+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 09:34:45 on 23-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh167 in P2(1)2(1)2(1) CELL 0.71073 7.5138 9.3146 12.8999 90.000 90.000 90.000 ZERR 4.00 0.0005 0.0007 0.0011 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O UNIT 40 44 4 8 V = 902.84 F(000) = 376.0 Mu = 0.09 mm-1 Cell Wt = 708.79 Rho = 1.304 MERG 2 OMIT -3.00 55.00 OMIT 2 0 0 OMIT 1 2 0 TWIN DFIX C1A N1A 1.4 0.02 DELU ISOR 0.01 C6B EQIV $1 -x, y-1/2, -z-1/2 EQIV $2 -x, y-1/2, -z+1/2 HTAB N1A O1A_$1 HTAB N1B O1B_$2 FMAP 2 PLAN 5 SIZE 0.08 0.12 0.18 ACTA BOND $H L.S. 22 TEMP -153.00 WGHT 0.013100 0.462700 EXTI 0.063510 BASF 2.95110 FVAR 1.96413 0.55715 PART 1 AFIX 66 C1A 1 0.057677 0.574745 -0.080530 21.00000 0.03430 0.02064 = 0.04309 0.00377 0.00186 0.00196 C2A 1 0.153742 0.689253 -0.039993 21.00000 0.03300 0.01909 = 0.04585 0.00093 0.00329 0.00238 AFIX 43 H2A 2 0.210216 0.755597 -0.085232 21.00000 -1.20000 AFIX 65 C3A 1 0.167177 0.706692 0.066734 21.00000 0.02149 0.02783 = 0.04645 0.00312 -0.00374 0.00015 AFIX 43 H3A 2 0.232834 0.784953 0.094439 21.00000 -1.20000 AFIX 65 C4A 1 0.084548 0.609622 0.132926 21.00000 0.03721 0.02607 = 0.03906 -0.00422 0.00196 0.00321 C5A 1 -0.011518 0.495113 0.092391 21.00000 0.02579 0.03668 = 0.05906 0.00232 0.00617 -0.00867 AFIX 43 H5A 2 -0.067991 0.428770 0.137631 21.00000 -1.20000 AFIX 65 C6A 1 -0.024955 0.477673 -0.014336 21.00000 0.02823 0.03125 = 0.03243 -0.00271 0.00196 -0.00649 AFIX 43 H6A 2 -0.090611 0.399411 -0.042040 21.00000 -1.20000 AFIX 0 C7A 1 0.065699 0.648435 -0.268261 21.00000 0.05384 0.02766 = 0.04124 0.01356 -0.00526 0.00705 C8A 1 0.017300 0.589521 -0.372878 21.00000 0.05463 0.03306 = 0.04664 0.00175 0.00367 0.00637 AFIX 137 H8A1 2 -0.088429 0.639309 -0.399077 21.00000 -1.50000 H8A2 2 -0.007906 0.486627 -0.366887 21.00000 -1.50000 H8A3 2 0.116646 0.604177 -0.420950 21.00000 -1.50000 AFIX 0 C9A 1 0.085969 0.637885 0.244477 21.00000 0.09375 0.03704 = 0.04307 -0.01043 0.01058 0.00304 C10A 1 -0.000587 0.539351 0.321454 21.00000 0.05582 0.07870 = 0.04001 0.00561 0.00260 -0.00545 AFIX 137 H10A 2 0.043891 0.441443 0.311343 21.00000 -1.50000 H10B 2 -0.129850 0.540820 0.311386 21.00000 -1.50000 H10C 2 0.027667 0.571434 0.391909 21.00000 -1.50000 AFIX 0 N1A 3 0.033522 0.550235 -0.187829 21.00000 0.03597 0.02501 = 0.04955 0.00124 -0.00414 -0.00516 AFIX 43 H1A 2 -0.005620 0.464825 -0.206007 21.00000 -1.20000 AFIX 0 O1A 4 0.116616 0.771347 -0.257684 21.00000 0.05083 0.02842 = 0.06556 -0.00086 -0.01011 0.00389 O2A 4 0.196333 0.726265 0.277748 21.00000 0.05939 0.04299 = 0.05539 -0.00641 -0.00957 -0.00002 PART 2 AFIX 66 SAME C1A > O2A C1B 1 0.056715 0.573475 0.078508 -21.00000 0.02280 0.03530 = 0.20060 0.01128 0.01269 0.01114 C6B 1 -0.021938 0.474807 0.011906 -21.00000 0.04232 0.01548 = 0.21178 0.02701 -0.01392 -0.00176 AFIX 43 H6B 2 -0.084744 0.394819 0.039280 -21.00000 -1.20000 AFIX 65 C5B 1 -0.008697 0.493171 -0.094749 -21.00000 0.03124 0.02779 = 0.20228 0.02697 -0.00073 0.01126 AFIX 43 H5B 2 -0.062453 0.425735 -0.140268 -21.00000 -1.20000 AFIX 65 C4B 1 0.083198 0.610205 -0.134803 -21.00000 0.02372 0.03044 = 0.19936 0.01220 -0.00061 0.00182 C3B 1 0.161852 0.708875 -0.068201 -21.00000 0.03232 0.03075 = 0.20086 0.01290 0.00480 -0.00153 AFIX 43 H3B 2 0.224658 0.788862 -0.095577 -21.00000 -1.20000 AFIX 65 C2B 1 0.148612 0.690511 0.038454 -21.00000 0.03439 0.02467 = 0.19421 -0.01377 0.00345 -0.00735 AFIX 43 H2B 2 0.202368 0.757948 0.083973 -21.00000 -1.20000 