000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof 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 = 6125 / 467723 wR2 = 0.3677 before cycle 1 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 1.0245 0.9170 0.1075 0.0300 DFIX B101_b H105_b 1.4921 1.6673 -0.1752 0.0400 DFIX B11 B12 1.5429 1.6673 -0.1244 0.0400 DFIX B101_b B102_b 1.8163 1.6673 0.1490 0.0400 DFIX B102_b B103_b -0.1526 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.070 0.000 0.000 0.000 0.000 0.000 0.007 0.025 0.000 0.000 GooF = S = 1.405; Restrained GooF = 1.386 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36918 0.00325 -0.048 OSF 2 1.66653 0.01435 -0.051 FVAR 2 3 0.43899 0.02130 -0.344 FVAR 3 4 0.11718 0.01104 -0.030 EXTI Mean shift/esd = 0.039 Maximum = -0.344 for FVAR 3 Max. shift = 0.035 A for H5A_a Max. dU =-0.001 for B1_a Least-squares cycle 2 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3676 before cycle 2 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 1.0255 0.9166 0.1089 0.0300 DFIX B101_b H105_b 1.4913 1.6665 -0.1752 0.0400 DFIX B11 B12 1.8143 1.6665 0.1478 0.0400 DFIX B102_b B103_b -0.1536 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.070 0.000 0.000 0.000 0.000 0.000 0.007 0.025 0.000 0.000 GooF = S = 1.405; Restrained GooF = 1.386 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36919 0.00325 0.003 OSF 2 1.66597 0.01436 -0.039 FVAR 2 3 0.43526 0.02116 -0.176 FVAR 3 4 0.11713 0.01101 -0.004 EXTI Mean shift/esd = 0.021 Maximum = 0.224 for y H5A_a Max. shift = 0.024 A for H5A_a Max. dU =-0.001 for B1_a Least-squares cycle 3 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3676 before cycle 3 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 1.0249 0.9163 0.1087 0.0300 DFIX B101_b H105_b 1.4906 1.6660 -0.1754 0.0400 DFIX B11 B12 1.8118 1.6660 0.1459 0.0400 DFIX B102_b B103_b -0.1540 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.405; Restrained GooF = 1.386 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36917 0.00325 -0.008 OSF 2 1.66630 0.01435 0.023 FVAR 2 3 0.43542 0.02114 0.007 FVAR 3 4 0.11702 0.01101 -0.011 EXTI Mean shift/esd = 0.010 Maximum = 0.087 for y H5A_a Max. shift = 0.009 A for H5A_a Max. dU = 0.000 for B103_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3676 before cycle 4 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 1.0258 0.9165 0.1094 0.0300 DFIX B101_b H105_b 1.4902 1.6663 -0.1761 0.0400 DFIX B11 B12 1.8118 1.6663 0.1455 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.070 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.386 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36914 0.00325 -0.007 OSF 2 1.66655 0.01436 0.017 FVAR 2 3 0.43499 0.02111 -0.020 FVAR 3 4 0.11694 0.01100 -0.007 EXTI Mean shift/esd = 0.006 Maximum = -0.043 for x H5A_a Max. shift = 0.005 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 5 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3676 before cycle 5 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 1.0258 0.9166 0.1092 0.0300 DFIX B101_b H105_b 1.4903 1.6665 -0.1763 0.0400 DFIX B11 B12 1.8113 1.6665 0.1447 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.386 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36912 0.00325 -0.008 OSF 2 1.66672 0.01437 0.012 FVAR 2 3 0.43454 0.02111 -0.021 FVAR 3 4 0.11685 0.01099 -0.008 EXTI Mean shift/esd = 0.005 Maximum = 0.032 for x B103_b Max. shift = 0.003 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 6 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3676 before cycle 6 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint 1.0261 0.9167 0.1094 0.0300 DFIX B101_b H105_b 1.4903 1.6667 -0.1764 0.0400 DFIX B11 B12 1.8109 1.6667 0.1442 0.0400 DFIX B102_b B103_b -0.1540 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.070 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.386 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36910 0.00324 -0.007 OSF 2 1.66674 0.01437 0.001 FVAR 2 3 0.43421 0.02109 -0.016 FVAR 3 4 0.11678 0.01099 -0.006 EXTI Mean shift/esd = 0.003 Maximum = 0.028 for x B103_b Max. shift = 0.002 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 7 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 7 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint 1.0261 0.9167 0.1094 0.0300 DFIX B101_b H105_b 1.4903 1.6667 -0.1764 0.0400 DFIX B11 B12 1.8105 1.6667 0.1438 0.0400 DFIX B102_b B103_b -0.1540 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.386 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36908 0.00324 -0.006 OSF 2 1.66680 0.01437 0.004 FVAR 2 3 0.43402 0.02109 -0.009 FVAR 3 4 0.11672 0.01098 -0.006 EXTI Mean shift/esd = 0.003 Maximum = -0.022 for U22 B3_a Max. shift = 0.001 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 8 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 8 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint 1.0263 0.9167 0.1096 0.0300 DFIX B101_b H105_b 1.4904 1.6668 -0.1764 0.0400 DFIX B11 B12 1.8103 1.6668 0.1435 0.0400 DFIX B102_b B103_b -0.1540 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.386 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36906 0.00324 -0.004 OSF 2 1.66681 0.01437 0.001 FVAR 2 3 0.43379 0.02108 -0.011 FVAR 3 4 0.11668 0.01098 -0.004 EXTI Mean shift/esd = 0.002 Maximum = 0.020 for x B103_b Max. shift = 0.001 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 9 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 9 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint 1.0263 0.9167 0.1095 0.0300 DFIX B101_b H105_b 1.4904 1.6668 -0.1764 0.0400 DFIX B11 B12 1.8100 1.6668 0.1432 0.0400 DFIX B102_b B103_b -0.1540 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.386 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36905 0.00324 -0.005 OSF 2 1.66684 0.01437 0.002 FVAR 2 3 0.43365 0.02108 -0.007 FVAR 3 4 0.11663 0.01097 -0.004 EXTI Mean shift/esd = 0.002 Maximum = -0.015 for U22 B3_a Max. shift = 0.001 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 10 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 10 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 10 Observed Target Error Sigma Restraint 1.0264 0.9168 0.1096 0.0300 DFIX B101_b H105_b 1.4904 1.6668 -0.1765 0.0400 DFIX B11 B12 1.8099 1.6668 0.1430 0.0400 DFIX B102_b B103_b -0.1540 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.386 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36904 0.00324 -0.003 OSF 2 1.66684 0.01437 0.000 FVAR 2 3 0.43348 0.02108 -0.008 FVAR 3 4 0.11660 0.01097 -0.003 EXTI Mean shift/esd = 0.001 Maximum = 0.014 for x B103_b Max. shift = 0.001 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 11 