AFIX 0 C7B 1 0.083777 0.635995 0.269479 -21.00000 0.03523 0.03979 = 0.18795 0.04062 -0.05235 -0.01764 C8B 1 0.010922 0.583486 0.371730 -21.00000 0.04351 0.04334 = 0.22028 0.02338 0.02480 -0.00111 AFIX 137 H8B1 2 0.101573 0.595019 0.425712 -21.00000 -1.50000 H8B2 2 -0.021229 0.481861 0.365729 -21.00000 -1.50000 H8B3 2 -0.094876 0.639490 0.390131 -21.00000 -1.50000 AFIX 0 C9B 1 0.091154 0.629090 -0.245867 -21.00000 0.04015 0.03151 = 0.20354 0.01698 -0.01082 0.01018 C10B 1 0.004385 0.539880 -0.326869 -21.00000 0.03624 0.04142 = 0.21407 0.02616 -0.02422 -0.00874 AFIX 137 H10D 2 0.049425 0.567774 -0.395260 -21.00000 -1.50000 H10E 2 -0.124685 0.554636 -0.324440 -21.00000 -1.50000 H10F 2 0.031183 0.438387 -0.314335 -21.00000 -1.50000 AFIX 0 N1B 3 0.032355 0.551075 0.184207 -21.00000 0.04055 0.02360 = 0.21156 0.00845 0.01848 0.01022 AFIX 43 H1B 2 -0.024030 0.471335 0.200326 -21.00000 -1.20000 AFIX 0 O1B 4 0.121291 0.765985 0.263520 -21.00000 0.06826 0.02753 = 0.23829 -0.00142 0.04845 -0.00904 O2B 4 0.195866 0.728611 -0.270971 -21.00000 0.05433 0.03130 = 0.19847 -0.00336 0.01352 -0.01327 HKLF 4 Covalent radii and connectivity table for 2008lsh167 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1A_a - C2A_a C6A_a N1A_a C2A_a - C3A_a C1A_a C3A_a - C2A_a C4A_a C4A_a - C3A_a C5A_a C9A_a C5A_a - C6A_a C4A_a C6A_a - C5A_a C1A_a C7A_a - O1A_a N1A_a C8A_a C8A_a - C7A_a C9A_a - O2A_a C4A_a C10A_a C10A_a - C9A_a N1A_a - C7A_a C1A_a O1A_a - C7A_a O2A_a - C9A_a C1B_b - C6B_b C2B_b N1B_b C6B_b - C1B_b C5B_b C5B_b - C6B_b C4B_b C4B_b - C3B_b C5B_b C9B_b C3B_b - C4B_b C2B_b C2B_b - C3B_b C1B_b C7B_b - O1B_b N1B_b C8B_b C8B_b - C7B_b C9B_b - O2B_b C4B_b C10B_b C10B_b - C9B_b N1B_b - C1B_b C7B_b O1B_b - C7B_b O2B_b - C9B_b Operators for generating equivalent atoms: $1 -x, y-1/2, -z-1/2 $2 -x, y-1/2, -z+1/2 7477 Reflections read, of which 43 rejected -9 =< h =< 9, -11 =< k =< 12, -16 =< l =< 16, Max. 2-theta = 54.98 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 7 6 2.40 0.55 5 3.25 1 Inconsistent equivalents 1993 Unique reflections, of which 0 suppressed R(int) = 0.0638 R(sigma) = 0.0684 Friedel opposites not merged Maximum memory for data reduction = 2933 / 19963 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 = 3589 / 270098 wR2 = 0.1523 before cycle 1 for 1993 data and 218 / 218 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.0475 0.0100 ISOR U11 C6B_b 0.0744 0.0100 ISOR U22 C6B_b -0.1219 0.0100 ISOR U33 C6B_b Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 30. 0. 0. 0. 60. 0. 6. 0. rms sigma 0.000 0.020 0.000 0.033 0.000 0.000 0.000 0.010 0.000 0.010 0.000 rms deviation 0.000 0.015 0.000 0.031 0.000 0.000 0.000 0.009 0.000 0.063 0.000 GooF = S = 1.152; Restrained GooF = 1.205 for 97 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0131 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.95724 0.01186 -0.581 OSF 2 0.56565 0.00622 1.366 FVAR 2 3 2.95643 4.91734 0.001 BASF 1 4 0.05893 0.01597 -0.287 EXTI 126 0.16768 0.00805 -5.478 U33 C6B_b 132 0.17314 0.00946 -3.079 U33 C5B_b Mean shift/esd = 0.395 Maximum = -5.478 for U33 C6B_b Max. shift = 0.022 A for H8B2_b Max. dU =-0.009 for C6B_b Least-squares cycle 2 Maximum vector length = 511 Memory required = 3589 / 270098 wR2 = 0.1530 before cycle 2 for 1993 data and 218 / 218 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.0570 0.0100 ISOR U22 C6B_b -0.0865 0.0100 ISOR U33 C6B_b Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 30. 0. 0. 0. 60. 0. 6. 0. rms sigma 0.000 0.020 0.000 0.033 0.000 0.000 0.000 0.010 0.000 0.010 0.000 rms deviation 0.000 0.013 0.000 0.032 0.000 0.000 0.000 0.010 0.000 0.045 0.000 GooF = S = 1.161; Restrained GooF = 1.186 for 97 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0131 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.95684 0.01159 -0.035 OSF 2 0.56976 0.00616 0.666 FVAR 2 3 2.82633 4.86072 -0.027 BASF 1 4 0.05895 0.01542 0.001 EXTI Mean shift/esd = 0.207 Maximum = -2.500 for U33 C6B_b Max. shift = 0.029 A for H8B2_b Max. dU =-0.003 for C5B_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 3589 / 270098 wR2 = 0.1534 before cycle 3 for 1993 data and 218 / 218 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 0.0303 0.0100 DELU C6B_b N1B_b 0.0458 0.0100 ISOR U22 C6B_b -0.0654 0.0100 ISOR U33 C6B_b Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 30. 0. 0. 0. 60. 0. 6. 0. rms sigma 0.000 0.020 0.000 0.033 0.000 0.000 0.000 0.010 0.000 0.010 0.000 rms deviation 0.000 0.012 0.000 0.033 0.000 0.000 0.000 0.011 0.000 0.034 0.000 GooF = S = 1.164; Restrained GooF = 1.179 for 97 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0131 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.96037 0.01167 0.303 OSF 2 0.56976 0.00614 0.001 FVAR 2 3 2.70759 4.84433 -0.025 BASF 1 4 0.06068 0.01540 0.112 EXTI Mean shift/esd = 0.101 Maximum = 1.580 for U22 C6B_b Max. shift = 0.036 A for H8B2_b Max. dU = 0.004 for C6B_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 3589 / 270098 wR2 = 0.1534 before cycle 4 for 1993 data and 218 / 218 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.0302 0.0100 DELU C6B_b N1B_b 0.0398 0.0100 ISOR U22 C6B_b -0.0600 0.0100 ISOR U33 C6B_b Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 30. 0. 0. 0. 60. 0. 6. 0. rms sigma 0.000 0.020 0.000 0.033 0.000 0.000 0.000 0.010 0.000 0.010 0.000 rms deviation 0.000 0.012 0.000 0.033 0.000 0.000 0.000 0.011 0.000 0.031 0.000 GooF = S = 1.162; Restrained GooF = 1.174 for 97 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0131 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.96340 0.01174 0.258 OSF 2 0.56974 0.00612 -0.003 FVAR 2 3 2.70474 4.84389 -0.001 BASF 1 4 0.06266 0.01548 0.127 EXTI Mean shift/esd = 0.073 Maximum = 0.859 for U22 C6B_b Max. shift = 0.027 A for H8B2_b Max. dU = 0.002 for C6B_b Least-squares cycle 5 Maximum vector length = 511 Memory required = 3589 / 270098 wR2 = 0.1536 before cycle 5 for 1993 data and 218 / 218 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 0.0300 0.0100 DELU C6B_b N1B_b 0.0362 0.0100 ISOR U22 C6B_b -0.0571 0.0100 ISOR U33 C6B_b Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 30. 0. 0. 0. 60. 0. 6. 0. rms sigma 0.000 0.020 0.000 0.033 0.000 0.000 0.000 0.010 0.000 0.010 0.000 rms deviation 0.000 0.012 0.000 0.033 0.000 0.000 0.000 0.011 0.000 0.030 0.000 GooF = S = 1.162; Restrained GooF = 1.173 for 97 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0131 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.96469 0.01179 0.109 OSF 2 0.56966 0.00611 -0.013 FVAR 2 3 2.71092 4.85131 0.001 BASF 1 4 0.06350 0.01560 0.054 EXTI Mean shift/esd = 0.045 Maximum = 0.452 for U22 C6B_b Max. shift = 0.015 A for H8B2_b Max. dU = 0.001 for C6B_b Least-squares cycle 6 Maximum vector length = 511 Memory required = 3589 / 270098 wR2 = 0.1536 before cycle 6 for 1993 data and 218 / 218 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint -0.0307 0.0100 DELU C6B_b C2B_b 0.0300 0.0100 DELU C6B_b N1B_b 0.0343 0.0100 ISOR U22 C6B_b -0.0557 0.0100 ISOR U33 C6B_b Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 30. 