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 11 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 11 Observed Target Error Sigma Restraint 1.0264 0.9168 0.1096 0.0300 DFIX B101_b H105_b 1.4904 1.6668 -0.1765 0.0400 DFIX B11 B12 1.8097 1.6668 0.1429 0.0400 DFIX B102_b B103_b -0.1540 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.385 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36903 0.00324 -0.003 OSF 2 1.66686 0.01437 0.001 FVAR 2 3 0.43338 0.02108 -0.005 FVAR 3 4 0.11657 0.01097 -0.003 EXTI Mean shift/esd = 0.001 Maximum = -0.010 for U22 B3_a Max. shift = 0.001 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 12 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 12 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 12 Observed Target Error Sigma Restraint 1.0264 0.9168 0.1097 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8096 1.6669 0.1427 0.0400 DFIX B102_b B103_b -0.1540 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.385 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36903 0.00324 -0.002 OSF 2 1.66686 0.01437 0.000 FVAR 2 3 0.43326 0.02107 -0.006 FVAR 3 4 0.11655 0.01097 -0.002 EXTI Mean shift/esd = 0.001 Maximum = 0.009 for x B103_b Max. shift = 0.001 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 13 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 13 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 13 Observed Target Error Sigma Restraint 1.0264 0.9168 0.1097 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8095 1.6669 0.1426 0.0400 DFIX B102_b B103_b -0.1540 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.385 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36902 0.00324 -0.002 OSF 2 1.66687 0.01437 0.001 FVAR 2 3 0.43319 0.02107 -0.003 FVAR 3 4 0.11653 0.01096 -0.002 EXTI Mean shift/esd = 0.001 Maximum = -0.007 for U22 B3_a Max. shift = 0.000 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 14 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 14 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 14 Observed Target Error Sigma Restraint 1.0265 0.9168 0.1097 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8094 1.6669 0.1425 0.0400 DFIX B102_b B103_b -0.1540 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.386 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36901 0.00324 -0.002 OSF 2 1.66688 0.01437 0.000 FVAR 2 3 0.43311 0.02107 -0.004 FVAR 3 4 0.11651 0.01096 -0.002 EXTI Mean shift/esd = 0.001 Maximum = -0.007 for z B103_b Max. shift = 0.000 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 15 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 15 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 15 Observed Target Error Sigma Restraint 1.0265 0.9168 0.1097 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8093 1.6669 0.1424 0.0400 DFIX B102_b B103_b -0.1540 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.385 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36901 0.00324 -0.001 OSF 2 1.66688 0.01437 0.001 FVAR 2 3 0.43306 0.02107 -0.002 FVAR 3 4 0.11650 0.01096 -0.001 EXTI Mean shift/esd = 0.001 Maximum = -0.005 for U22 B3_a Max. shift = 0.000 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 16 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 16 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 16 Observed Target Error Sigma Restraint 1.0265 0.9168 0.1097 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8093 1.6669 0.1424 0.0400 DFIX B102_b B103_b -0.1540 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.385 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36900 0.00324 -0.002 OSF 2 1.66688 0.01437 0.000 FVAR 2 3 0.43300 0.02107 -0.003 FVAR 3 4 0.11648 0.01096 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.005 for z B103_b Max. shift = 0.000 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 17 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 17 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 17 Observed Target Error Sigma Restraint 1.0265 0.9168 0.1097 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8092 1.6669 0.1423 0.0400 DFIX B102_b B103_b -0.1540 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.386 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36900 0.00324 -0.001 OSF 2 1.66689 0.01437 0.000 FVAR 2 3 0.43297 0.02107 -0.002 FVAR 3 4 0.11647 0.01096 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.003 for U22 B3_a Max. shift = 0.000 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 18 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 18 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 18 Observed Target Error Sigma Restraint 1.0265 0.9168 0.1097 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8092 1.6669 0.1423 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 18 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.386 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36900 0.00324 0.000 OSF 2 1.66689 0.01437 0.000 FVAR 2 3 0.43293 0.02107 -0.002 FVAR 3 4 0.11647 0.01096 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.003 for z B103_b Max. shift = 0.000 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 19 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 19 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 19 Observed Target Error Sigma Restraint 1.0265 0.9168 0.1097 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8091 1.6669 0.1422 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 19 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.386 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36900 0.00324 -0.001 OSF 2 1.66689 0.01437 0.000 FVAR 2 3 0.43291 0.02107 -0.001 FVAR 3 4 0.11646 0.01096 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for U22 B3_a Max. shift = 0.000 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 20 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 20 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 20 Observed Target Error Sigma Restraint 1.0265 0.9168 0.1097 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8091 1.6669 0.1422 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 20 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.386 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36900 0.00324 0.000 OSF 2 1.66689 0.01437 0.000 FVAR 2 3 0.43288 0.02107 -0.001 FVAR 3 4 0.11646 0.01096 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for z B103_b Max. shift = 0.000 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 21 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 21 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 21 Observed Target Error Sigma Restraint 1.0265 0.9168 0.1097 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8091 1.6669 0.1422 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 21 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.386 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36900 0.00324 0.000 OSF 2 1.66689 0.01437 0.000 FVAR 2 3 0.43287 0.02107 -0.001 FVAR 3 4 0.11646 0.01096 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for U22 B3_a Max. shift = 0.000 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 22 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 22 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 22 Observed Target Error Sigma Restraint 1.0265 0.9168 0.1098 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8091 1.6669 0.1422 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 22 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.386 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36900 0.00324 0.000 OSF 2 1.66689 0.01437 0.000 FVAR 2 3 0.43285 0.02106 -0.001 FVAR 3 4 0.11646 0.01096 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for z B103_b Max. shift = 0.000 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 23 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 23 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 23 Observed Target Error Sigma Restraint 1.0265 0.9168 0.1097 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8090 1.6669 0.1422 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 23 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.386 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36899 0.00324 0.000 OSF 2 1.66690 0.01437 0.000 FVAR 2 3 0.43284 0.02106 -0.001 FVAR 3 4 0.11645 0.01096 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for U22 B3_a Max. shift = 0.000 A for H5A_a Max. dU = 0.000 for B3_a Least-squares cycle 24 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 24 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 24 Observed Target Error Sigma Restraint 1.0265 0.9168 0.1098 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8090 1.6669 0.1421 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 24 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.385 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36899 0.00324 0.000 OSF 2 1.66690 0.01437 0.000 FVAR 2 3 0.43282 0.02106 -0.001 FVAR 3 4 0.11645 0.01096 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for z B103_b Max. shift = 0.000 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 25 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 25 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 25 Observed Target Error Sigma Restraint 1.0265 0.9168 0.1098 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8090 1.6669 0.1421 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 25 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.386 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36899 0.00324 0.000 OSF 2 1.66690 0.01437 0.000 FVAR 2 3 0.43282 0.02106 0.000 FVAR 3 4 0.11645 0.01096 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for U12 B3_a Max. shift = 0.000 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 26 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 26 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 26 Observed Target Error Sigma Restraint 1.0266 0.9168 0.1098 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8090 1.6669 0.1421 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 26 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.385 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36899 0.00324 0.000 OSF 2 1.66690 0.01437 0.000 FVAR 2 3 0.43281 0.02106 0.000 FVAR 3 4 0.11645 0.01096 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for x B103_b Max. shift = 0.000 A for H5A_a Max. dU = 0.000 for B3_a Least-squares cycle 27 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 27 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 27 Observed Target Error Sigma Restraint 1.0266 0.9168 0.1098 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8090 1.6669 0.1421 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 27 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.385 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36899 0.00324 0.000 OSF 2 1.66690 0.01437 0.000 FVAR 2 3 0.43280 0.02106 0.000 FVAR 3 4 0.11645 0.01096 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for z B103_b Max. shift = 0.000 A for H5A_a Max. dU = 0.000 for B103_b Least-squares cycle 28 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 28 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 28 Observed Target Error Sigma Restraint 1.0266 0.9168 0.1098 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8090 1.6669 0.1421 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 28 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.385 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36899 0.00324 0.000 OSF 2 1.66690 0.01437 0.000 FVAR 2 3 0.43280 0.02106 0.000 FVAR 3 4 0.11645 0.01096 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y P1 Max. shift = 0.000 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 29 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 29 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 29 Observed Target Error Sigma Restraint 1.0266 0.9168 0.1098 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8090 1.6669 0.1421 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 29 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.385 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36899 0.00324 0.000 OSF 2 1.66690 0.01437 0.000 FVAR 2 3 0.43279 0.02106 0.000 FVAR 3 4 0.11645 0.01096 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x B103_b Max. shift = 0.000 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 30 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 30 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 30 Observed Target Error Sigma Restraint 1.0266 0.9168 0.1098 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8090 1.6669 0.1421 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 30 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.385 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36899 0.00324 0.000 OSF 2 1.66690 0.01437 0.000 FVAR 2 3 0.43279 0.02106 0.000 FVAR 3 4 0.11644 0.01096 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H105_b Max. dU = 0.000 for B2_a Least-squares cycle 31 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 31 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 31 Observed Target Error Sigma Restraint 1.0266 0.9168 0.1098 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8090 1.6669 0.1421 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 