0. 0. 0. 60. 0. 6. 0. rms sigma 0.000 0.020 0.000 0.033 0.000 0.000 0.000 0.010 0.000 0.010 0.000 rms deviation 0.000 0.012 0.000 0.033 0.000 0.000 0.000 0.011 0.000 0.029 0.000 GooF = S = 1.162; Restrained GooF = 1.172 for 97 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0131 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.96522 0.01181 0.045 OSF 2 0.56967 0.00611 0.001 FVAR 2 3 2.72643 4.86036 0.003 BASF 1 4 0.06384 0.01565 0.022 EXTI Mean shift/esd = 0.028 Maximum = 0.223 for U22 C6B_b Max. shift = 0.007 A for H8B2_b Max. dU = 0.001 for C6B_b Least-squares cycle 7 Maximum vector length = 511 Memory required = 3589 / 270098 wR2 = 0.1537 before cycle 7 for 1993 data and 218 / 218 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint -0.0311 0.0100 DELU C6B_b C2B_b 0.0334 0.0100 ISOR U22 C6B_b -0.0550 0.0100 ISOR U33 C6B_b Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 30. 0. 0. 0. 60. 0. 6. 0. rms sigma 0.000 0.020 0.000 0.033 0.000 0.000 0.000 0.010 0.000 0.010 0.000 rms deviation 0.000 0.012 0.000 0.033 0.000 0.000 0.000 0.011 0.000 0.029 0.000 GooF = S = 1.162; Restrained GooF = 1.172 for 97 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0131 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.96556 0.01182 0.029 OSF 2 0.56970 0.00611 0.004 FVAR 2 3 2.74968 4.86749 0.005 BASF 1 4 0.06404 0.01567 0.013 EXTI Mean shift/esd = 0.019 Maximum = 0.109 for U22 C6B_b Max. shift = 0.005 A for H10D_b Max. dU = 0.000 for C6B_b Least-squares cycle 8 Maximum vector length = 511 Memory required = 3589 / 270098 wR2 = 0.1537 before cycle 8 for 1993 data and 218 / 218 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint -0.0313 0.0100 DELU C6B_b C2B_b 0.0329 0.0100 ISOR U22 C6B_b -0.0546 0.0100 ISOR U33 C6B_b Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 30. 0. 0. 0. 60. 0. 6. 0. rms sigma 0.000 0.020 0.000 0.033 0.000 0.000 0.000 0.010 0.000 0.010 0.000 rms deviation 0.000 0.012 0.000 0.033 0.000 0.000 0.000 0.011 0.000 0.028 0.000 GooF = S = 1.162; Restrained GooF = 1.172 for 97 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0131 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.96570 0.01182 0.012 OSF 2 0.56974 0.00611 0.007 FVAR 2 3 2.76818 4.87347 0.004 BASF 1 4 0.06412 0.01569 0.005 EXTI Mean shift/esd = 0.013 Maximum = -0.079 for U11 C4B_b Max. shift = 0.003 A for H10D_b Max. dU = 0.000 for C6B_b Least-squares cycle 9 Maximum vector length = 511 Memory required = 3589 / 270098 wR2 = 0.1537 before cycle 9 for 1993 data and 218 / 218 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint -0.0314 0.0100 DELU C6B_b C2B_b 0.0327 0.0100 ISOR U22 C6B_b -0.0544 0.0100 ISOR U33 C6B_b Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 30. 0. 0. 0. 60. 0. 6. 0. rms sigma 0.000 0.020 0.000 0.033 0.000 0.000 0.000 0.010 0.000 0.010 0.000 rms deviation 0.000 0.012 0.000 0.033 0.000 0.000 0.000 0.011 0.000 0.028 0.000 GooF = S = 1.162; Restrained GooF = 1.172 for 97 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0131 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.96580 0.01183 0.008 OSF 2 0.56977 0.00611 0.005 FVAR 2 3 2.78278 4.87661 0.003 BASF 1 4 0.06418 0.01569 0.004 EXTI Mean shift/esd = 0.010 Maximum = -0.062 for U11 C4B_b Max. shift = 0.002 A for H10D_b Max. dU = 0.000 for C4B_b Least-squares cycle 10 Maximum vector length = 511 Memory required = 3589 / 270098 wR2 = 0.1537 before cycle 10 for 1993 data and 218 / 218 parameters Disagreeable restraints before cycle 10 Observed Target Error Sigma Restraint -0.0314 0.0100 DELU C6B_b C2B_b 0.0326 0.0100 ISOR U22 C6B_b -0.0543 0.0100 ISOR U33 C6B_b Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 30. 0. 0. 0. 60. 0. 6. 0. rms sigma 0.000 0.020 0.000 0.033 0.000 0.000 0.000 0.010 0.000 0.010 0.000 rms deviation 0.000 0.012 0.000 0.033 0.000 0.000 0.000 0.011 0.000 0.028 0.000 GooF = S = 1.162; Restrained GooF = 1.172 for 97 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0131 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.96584 0.01183 0.004 OSF 2 0.56980 0.00612 0.004 FVAR 2 3 2.79064 4.87934 0.002 BASF 1 4 0.06421 0.01569 0.002 EXTI Mean shift/esd = 0.007 Maximum = -0.045 for U11 C4B_b Max. shift = 0.001 A for H10D_b Max. dU = 0.000 for C4B_b Least-squares cycle 11 Maximum vector length = 511 Memory required = 3589 / 270098 wR2 = 0.1537 before cycle 11 for 1993 data and 218 / 218 parameters Disagreeable restraints before cycle 11 Observed Target Error Sigma Restraint -0.0315 0.0100 DELU C6B_b C2B_b 0.0300 0.0100 DELU C6B_b N1B_b 0.0325 0.0100 ISOR U22 C6B_b -0.0543 0.0100 ISOR U33 C6B_b Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 30. 0. 0. 0. 60. 0. 6. 0. rms sigma 0.000 0.020 0.000 0.033 0.000 0.000 0.000 0.010 0.000 0.010 0.000 rms deviation 0.000 0.012 0.000 0.033 0.000 0.000 0.000 0.011 0.000 0.028 0.000 GooF = S = 1.162; Restrained GooF = 1.172 for 97 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0131 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.96587 0.01183 0.002 OSF 2 0.56982 0.00612 0.003 FVAR 2 3 2.80019 4.88150 0.002 BASF 1 4 0.06421 0.01570 0.000 EXTI Mean shift/esd = 0.005 Maximum = -0.032 for U11 C4B_b Max. shift = 0.001 A for H10D_b Max. dU = 0.000 for C4B_b Least-squares cycle 12 Maximum vector length = 511 Memory required = 3589 / 270098 wR2 = 0.1537 before cycle 12 for 1993 data and 218 / 218 parameters Disagreeable restraints before cycle 12 Observed Target Error Sigma Restraint -0.0315 0.0100 DELU C6B_b C2B_b 0.0300 0.0100 DELU C6B_b N1B_b 0.0325 0.0100 ISOR U22 C6B_b -0.0542 0.0100 ISOR U33 C6B_b Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 30. 0. 0. 0. 60. 0. 6. 0. rms sigma 0.000 0.020 0.000 0.033 0.000 0.000 0.000 0.010 0.000 0.010 0.000 rms deviation 0.000 0.012 0.000 0.033 0.000 0.000 0.000 0.011 0.000 0.028 0.000 GooF = S = 1.162; Restrained GooF = 1.172 for 97 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0131 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.96588 0.01183 0.001 OSF 2 0.56983 0.00612 0.002 FVAR 2 3 2.80638 4.88319 0.001 BASF 1 4 0.06422 0.01570 0.000 EXTI Mean shift/esd = 0.004 Maximum = -0.022 for U11 C4B_b Max. shift = 0.001 A for H10D_b Max. dU = 0.000 for C4B_b Least-squares cycle 13 Maximum vector length = 511 Memory required = 3589 / 270098 wR2 = 0.1537 before cycle 13 for 1993 data and 218 / 218 parameters Disagreeable restraints before cycle 13 Observed Target Error Sigma Restraint -0.0315 0.0100 DELU C6B_b C2B_b 0.0300 0.0100 DELU C6B_b N1B_b 0.0325 0.0100 ISOR U22 C6B_b -0.0542 0.0100 ISOR U33 C6B_b Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 30. 0. 0. 0. 60. 0. 6. 