31 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.385 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36899 0.00324 0.000 OSF 2 1.66690 0.01437 0.000 FVAR 2 3 0.43279 0.02106 0.000 FVAR 3 4 0.11644 0.01096 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H5A_a Max. dU = 0.000 for B3_a Least-squares cycle 32 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 32 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 32 Observed Target Error Sigma Restraint 1.0266 0.9168 0.1098 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8090 1.6669 0.1421 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 32 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.385 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36899 0.00324 0.000 OSF 2 1.66690 0.01437 0.000 FVAR 2 3 0.43279 0.02106 0.000 FVAR 3 4 0.11644 0.01096 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y P1 Max. shift = 0.000 A for H5A_a Max. dU = 0.000 for B101_b Least-squares cycle 33 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 33 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 33 Observed Target Error Sigma Restraint 1.0266 0.9168 0.1098 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8090 1.6669 0.1421 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 33 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.385 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36899 0.00324 0.000 OSF 2 1.66690 0.01437 0.000 FVAR 2 3 0.43279 0.02106 0.000 FVAR 3 4 0.11644 0.01096 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 34 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 34 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 34 Observed Target Error Sigma Restraint 1.0266 0.9168 0.1098 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8090 1.6669 0.1421 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 34 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.385 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36899 0.00324 0.000 OSF 2 1.66690 0.01437 0.000 FVAR 2 3 0.43278 0.02106 0.000 FVAR 3 4 0.11644 0.01096 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y P1 Max. shift = 0.000 A for H5A_a Max. dU = 0.000 for B2_a Least-squares cycle 35 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 35 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 35 Observed Target Error Sigma Restraint 1.0266 0.9168 0.1098 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8090 1.6669 0.1421 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 35 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.385 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36899 0.00324 0.000 OSF 2 1.66690 0.01437 0.000 FVAR 2 3 0.43278 0.02106 0.000 FVAR 3 4 0.11644 0.01096 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H13A Max. dU = 0.000 for B2_a Least-squares cycle 36 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 36 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 36 Observed Target Error Sigma Restraint 1.0266 0.9168 0.1098 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8090 1.6669 0.1421 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 36 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.385 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36899 0.00324 0.000 OSF 2 1.66690 0.01437 0.000 FVAR 2 3 0.43278 0.02106 0.000 FVAR 3 4 0.11644 0.01096 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x P1 Max. shift = 0.000 A for H13A Max. dU = 0.000 for B3_a Least-squares cycle 37 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 37 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 37 Observed Target Error Sigma Restraint 1.0266 0.9168 0.1098 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8090 1.6669 0.1421 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 37 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.385 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36899 0.00324 0.000 OSF 2 1.66690 0.01437 0.000 FVAR 2 3 0.43278 0.02106 0.000 FVAR 3 4 0.11644 0.01096 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y P1 Max. shift = 0.000 A for H5A_a Max. dU = 0.000 for B12 Least-squares cycle 38 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 38 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 38 Observed Target Error Sigma Restraint 1.0266 0.9168 0.1098 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8090 1.6669 0.1421 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 38 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.385 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36899 0.00324 0.000 OSF 2 1.66690 0.01437 0.000 FVAR 2 3 0.43278 0.02106 0.000 FVAR 3 4 0.11644 0.01096 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H105_b Max. dU = 0.000 for B2_a Least-squares cycle 39 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 39 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 39 Observed Target Error Sigma Restraint 1.0266 0.9168 0.1098 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8090 1.6669 0.1421 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 39 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.385 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36899 0.00324 0.000 OSF 2 1.66690 0.01437 0.000 FVAR 2 3 0.43278 0.02106 0.000 FVAR 3 4 0.11644 0.01096 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x P1 Max. shift = 0.000 A for H5A_a Max. dU = 0.000 for B101_b Least-squares cycle 40 Maximum vector length = 511 Memory required = 6125 / 467723 wR2 = 0.3675 before cycle 40 for 5893 data and 368 / 368 parameters Disagreeable restraints before cycle 40 Observed Target Error Sigma Restraint 1.0266 0.9168 0.1098 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8090 1.6669 0.1421 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 40 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.385 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36899 0.00324 0.000 OSF 2 1.66690 0.01437 0.000 FVAR 2 3 0.43278 0.02106 0.000 FVAR 3 4 0.11644 0.01096 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x P1 Max. shift = 0.000 A for H105_b Max. dU = 0.000 for B101_b Largest correlation matrix elements -0.794 y H13A / x H13A -0.610 x B102_b / x B1_a -0.540 U12 B103_b / U23 B103_b 0.711 z B103_b / FVAR 3 -0.584 x B103_b / x B3_a -0.532 z B103_b / y B3_a -0.673 y B1_a / FVAR 3 -0.581 y B102_b / FVAR 3 -0.525 y H5A_a / x H5A_a 0.669 EXTI / OSF -0.573 y B101_b / z B2_a 0.504 x B103_b / U12 B3_a -0.662 U13 B103_b / U11 B103_b -0.565 z B102_b / y B1_a 0.504 z B3_a / FVAR 3 -0.637 U13 B103_b / U33 B103_b -0.555 U13 C14 / U33 C14 0.501 U11 B3_a / U11 B2_a 0.633 U22 P1 / OSF -0.553 