0. rms sigma 0.000 0.020 0.000 0.033 0.000 0.000 0.000 0.010 0.000 0.010 0.000 rms deviation 0.000 0.012 0.000 0.033 0.000 0.000 0.000 0.011 0.000 0.028 0.000 GooF = S = 1.162; Restrained GooF = 1.172 for 97 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0131 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.96589 0.01183 0.001 OSF 2 0.56984 0.00612 0.002 FVAR 2 3 2.81180 4.88373 0.001 BASF 1 4 0.06422 0.01570 0.000 EXTI Mean shift/esd = 0.003 Maximum = -0.016 for U11 C4B_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C4B_b Least-squares cycle 14 Maximum vector length = 511 Memory required = 3589 / 270098 wR2 = 0.1537 before cycle 14 for 1993 data and 218 / 218 parameters Disagreeable restraints before cycle 14 Observed Target Error Sigma Restraint -0.0315 0.0100 DELU C6B_b C2B_b 0.0300 0.0100 DELU C6B_b N1B_b 0.0325 0.0100 ISOR U22 C6B_b -0.0542 0.0100 ISOR U33 C6B_b Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 30. 0. 0. 0. 60. 0. 6. 0. rms sigma 0.000 0.020 0.000 0.033 0.000 0.000 0.000 0.010 0.000 0.010 0.000 rms deviation 0.000 0.012 0.000 0.033 0.000 0.000 0.000 0.011 0.000 0.028 0.000 GooF = S = 1.162; Restrained GooF = 1.172 for 97 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0131 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.96589 0.01183 0.000 OSF 2 0.56985 0.00612 0.001 FVAR 2 3 2.81179 4.88466 0.000 BASF 1 4 0.06422 0.01570 0.000 EXTI Mean shift/esd = 0.002 Maximum = -0.011 for U11 C4B_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C4B_b Least-squares cycle 15 Maximum vector length = 511 Memory required = 3589 / 270098 wR2 = 0.1537 before cycle 15 for 1993 data and 218 / 218 parameters Disagreeable restraints before cycle 15 Observed Target Error Sigma Restraint -0.0315 0.0100 DELU C6B_b C2B_b 0.0301 0.0100 DELU C6B_b N1B_b 0.0324 0.0100 ISOR U22 C6B_b -0.0542 0.0100 ISOR U33 C6B_b Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 30. 0. 0. 0. 60. 0. 6. 0. rms sigma 0.000 0.020 0.000 0.033 0.000 0.000 0.000 0.010 0.000 0.010 0.000 rms deviation 0.000 0.012 0.000 0.033 0.000 0.000 0.000 0.011 0.000 0.028 0.000 GooF = S = 1.162; Restrained GooF = 1.172 for 97 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0131 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.96590 0.01183 0.001 OSF 2 0.56986 0.00612 0.001 FVAR 2 3 2.81251 4.88533 0.000 BASF 1 4 0.06423 0.01570 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.008 for U11 C4B_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C10B_b Least-squares cycle 16 Maximum vector length = 511 Memory required = 3589 / 270098 wR2 = 0.1537 before cycle 16 for 1993 data and 218 / 218 parameters Disagreeable restraints before cycle 16 Observed Target Error Sigma Restraint -0.0315 0.0100 DELU C6B_b C2B_b 0.0301 0.0100 DELU C6B_b N1B_b 0.0324 0.0100 ISOR U22 C6B_b -0.0542 0.0100 ISOR U33 C6B_b Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 30. 0. 0. 0. 60. 0. 6. 0. rms sigma 0.000 0.020 0.000 0.033 0.000 0.000 0.000 0.010 0.000 0.010 0.000 rms deviation 0.000 0.012 0.000 0.033 0.000 0.000 0.000 0.011 0.000 0.028 0.000 GooF = S = 1.162; Restrained GooF = 1.172 for 97 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0131 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.96590 0.01183 0.000 OSF 2 0.56986 0.00612 0.001 FVAR 2 3 2.81529 4.88546 0.001 BASF 1 4 0.06422 0.01570 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.005 for U11 C4B_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C10B_b Least-squares cycle 17 Maximum vector length = 511 Memory required = 3589 / 270098 wR2 = 0.1537 before cycle 17 for 1993 data and 218 / 218 parameters Disagreeable restraints before cycle 17 Observed Target Error Sigma Restraint -0.0315 0.0100 DELU C6B_b C2B_b 0.0301 0.0100 DELU C6B_b N1B_b 0.0324 0.0100 ISOR U22 C6B_b -0.0542 0.0100 ISOR U33 C6B_b Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 30. 0. 0. 0. 60. 0. 6. 0. rms sigma 0.000 0.020 0.000 0.033 0.000 0.000 0.000 0.010 0.000 0.010 0.000 rms deviation 0.000 0.012 0.000 0.033 0.000 0.000 0.000 0.011 0.000 0.028 0.000 GooF = S = 1.162; Restrained GooF = 1.172 for 97 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0131 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.96590 0.01183 0.000 OSF 2 0.56987 0.00612 0.000 FVAR 2 3 2.81662 4.88557 0.000 BASF 1 4 0.06422 0.01570 0.000 EXTI Mean shift/esd = 0.001 Maximum = 0.004 for U11 C3B_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C10B_b Least-squares cycle 18 Maximum vector length = 511 Memory required = 3589 / 270098 wR2 = 0.1537 before cycle 18 for 1993 data and 218 / 218 parameters Disagreeable restraints before cycle 18 Observed Target Error Sigma Restraint -0.0315 0.0100 DELU C6B_b C2B_b 0.0301 0.0100 DELU C6B_b N1B_b 0.0324 0.0100 ISOR U22 C6B_b -0.0542 0.0100 ISOR U33 C6B_b Summary of restraints applied in cycle 18 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 30. 0. 0. 0. 60. 0. 6. 0. rms sigma 0.000 0.020 0.000 0.033 0.000 0.000 0.000 0.010 0.000 0.010 0.000 rms deviation 0.000 0.012 0.000 0.033 0.000 0.000 0.000 0.011 0.000 0.028 0.000 GooF = S = 1.162; Restrained GooF = 1.172 for 97 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0131 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.96590 0.01183 0.000 OSF 2 0.56987 0.00612 0.001 FVAR 2 3 2.81653 4.88588 0.000 BASF 1 4 0.06422 0.01570 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.003 for U11 C3A_a Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C10B_b Least-squares cycle 19 Maximum vector length = 511 Memory required = 3589 / 270098 wR2 = 0.1537 before cycle 19 for 1993 data and 218 / 218 parameters Disagreeable restraints before cycle 19 Observed Target Error Sigma Restraint -0.0315 0.0100 DELU C6B_b C2B_b 0.0301 0.0100 DELU C6B_b N1B_b 0.0324 0.0100 ISOR U22 C6B_b -0.0542 0.0100 ISOR U33 C6B_b Summary of restraints applied in cycle 19 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 30. 0. 0. 0. 60. 0. 6. 0. rms sigma 0.000 0.020 0.000 0.033 0.000 0.000 0.000 0.010 0.000 0.010 0.000 rms deviation 0.000 0.012 0.000 0.033 0.000 0.000 0.000 0.011 0.000 0.028 0.000 GooF = S = 1.162; Restrained GooF = 1.172 for 97 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0131 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.96589 0.01183 0.000 OSF 2 0.56987 0.00612 0.000 FVAR 2 3 2.81580 4.88597 0.000 BASF 1 4 0.06422 0.01570 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for U11 C4B_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C10B_b Least-squares cycle 20 Maximum vector length = 511 Memory required = 3589 / 270098 wR2 = 0.1537 before cycle 20 for 1993 data and 218 / 218 parameters Disagreeable restraints before cycle 20 Observed Target Error Sigma Restraint -0.0315 0.0100 DELU C6B_b C2B_b 0.0301 0.0100 DELU C6B_b N1B_b 0.0324 0.0100 ISOR U22 C6B_b -0.0542 0.0100 ISOR U33 C6B_b Summary of restraints applied in cycle 20 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 30. 0. 0. 0. 60. 0. 6. 