U13 C15 / U33 C15 -0.626 z B103_b / x B103_b 0.541 U13 B2_a / U33 B2_a Idealized hydrogen atom generation before cycle 41 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.7620 0.6255 -0.0459 43 0.950 0.000 C2 C3 C1 H3 0.7758 0.6911 -0.2492 43 0.950 0.000 C3 C2 C4 H4 0.7237 0.7594 -0.2372 43 0.950 0.000 C4 C5 C3 H5 0.6632 0.7640 -0.0112 43 0.950 0.000 C5 C4 C6 H6 0.6496 0.6983 0.1983 43 0.950 0.000 C6 C5 C1 H8 0.6745 0.6712 0.5410 43 0.950 0.000 C8 C9 C7 H9 0.6081 0.6843 0.7421 43 0.950 0.000 C9 C8 C10 H10 0.5408 0.6318 0.7303 43 0.950 0.000 C10 C11 C9 H11 0.5411 0.5664 0.5208 43 0.950 0.000 C11 C12 C10 H12 0.6035 0.5565 0.3028 43 0.950 0.000 C12 C11 C7 H14 0.6323 0.5811 -0.0421 43 0.950 0.000 C14 C15 C13 H15 0.6203 0.5142 -0.2366 43 0.950 0.000 C15 C14 C16 H16 0.6748 0.4474 -0.2291 43 0.950 0.000 C16 C17 C15 H17 0.7364 0.4465 -0.0034 43 0.950 0.000 C17 C16 C18 H18 0.7488 0.5122 0.2003 43 0.950 0.000 C18 C17 C13 H20 0.7211 0.5398 0.5488 43 0.950 0.000 C20 C19 C21 H21 0.7886 0.5282 0.7477 43 0.950 0.000 C21 C22 C20 H22 0.8555 0.5794 0.7243 43 0.950 0.000 C22 C23 C21 H23 0.8571 0.6402 0.4999 43 0.950 0.000 C23 C22 C24 H24 0.7919 0.6524 0.2951 43 0.950 0.000 C24 C23 C19 H32 0.9803 0.5710 1.0364 43 0.950 0.000 C32 C33 C31 H33 0.9139 0.5870 1.2365 43 0.950 0.000 C33 C32 C34 H34 0.8457 0.5355 1.2308 43 0.950 0.000 C34 C35 C33 H35 0.8410 0.4722 1.0154 43 0.950 0.000 C35 C34 C36 H36 0.9053 0.4575 0.8071 43 0.950 0.000 C36 C35 C31 H1A 0.8983 0.7432 -0.2383 23 0.990 0.000 B1_a B2_a B3_a H1B 0.9013 0.6832 -0.2567 23 0.990 0.000 B1_a B2_a B3_a H2A 0.8497 0.6746 0.0390 23 0.990 0.000 B2_a B1_a B3_a H2B 0.8467 0.7349 0.0575 23 0.990 0.000 B2_a B1_a B3_a H3A 0.9438 0.7393 0.0766 23 0.990 0.000 B3_a B1_a B2_a H3B 0.9468 0.6790 0.0581 23 0.990 0.000 B3_a B1_a B2_a H10A 0.8580 0.6592 0.0989 23 0.990 0.000 B101_b B102_b B103_b H10B 0.8504 0.7179 0.0578 23 0.990 0.000 B101_b B102_b B103_b H10C 0.9014 0.7118 -0.2280 23 0.990 0.000 B102_b B101_b B103_b H10D 0.9091 0.6526 -0.1865 23 0.990 0.000 B102_b B101_b B103_b H10E 0.9461 0.6735 0.1667 23 0.990 0.000 B103_b B101_b B102_b H10F 0.9384 0.7328 0.1251 23 0.990 0.000 B103_b B101_b B102_b H11A 0.5524 0.4782 -0.0193 23 0.990 0.000 B11 B12 B11_$1 H11B 0.5421 0.5380 -0.0193 23 0.990 0.000 B11 B12 B11_$1 H12A 0.5051 0.4704 0.2662 23 0.990 0.000 B12 B11_$1 B11 H12B 0.4949 0.5296 0.2662 23 0.990 0.000 B12 B11_$1 B11 s93 in I-4 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.70570 0.65594 0.09854 1.00000 0.06564 0.01962 0.03377 -0.00045 -0.01371 0.02111 0.03968 0.00763 0.00017 0.00014 0.00061 0.00000 0.00287 0.00179 0.00226 0.00159 0.00199 0.00176 0.00107 C2 0.74225 0.65366 -0.03716 1.00000 0.07152 0.04120 0.03527 -0.00526 -0.01081 0.03319 0.04933 0.00844 0.00018 0.00016 0.00066 0.00000 0.00321 0.00248 0.00242 0.00189 0.00213 0.00226 0.00129 H2 0.76198 0.62554 -0.04594 1.00000 0.05920 0.00000 0.00000 C3 0.75006 0.69219 -0.15970 1.00000 0.09495 0.03736 0.03088 -0.00721 -0.00399 0.01948 0.05440 0.00913 0.00021 0.00016 0.00071 0.00000 0.00390 0.00254 0.00224 0.00192 0.00241 0.00239 0.00133 H3 0.77584 0.69111 -0.24917 1.00000 0.06528 0.00000 0.00000 C4 0.71918 0.73338 -0.15045 1.00000 0.09660 0.03741 0.03445 0.00459 -0.01582 0.01579 0.05615 0.00903 0.00020 0.00017 0.00072 0.00000 0.00406 0.00261 0.00245 0.00204 0.00251 0.00242 0.00137 H4 0.72374 0.75939 -0.23717 1.00000 0.06739 0.00000 0.00000 C5 0.68306 0.73592 -0.01824 1.00000 0.07716 0.03237 0.04363 -0.00070 -0.01757 0.02293 0.05105 0.00844 0.00019 0.00016 0.00069 0.00000 0.00351 0.00223 0.00269 0.00196 0.00239 0.00224 0.00130 H5 0.66317 0.76398 -0.01119 1.00000 0.06126 0.00000 0.00000 C6 0.67520 0.69698 0.10793 1.00000 0.05824 0.03212 0.04391 0.00391 -0.01202 0.02647 0.04476 0.00823 0.00017 0.00015 0.00069 0.00000 0.00287 0.00215 0.00255 0.00189 0.00209 0.00197 0.00118 H6 0.64964 0.69833 0.19831 1.00000 0.05371 0.00000 0.00000 C7 0.64563 0.61300 0.40101 1.00000 0.04897 0.04531 0.03851 0.00688 -0.02187 0.01096 0.04426 0.00809 0.00017 0.00017 0.00065 0.00000 0.00246 0.00254 0.00244 0.00185 0.00204 0.00189 0.00110 C8 0.64694 0.65067 0.53352 1.00000 0.04334 0.05723 0.04335 -0.00083 -0.01441 0.01809 0.04797 0.00842 0.00017 0.00018 0.00069 0.00000 0.00252 0.00286 0.00263 0.00215 0.00202 0.00207 0.00120 H8 0.67451 0.67122 0.54098 1.00000 0.05757 0.00000 0.00000 C9 0.60770 0.65801 0.65467 1.00000 0.04883 0.08606 0.04913 -0.00219 -0.01829 0.03129 0.06134 0.01009 0.00018 0.00022 0.00079 0.00000 0.00293 0.00385 0.00288 0.00279 0.00237 0.00247 0.00146 H9 0.60805 0.68426 0.74208 1.00000 0.07361 0.00000 0.00000 C10 0.56767 0.62675 0.64801 1.00000 0.05319 0.10738 0.05672 0.02352 -0.01420 0.01521 0.07243 0.01162 0.00021 0.00025 0.00092 0.00000 0.00327 0.00480 0.00336 0.00319 0.00264 0.00291 0.00168 H10 0.54083 0.63182 0.73025 1.00000 0.08692 0.00000 0.00000 C11 0.56751 0.58846 0.52076 1.00000 0.05262 0.09184 0.07569 0.03619 -0.01859 -0.00186 0.07338 0.01159 0.00021 0.00024 0.00093 0.00000 0.00310 0.00432 0.00421 0.00330 0.00291 0.00290 0.00170 H11 0.54110 0.56638 0.52084 1.00000 0.08806 0.00000 0.00000 C12 0.60498 0.58183 0.39413 1.00000 0.06444 0.05562 0.05952 0.02471 -0.02785 0.00280 0.05986 0.00969 0.00020 0.00019 0.00083 0.00000 0.00311 0.00307 0.00332 0.00251 0.00258 0.00234 0.00141 H12 0.60355 0.55650 0.30280 1.00000 0.07183 0.00000 0.00000 C13 0.69078 0.55275 0.10089 1.00000 0.08514 0.02068 0.03755 -0.00419 -0.03165 0.00480 0.04779 0.00730 0.00019 0.00015 0.00063 0.00000 0.00351 0.00186 0.00250 0.00171 0.00244 0.00192 0.00130 C14 0.65304 0.55373 -0.03272 1.00000 0.11487 0.04031 0.05352 -0.00045 -0.05392 0.01332 0.06957 0.00875 0.00023 0.00018 0.00078 0.00000 0.00475 0.00270 0.00325 0.00223 0.00345 0.00271 0.00184 H14 0.63228 0.58109 -0.04214 1.00000 0.08348 0.00000 0.00000 C15 0.64667 0.51438 -0.14967 1.00000 0.14457 0.03636 0.05568 0.00380 -0.05896 -0.00980 0.07887 0.00919 0.00026 0.00018 0.00084 0.00000 0.00554 0.00277 0.00336 0.00236 0.00391 0.00289 0.00206 H15 0.62031 0.51415 -0.23660 1.00000 0.09464 0.00000 0.00000 C16 0.67873 0.47381 -0.14366 1.00000 0.12991 0.02734 0.04913 0.00056 -0.03539 -0.02431 0.06879 0.00854 0.00023 0.00017 0.00079 0.00000 0.00507 0.00239 0.00292 0.00211 0.00337 0.00253 0.00175 H16 0.67478 0.44743 -0.22910 1.00000 0.08255 0.00000 0.00000 C17 0.71552 0.47376 -0.01116 1.00000 0.10662 0.02066 0.03683 0.00154 -0.02202 -0.00563 0.05470 0.00773 0.00021 0.00015 0.00066 0.00000 0.00418 0.00202 0.00252 0.00178 0.00274 0.00219 0.00145 H17 0.73643 0.44647 -0.00344 1.00000 0.06564 0.00000 0.00000 C18 0.72285 0.51252 0.11133 1.00000 0.07782 0.01862 0.03942 -0.00041 -0.01324 -0.00071 0.04528 0.00760 0.00018 0.00014 0.00065 0.00000 0.00326 0.00184 0.00241 0.00174 0.00237 0.00188 0.00116 H18 0.74876 0.51218 0.20029 1.00000 0.05434 0.00000 0.00000 C19 0.74983 0.59643 0.39932 1.00000 0.05643 0.02654 0.03182 -0.00775 -0.02064 0.02055 0.03826 0.00709 0.00017 0.00014 0.00059 0.00000 0.00250 0.00200 0.00223 0.00160 0.00204 0.00175 0.00107 C20 0.74877 0.56005 0.53648 1.00000 0.05974 0.03163 0.03016 -0.00055 -0.01636 0.01596 0.04051 0.00762 0.00017 0.00015 0.00060 0.00000 0.00275 0.00213 0.00219 0.00169 0.00201 0.00185 0.00111 H20 0.72108 0.53983 0.54878 1.00000 0.04861 0.00000 0.00000 C21 0.78879 0.55347 0.65615 1.00000 0.07293 0.04175 0.02517 0.00074 -0.01312 0.02445 0.04662 0.00876 0.00018 0.00017 0.00065 0.00000 0.00325 0.00250 0.00208 0.00188 0.00220 0.00210 0.00120 H21 0.78859 0.52816 0.74774 1.00000 0.05594 0.00000 0.00000 C22 0.82865 0.58372 0.64150 1.00000 0.06637 0.03995 0.03372 -0.00773 -0.01827 0.02129 0.04668 0.00821 0.00019 0.00017 0.00068 0.00000 0.00305 0.00246 0.00234 0.00193 0.00225 0.00204 0.00120 H22 0.85551 0.57937 0.72426 1.00000 0.05602 0.00000 0.00000 C23 0.82950 0.61976 0.50868 1.00000 0.05873 0.04159 0.04058 -0.01497 -0.01506 0.01145 0.04697 0.00784 0.00018 0.00017 0.00065 0.00000 0.00281 0.00246 0.00248 0.00201 0.00222 0.00205 0.00116 H23 0.85711 0.64020 0.49988 1.00000 0.05636 0.00000 0.00000 C24 0.79088 0.62706 0.38657 1.00000 0.07388 0.02227 0.03930 -0.00633 -0.01800 0.01390 0.04515 0.00751 0.00018 0.00015 0.00066 0.00000 0.00300 0.00203 0.00247 0.00177 0.00229 0.00186 0.00115 H24 0.79188 0.65238 0.29509 1.00000 0.05418 0.00000 0.00000 P1 0.69779 0.60465 0.25025 1.00000 0.06198 0.02171 0.03366 0.00034 -0.02065 0.01499 0.03912 0.00160 0.00004 0.00003 0.00015 0.00000 0.00082 0.00059 0.00082 0.00042 0.00072 0.00043 0.00048 C31 0.94813 0.51304 0.90120 1.00000 0.05906 0.03191 0.03863 0.00112 0.00129 -0.00242 0.04320 0.00802 0.00017 0.00016 0.00064 0.00000 0.00272 0.00226 0.00250 0.00177 0.00215 0.00194 0.00108 C32 0.95190 0.55158 1.03091 1.00000 0.05266 0.05437 0.04295 -0.00367 0.00068 -0.02716 0.04999 0.00775 0.00018 0.00017 0.00070 0.00000 0.00276 0.00288 0.00263 0.00216 0.00214 0.00217 0.00125 H32 0.98028 0.57102 1.03639 1.00000 0.05999 0.00000 0.00000 C33 0.91295 0.56041 1.15075 1.00000 0.05646 0.03874 0.03644 -0.00446 0.00192 -0.01217 0.04388 0.00780 0.00017 0.00017 0.00070 0.00000 0.00288 0.00243 0.00233 0.00189 0.00207 0.00188 0.00113 H33 0.91391 0.58700 1.23652 1.00000 0.05266 0.00000 0.00000 C34 0.87178 0.52983 1.14533 1.00000 0.05256 0.01985 0.03640 0.00392 -0.00532 -0.01180 0.03627 0.00672 0.00017 0.00013 0.00063 0.00000 0.00263 0.00183 0.00212 0.00159 0.00193 0.00158 0.00100 H34 0.84573 0.53547 1.23081 1.00000 0.04352 0.00000 0.00000 C35 0.86897 0.49222 1.01860 1.00000 0.05025 0.01983 0.03678 -0.00064 -0.00584 0.00212 0.03562 0.00720 0.00016 0.00014 0.00060 0.00000 0.00242 0.00184 0.00227 0.00162 0.00191 0.00164 0.00099 H35 0.84097 0.47221 1.01538 1.00000 0.04274 0.00000 0.00000 C36 0.90704 0.48352 0.89542 1.00000 0.06872 0.02697 0.03564 -0.00075 -0.00445 0.00597 0.04377 0.00810 0.00017 0.00015 0.00065 0.00000 0.00299 0.00212 0.00241 0.00176 0.00214 0.00187 0.00112 H36 0.90526 0.45753 0.80709 1.00000 0.05253 0.00000 0.00000 P31 1.00000 0.50000 0.75000 0.25000 0.07131 0.07131 0.03684 0.00000 0.00000 0.00000 0.05982 0.00000 0.00000 0.00000 0.00000 0.00000 0.00112 0.00112 0.00141 0.00000 0.00000 0.00000 0.00076 B1_a 0.89900 0.71160 -0.17135 0.43278 0.02492 0.13325 0.01394 0.00098 0.00149 0.00900 0.05737 0.03359 0.00053 0.00102 0.00172 0.02106 0.00634 0.01511 0.00512 0.00737 0.00380 0.00865 0.00507 H1A_a 0.89831 0.74316 -0.23830 0.43278 0.06884 0.02106 0.00000 H1B_a 0.90128 0.68316 -0.25670 0.43278 0.06884 0.02106 0.00000 B2_a 0.86542 0.70622 0.01542 0.43278 0.03662 0.14304 0.05652 0.02726 0.01724 0.05991 0.07873 0.04532 0.00062 0.00091 0.00291 0.02106 0.00589 0.01496 0.01025 0.01011 0.00709 0.00816 0.00575 H2A_a 0.84966 0.67455 0.03900 0.43278 0.09448 0.02106 0.00000 H2B_a 0.84667 0.73488 0.05750 0.43278 0.09448 0.02106 0.00000 B3_a 0.92884 0.70911 0.02822 0.43278 0.03728 0.05451 0.01872 0.02650 -0.00088 0.00933 0.03684 0.02725 0.00054 0.00061 0.00173 0.02106 0.00540 0.00827 0.00545 0.00522 0.00448 0.00568 0.00324 H3A_a 0.94376 0.73932 0.07660 0.43278 0.04421 0.02106 0.00000 H3B_a 0.94675 0.67897 0.05809 0.43278 0.04421 0.02106 0.00000 H4A_a 0.86851 0.70985 -0.11744 0.43278 0.05526 0.12483 0.00099 0.00414 0.00448 0.02106 0.00000 H5A_a 0.92823 0.71656 -0.09839 0.43278 0.05526 0.10301 0.00119 0.00360 0.00442 0.02106 0.00000 B101_b 0.87238 0.68961 0.04948 0.56722 0.04343 0.15793 0.04962 0.05476 -0.02291 -0.00190 0.08366 0.03285 0.00050 0.00082 0.00209 0.02106 0.00620 0.01410 0.00605 0.00775 0.00482 0.00780 0.00496 H10A_b 0.85803 0.65924 0.09891 0.56722 0.10039 0.02106 0.00000 H10B_b 0.85036 0.71786 0.05783 0.56722 0.10039 0.02106 0.00000 B102_b 0.90332 0.68534 -0.13339 0.56722 0.04539 0.07052 0.07420 -0.01826 -0.01092 0.02835 0.06337 0.02445 0.00047 0.00063 0.00235 0.02106 0.00639 0.00867 0.00719 0.00682 0.00542 0.00622 0.00374 H10C_b 0.90136 0.71183 -0.22803 0.56722 0.07605 0.02106 0.00000 H10D_b 0.90911 0.65262 -0.18653 0.56722 0.07605 0.02106 0.00000 B103_b 0.92794 0.69913 0.09884 0.56722 0.06501 0.03802 0.12281 0.03770 -0.07747 -0.02140 0.07528 0.02089 0.00056 0.00046 0.00318 0.02106 0.00711 0.00568 0.01122 0.00703 0.00884 0.00484 0.00496 H10E_b 0.94614 0.67350 0.16669 0.56722 0.09034 0.02106 0.00000 H10F_b 0.93838 0.73280 0.12514 0.56722 0.09034 0.02106 0.00000 H104_b 0.87522 0.69645 -0.08274 0.56722 0.11292 0.10848 0.00116 0.00315 0.00383 0.02106 0.00000 H105_b 0.90076 0.68694 0.14326 0.56722 0.11292 0.09185 0.00122 0.00330 0.00421 0.02106 0.00000 B11 0.53051 0.50523 0.01546 0.50000 0.06594 0.05117 0.05252 -0.00577 -0.01180 0.00144 0.05654 0.01952 0.00036 0.00053 0.00182 0.00000 0.00742 0.00646 0.00629 0.00571 0.00548 0.00677 0.00289 H11A 0.55238 0.47820 -0.01926 0.50000 0.06785 0.00000 0.00000 H11B 0.54212 0.53801 -0.01926 0.50000 0.06785 0.00000 0.00000 B12 0.50000 0.50000 0.18917 0.25000 0.21988 0.02996 0.01908 0.00000 0.00000 -0.01386 0.08964 0.01434 0.00000 0.00000 0.00204 0.00000 0.02200 0.00819 0.00642 0.00000 0.00000 0.01274 0.00668 H12A 0.50508 0.47040 0.26622 0.25000 0.10757 0.00000 0.00000 H12B 0.49492 0.52960 0.26622 0.25000 0.10757 0.00000 0.00000 H13A 0.53071 0.50741 0.14746 0.50000 0.13446 0.13529 0.00210 0.00651 0.00495 0.00000 0.00000 Final Structure Factor Calculation for s93 in I-4 Total number of l.s. parameters = 368 Maximum vector length = 511 Memory required = 5759 / 25046 wR2 = 0.3675 before cycle 41 for 5893 data and 2 / 368 parameters Disagreeable restraints before cycle 41 Observed Target Error Sigma Restraint 1.0266 0.9168 0.1098 0.0300 DFIX B101_b H105_b 1.4904 1.6669 -0.1765 0.0400 DFIX B11 B12 1.8090 1.6669 0.1421 0.0400 DFIX B102_b B103_b -0.1539 0.0400 SIMU U11 B11 B12 Summary of restraints applied in cycle 41 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 22. 0. 0. 0. 0. 0. 94. 246. 0. 0. rms sigma 0.000 0.034 0.000 0.000 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.069 0.000 0.000 0.000 0.000 0.000 0.007 0.026 0.000 0.000 GooF = S = 1.404; Restrained GooF = 1.385 for 362 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1292 for 4575 Fo > 4sig(Fo) and 0.1533 for all 5893 data wR2 = 0.3675, GooF = S = 1.404, Restrained GooF = 1.385 for all data Flack x parameter = 0.2426 with esd 0.2138 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 35.00 for non-hydrogen and 35.00 for hydrogen atoms Principal mean square atomic displacements U 0.0777 0.0309 0.0104 C1 0.0952 0.0330 0.0197 C2 0.1014 0.0366 0.0252 C3 0.1035 0.0406 0.0243 C4 0.0924 0.0400 0.0207 C5 0.0768 0.0449 0.0126 C6 0.0672 0.0495 0.0161 C7 0.0727 0.0476 0.0237 C8 0.1061 0.0556 0.0224 C9 0.1180 0.0684 0.0309 C10 0.1233 0.0616 0.0352 C11 0.0962 0.0622 0.0211 C12 0.1014 0.0228 0.0192 C13 0.1475 0.0411 0.0201 C14 0.1748 0.0357 0.0262 C15 0.1476 0.0395 0.0192 C16 0.1133 0.0305 0.0203 C17 0.0819 0.0353 0.0186 C18 0.0774 0.0221 0.0152 C19 0.0725 0.0304 0.0187 C20 0.0883 0.0331 0.0184 C21 0.0857 0.0294 0.0250 C22 0.0762 0.0389 0.0257 C23 0.0853 0.0316 0.0186 C24 0.0761 0.0280 0.0133 P1 0.0593 0.0388 0.0315 C31 0.0809 0.0430 0.0261 C32 0.0632 0.0377 0.0307 C33 0.0582 0.0348 0.0158 C34 0.0526 0.0346 0.0197 C35 0.0701 0.0351 0.0261 C36 0.0713 0.0713 0.0368 P31 0.1340 0.0244 0.0137 B1_a 0.1783 0.0487 0.0092 B2_a 0.0705 0.0362 0.0038 B3_a 0.1816 0.0565 0.0128 B101_b 0.1041 0.0591 0.0269 B102_b 0.1890 0.0266 0.0103 B103_b 0.0736 0.0528 0.0432 B11 0.2209 0.0290 0.0191 B12 may be split into 0.5079 0.4994 0.1892 and 0.4921 0.5006 0.1892 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.017 0.022 0.027 0.033 0.040 0.049 0.062 0.094 1.000 Number in group 645. 630. 611. 531. 591. 582. 607. 521. 581. 594. GooF 1.429 1.407 1.448 1.552 1.641 1.417 1.399 1.376 1.187 1.119 K 3.051 1.435 1.210 1.116 1.174 1.084 1.095 1.100 1.098 1.083 Resolution(A) 0.77 0.80 0.84 0.88 0.92 0.98 1.06 1.16 1.33 1.67 inf Number in group 620. 566. 602. 579. 584. 582. 599. 580. 598. 583. GooF 1.493 1.400 1.311 1.347 1.329 1.420 1.413 1.342 1.396 1.568 K 1.191 1.168 1.149 1.122 1.037 1.058 1.006 0.968 0.962 1.180 R1 0.263 0.230 0.186 0.168 0.152 0.136 0.128 0.114 0.114 0.134 Recommended weighting scheme: WGHT 0.2000 0.0000 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) 4 6 0 500.29 93.83 6.09 0.026 3.83 10 10 8 -18.29 148.53 4.96 0.033 0.80 28 14 4 -7.35 401.87 4.71 0.053 0.79 -6 20 0 488.98 137.85 4.30 0.031 1.32 -4 26 0 211.83 39.32 4.22 0.017 1.05 4 35 1 -20.24 367.05 3.97 0.051 0.78 23 20 1 196.51 18.38 3.96 0.011 0.90 -20 23 1 198.69 16.03 3.95 0.011 0.90 -16 18 0 101.82 12.51 3.93 0.009 1.15 9 23 2 215.32 6.85 3.91 0.007 1.06 -18 17 1 167.87 41.53 3.81 0.017 1.10 3 25 0 7.93 127.46 3.80 0.030 1.10 -16 9 1 486.95 171.80 3.68 0.035 1.47 20 17 1 118.57 26.08 3.65 0.014 1.04 -8 30 4 457.06 116.26 3.60 0.029 0.79 6 22 0 977.28 317.84 3.54 0.048 1.21 -21 20 1 395.03 145.23 3.54 0.032 0.94 -13 3 4 123.43 40.94 3.48 0.017 1.34 -21 23 0 117.32 3.13 3.47 0.005 0.89 -25 12 1 392.68 120.62 3.44 0.029 0.99 9 4 1 150.18 61.75 3.40 0.021 2.60 -4 9 1 152.33 61.16 3.37 0.021 2.60 11 19 4 119.17 12.25 3.36 0.009 1.02 17 8 1 60.98 13.61 3.35 0.010 1.44 -24 19 3 218.50 24.89 3.31 0.013 0.84 -28 18 2 392.49 49.27 3.31 0.019 0.81 15 21 0 195.14 68.06 3.31 0.022 1.07 -21 25 0 168.29 8.39 3.30 0.008 0.85 -14 30 0 70.66 289.57 3.28 0.045 0.83 -18 30 0 44.22 260.24 3.28 0.043 0.79 24 0 4 265.71 56.24 3.27 0.020 0.96 -1 21 6 428.64 146.62 3.26 0.032 0.87 -34 5 1 508.82 126.00 3.26 0.030 0.80 8 16 0 349.36 145.31 3.23 0.032 1.54 -12 20 0 67.69 232.76 3.20 0.041 1.18 -22 22 4 1460.01 488.96 3.19 0.059 0.79 -27 11 4 553.70 131.81 3.19 0.031 0.83 -3 9 0 844.93 371.91 3.18 0.051 2.91 1 31 0 246.24 4.20 3.15 0.005 0.89 -5 11 0 103.44 44.00 3.13 0.018 2.28 -4 10 0 25.20 85.61 3.12 0.025 2.56 9 16 1 525.73 163.07 3.11 0.034 1.47 -3 23 4 68.32 250.84 3.11 0.042 0.99 0 32 0 103.15 5.78 3.10 0.006 0.86 -2 6 0 183.87 544.75 3.10 0.062 4.36 -13 33 0 2.24 113.48 3.10 0.028 0.78 0 24 4 304.54 58.72 3.09 0.020 0.96 -23 9 2 243.73 6.43 3.06 0.007 1.06 9 31 0 346.18 40.64 3.06 0.017 0.85 12 22 6 297.41 96.68 3.05 0.026 0.80 Bond lengths and angles C1 - Distance Angles C2 1.3898 (0.0068) C6 1.4124 (0.0051) 120.05 (0.41) P1 1.7857 (0.0042) 117.58 (0.29) 122.32 (0.38) C1 - C2 C6 C2 - Distance Angles C3 1.3854 (0.0067) C1 1.3898 (0.0068) 120.35 (0.38) H2 0.9500 119.83 119.83 C2 - C3 C1 C3 - Distance Angles C2 1.3854 (0.0066) C4 1.4220 (0.0061) 119.45 (0.49) H3 0.9500 120.28 120.28 C3 - C2 C4 C4 - Distance Angles C5 1.3648 (0.0070) C3 1.4220 (0.0061) 120.66 (0.46) H4 0.9500 119.67 119.67 C4 - C5 C3 C5 - Distance Angles C4 1.3648 (0.0070) C6 1.4103 (0.0063) 120.11 (0.41) H5 0.9500 119.95 119.95 C5 - C4 C6 C6 - Distance Angles C5 1.4103 (0.0063) C1 1.4124 (0.0051) 119.33 (0.46) H6 0.9500 120.33 120.33 C6 - C5 C1 C7 - Distance Angles C8 1.3964 (0.0066) C12 1.4142 (0.0069) 119.76 (0.50) P1 1.8024 (0.0050) 117.83 (0.38) 122.37 (0.42) C7 - C8 C12 C8 - Distance Angles C9 1.3925 (0.0069) C7 1.3964 (0.0066) 119.74 (0.50) H8 0.9500 120.13 120.13 C8 - C9 C7 C9 - Distance Angles C8 1.3925 (0.0069) C10 1.4023 (0.0076) 120.18 (0.58) H9 0.9500 119.91 119.91 C9 - C8 C10 C10 - Distance Angles C11 1.3846 (0.0084) C9 1.4023 (0.0076) 119.56 (0.60) H10 0.9500 120.22 120.22 C10 - C11 C9 C11 - Distance Angles C12 1.3766 (0.0081) C10 1.3846 (0.0084) 121.14 (0.59) H11 0.9500 119.43 119.43 C11 - C12 C10 C12 - Distance Angles C11 1.3766 (0.0081) C7 1.4142 (0.0069) 119.51 (0.57) H12 0.9500 120.25 120.25 C12 - C11 C7 C13 - Distance Angles C14 1.4027 (0.0063) C18 1.4215 (0.0059) 120.78 (0.41) P1 1.7863 (0.0041) 117.31 (0.34) 121.88 (0.34) C13 - C14 C18 C14 - Distance Angles C15 1.3733 (0.0068) C13 1.4027 (0.0063) 118.74 (0.48) H14 0.9500 120.63 120.63 C14 - C15 C13 C15 - Distance Angles C14 1.3733 (0.0068) C16 1.4273 (0.0076) 121.53 (0.52) H15 0.9500 119.23 119.23 C15 - C14 C16 C16 - Distance Angles C17 1.3780 (0.0069) C15 1.4273 (0.0076) 118.53 (0.47) H16 0.9500 120.74 120.74 C16 - C17 C15 C17 - Distance Angles C16 1.3780 (0.0069) C18 1.3881 (0.0059) 121.73 (0.47) H17 0.9500 119.13 119.13 C17 - C16 C18 C18 - Distance Angles C17 1.3881 (0.0059) C13 1.4215 (0.0059) 118.62 (0.43) H18 0.9500 120.69 120.69 C18 - C17 C13 C19 - Distance Angles C20 1.3923 (0.0059) C24 1.4160 (0.0065) 119.41 (0.40) P1 1.7923 (0.0040) 118.65 (0.36) 121.89 (0.33) C19 - C20 C24 C20 - Distance Angles C19 1.3923 (0.0059) C21 1.4000 (0.0059) 119.55 (0.46) H20 0.9500 120.22 120.22 C20 - C19 C21 C21 - Distance Angles C22 1.3846 (0.0070) C20 1.4000 (0.0059) 120.24 (0.43) H21 0.9500 119.88 119.88 C21 - C22 C20 C22 - Distance Angles C23 1.3643 (0.0065) C21 1.3846 (0.0070) 120.26 (0.44) H22 0.9500 119.87 119.87 C22 - C23 C21 C23 - Distance Angles C22 1.3643 (0.0065) C24 1.3833 (0.0062) 121.19 (0.49) H23 0.9500 119.41 119.41 C23 - C22 C24 C24 - Distance Angles C23 1.3833 (0.0062) C19 1.4160 (0.0065) 119.33 (0.43) H24 0.9500 120.33 120.33 C24 - C23 C19 P1 - Distance Angles C1 1.7857 (0.0043) C13 1.7863 (0.0041) 107.30 (0.23) C19 1.7923 (0.0040) 110.59 (0.20) 109.22 (0.18) C7 1.8024 (0.0050) 110.34 (0.19) 111.21 (0.23) 108.19 (0.23) P1 - C1 C13 C19 C31 - Distance Angles C36 1.3967 (0.0064) C32 1.4047 (0.0064) 121.37 (0.44) P31 1.8189 (0.0047) 120.42 (0.35) 118.10 (0.35) C31 - C36 C32 C32 - Distance Angles C33 1.3871 (0.0066) C31 1.4047 (0.0064) 118.04 (0.40) H32 0.9500 120.98 120.98 C32 - C33 C31 C33 - Distance Angles C32 1.3871 (0.0066) C34 1.4156 (0.0055) 120.03 (0.43) H33 0.9500 119.98 119.98 C33 - C32 C34 C34 - Distance Angles C35 1.3700 (0.0054) C33 1.4156 (0.0055) 120.97 (0.45) H34 0.9500 119.51 119.52 C34 - C35 C33 C35 - Distance Angles C34 1.3700 (0.0054) C36 1.3827 (0.0061) 119.73 (0.41) H35 0.9500 120.13 120.13 C35 - C34 C36 C36 - Distance Angles C35 1.3827 (0.0061) C31 1.3967 (0.0064) 119.81 (0.41) H36 0.9500 120.09 120.09 C36 - C35 C31 P31 - Distance Angles C31_$6 1.8189 (0.0047) C31_$4 1.8189 (0.0047) 109.98 (0.15) C31 1.8189 (0.0047) 109.98 (0.15) 108.46 (0.29) C31_$5 1.8189 (0.0047) 108.46 (0.29) 109.98 (0.15) 109.98 (0.15) P31 - C31_$6 C31_$4 C31 B1_a - Distance Angles B2_a 1.6142 (0.0188) B3_a 1.6285 (0.0155) 65.50 (0.86) H1A_a 0.9900 117.18 117.18 H1B_a 0.9900 117.18 117.18 114.22 H4A_a 0.9241 (0.0256) 30.54 (1.75) 96.01 (1.91) 102.92 105.36 H5A_a 0.9655 (0.0263) 93.46 (2.00) 29.05 (1.86) 98.29 112.42 123.36 (3.48) H104_b 0.9968 (0.0541) 22.32 (4.40) 77.08 (2.05) 130.80 95.06 28.63 (6.83) 106.09 (2.89) B1_a - B2_a B3_a H1A_a H1B_a H4A_a H5A_a B2_a - Distance Angles B1_a 1.6142 (0.0188) B3_a 1.7543 (0.0204) 57.64 (0.67) H2A_a 0.9900 118.01 118.01 H2B_a 0.9900 118.01 118.01 115.18 H4A_a 0.9434 (0.0259) 29.85 (1.65) 87.46 (1.86) 107.41 104.98 H104_b 0.7888 (0.0421) 28.68 (6.23) 73.63 (3.17) 89.74 135.53 30.55 (8.82) H105_b 1.4291 (0.0479) 98.87 (1.60) 45.87 (1.57) 82.28 117.77 126.91 (3.92) 100.89 (3.79) B2_a - B1_a B3_a H2A_a H2B_a H4A_a H104_b B3_a - Distance Angles B1_a 1.6285 (0.0155) B2_a 1.7543 (0.0204) 56.86 (0.75) H3A_a 0.9900 118.08 118.08 H3B_a 0.9900 118.08 118.08 115.27 H5A_a 0.9139 (0.0268) 30.87 (1.93) 86.66 (1.99) 98.80 113.89 H105_b 1.2762 (0.0417) 105.04 (1.72) 53.49 (2.01) 116.00 76.46 135.56 (3.34) B3_a - B1_a B2_a H3A_a H3B_a H5A_a B101_b - Distance Angles B102_b 1.5480 (0.0194) B103_b 1.5938 (0.0178) 70.29 (1.09) H4A_a 1.3040 (0.0530) 47.95 (2.91) 101.78 (2.06) H10A_b 0.9900 116.60 116.60 130.22 H10B_b 0.9900 116.60 116.60 70.49 113.60 H104_b 0.9518 (0.0298) 32.69 (2.34) 95.78 (2.69) 16.84 (6.39) 122.94 87.27 H105_b 1.0266 (0.0280) 96.15 (2.34) 30.45 (1.91) 132.17 (3.27) 91.07 119.14 125.36 (2.95) B101_b - B102_b B103_b H4A_a H10A_b H10B_b H104_b B102_b - Distance Angles B101_b 1.5480 (0.0193) B103_b 1.8090 (0.0196) 56.04 (0.86) H4A_a 1.1801 (0.0731) 55.14 (2.05) 95.70 (2.52) H5A_a 1.1291 (0.0721) 95.54 (2.62) 54.15 (1.74) 92.15 (6.09) H10C_b 0.9900 118.16 118.16 66.19 67.44 H10D_b 0.9900 118.16 118.16 133.61 132.83 115.37 H104_b 0.9067 (0.0299) 34.54 (2.43) 84.00 (2.33) 21.99 (5.44) 100.19 (6.48) 88.14 126.48 B102_b - B101_b B103_b H4A_a H5A_a H10C_b H10D_b B103_b - Distance Angles B101_b 1.5938 (0.0179) B102_b 1.8090 (0.0196) 53.67 (0.75) H5A_a 1.4678 (0.0354) 81.57 (1.36) 38.57 (2.83) H10E_b 0.9900 118.37 118.37 133.37 H10F_b 0.9900 118.37 118.37 82.38 115.64 H105_b 0.8793 (0.0286) 36.28 (2.21) 85.40 (2.28) 117.75 (2.40) 89.32 122.75 B103_b - B101_b B102_b H5A_a H10E_b H10F_b B11 - Distance Angles B12 1.4904 (0.0177) B11_$1 1.7083 (0.0199) 55.03 (0.51) H11A 0.9900 118.25 118.25 H11B 0.9900 118.25 118.25 115.49 H13A 0.9301 (0.0308) 36.08 (2.26) 90.95 (2.44) 106.92 100.68 B11 - B12 B11_$1 H11A H11B B12 - Distance Angles B11_$1 1.4904 (0.0177) B11 1.4904 (0.0177) 69.93 (1.01) H12A 0.9900 116.64 116.64 H12B 0.9900 116.64 116.64 113.65 H13A 0.9196 (0.0302) 106.30 (2.97) 36.55 (2.33) 103.15 96.99 B12 - B11_$1 B11 H12A H12B FMAP and GRID set by program FMAP 2 3 -11 GRID -3.125 -1 -1 3.125 1 1 R1 = 0.1481 for 3289 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.77 at 0.0920 0.7717 0.2469 [ 0.91 A from P1 ] Deepest hole -1.07 at 0.9142 0.2058 0.2464 [ 0.57 A from P1 ] Mean = 0.00, Rms deviation from mean = 0.14 e/A^3, Highest memory used = 6846 / 68429 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7283 0.5920 0.2531 1.00000 0.05 0.77 0.91 P1 1.19 C19 1.84 C13 2.16 C1 Q2 1 0.7192 0.5245 0.1225 1.00000 0.05 0.75 0.35 C18 1.04 H18 1.12 C13 1.69 C17 Q3 1 0.6271 0.5901 0.3848 1.00000 0.05 0.73 0.65 C12 0.82 C7 1.27 H12 1.90 C11 Q4 1 0.7730 0.6040 0.3877 1.00000 0.05 0.69 0.68 C19 0.81 C24 1.57 H24 1.74 C20 Q5 1 0.9212 0.4872 0.8852 1.00000 0.05 0.67 0.41 C36 1.04 C31 1.08 H36 1.72 C35 Q6 1 0.6766 0.5810 0.2635 1.00000 0.05 0.57 0.88 P1 1.44 C13 1.56 C7 2.15 H12 Q7 1 0.6632 0.6796 0.1254 1.00000 0.05 0.52 0.60 C6 0.82 H6 1.36 C1 1.93 C5 Q8 1 0.6993 0.6788 0.1345 1.00000 0.05 0.49 0.70 C1 0.85 C6 1.54 H6 1.83 C2 Q9 1 0.5521 0.5793 0.5079 1.00000 0.05 0.49 0.48 H11 0.50 C11 1.67 C12 1.69 C10 Q10 1 0.6809 0.7499 0.2475 1.00000 0.05 0.49 1.70 H6 1.77 C6 1.91 C5 1.92 H5 Shortest distances between peaks (including symmetry equivalents) 7 8 1.00 1 6 1.46 1 4 1.59 3 6 1.63 1 2 2.09 8 10 2.17 7 10 2.18 2 6 2.19 3 9 2.26 1 8 2.66 4 6 2.87 6 7 2.91 6 8 2.92 1 3 2.94 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.01: Analyse DFIX/DANG restraints 0.01: 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 0.02: Analyse other restraints etc. 2.02: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.07: Set up l.s. refinement 0.01: Generate idealized H-atoms 39.20: Structure factors and derivatives 49.47: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.73: Apply other restraints 5.86: Solve l.s. equations 0.00: Generate HTAB table 0.14: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.15: Fourier summations 0.10: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s93 finished at 16:59:48 Total CPU time: 97.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++