0. rms sigma 0.000 0.020 0.000 0.033 0.000 0.000 0.000 0.010 0.000 0.010 0.000 rms deviation 0.000 0.012 0.000 0.033 0.000 0.000 0.000 0.011 0.000 0.028 0.000 GooF = S = 1.162; Restrained GooF = 1.172 for 97 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0131 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.96590 0.01183 0.000 OSF 2 0.56987 0.00612 0.000 FVAR 2 3 2.81514 4.88619 0.000 BASF 1 4 0.06422 0.01570 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for U11 C3A_a Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C10B_b Least-squares cycle 21 Maximum vector length = 511 Memory required = 3589 / 270098 wR2 = 0.1537 before cycle 21 for 1993 data and 218 / 218 parameters Disagreeable restraints before cycle 21 Observed Target Error Sigma Restraint -0.0315 0.0100 DELU C6B_b C2B_b 0.0301 0.0100 DELU C6B_b N1B_b 0.0324 0.0100 ISOR U22 C6B_b -0.0542 0.0100 ISOR U33 C6B_b Summary of restraints applied in cycle 21 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 30. 0. 0. 0. 60. 0. 6. 0. rms sigma 0.000 0.020 0.000 0.033 0.000 0.000 0.000 0.010 0.000 0.010 0.000 rms deviation 0.000 0.012 0.000 0.033 0.000 0.000 0.000 0.011 0.000 0.028 0.000 GooF = S = 1.162; Restrained GooF = 1.172 for 97 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0131 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.96590 0.01183 0.000 OSF 2 0.56987 0.00612 0.000 FVAR 2 3 2.81756 4.88618 0.000 BASF 1 4 0.06422 0.01570 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for U11 C3B_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C10B_b Least-squares cycle 22 Maximum vector length = 511 Memory required = 3589 / 270098 wR2 = 0.1537 before cycle 22 for 1993 data and 218 / 218 parameters Disagreeable restraints before cycle 22 Observed Target Error Sigma Restraint -0.0315 0.0100 DELU C6B_b C2B_b 0.0301 0.0100 DELU C6B_b N1B_b 0.0324 0.0100 ISOR U22 C6B_b -0.0542 0.0100 ISOR U33 C6B_b Summary of restraints applied in cycle 22 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 30. 0. 0. 0. 60. 0. 6. 0. rms sigma 0.000 0.020 0.000 0.033 0.000 0.000 0.000 0.010 0.000 0.010 0.000 rms deviation 0.000 0.012 0.000 0.033 0.000 0.000 0.000 0.011 0.000 0.028 0.000 GooF = S = 1.162; Restrained GooF = 1.172 for 97 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0131 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.96589 0.01183 -0.001 OSF 2 0.56988 0.00612 0.001 FVAR 2 3 2.81743 4.88628 0.000 BASF 1 4 0.06421 0.01570 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for U11 C4B_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C10B_b Largest correlation matrix elements -0.893 rotZ C1B_b / rotZ C1A_a -0.748 U22 C6B_b / U22 C6A_a -0.684 y C9B_b / y C7A_a -0.793 U11 C6B_b / U11 C6A_a -0.738 x C9B_b / x C7A_a -0.674 U12 N1B_b / U12 N1A_a 0.793 x C1B_b / rotY C1B_b -0.730 U22 C7B_b / U22 C9A_a -0.665 U11 C2B_b / U11 C2A_a -0.791 y C1B_b / rotX C1B_b 0.728 EXTI / OSF 0.657 U33 C9B_b / U33 C4B_b -0.790 U12 C6B_b / U12 C6A_a -0.726 x C1A_a / rotY C1A_a -0.655 x C9B_b / U11 C7A_a 0.776 y C1A_a / rotX C1A_a 0.701 U33 C2B_b / U33 C3B_b -0.643 U12 C4B_b / U12 C4A_a -0.761 x C7B_b / x C9A_a 0.696 y C9B_b / U22 C7A_a -0.643 U12 C2B_b / U12 C2A_a -0.750 y C7B_b / y C9A_a 0.693 U23 C7B_b / y C9A_a -0.643 U12 O1B_b / U12 O1A_a Idealized hydrogen atom generation before cycle 23 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.2094 0.7570 -0.0847 43 0.950 0.000 C2A_a C3A_a C1A_a H3A 0.2302 0.7856 0.0951 43 0.950 0.000 C3A_a C2A_a C4A_a H5A -0.0674 0.4272 0.1365 43 0.950 0.000 C5A_a C6A_a C4A_a H6A -0.0882 0.3986 -0.0433 43 0.950 0.000 C6A_a C5A_a C1A_a H8A1 -0.0851 0.6418 -0.4008 137 0.980 0.000 C8A_a C7A_a H8A1_a H8A2 -0.0129 0.4875 -0.3661 137 0.980 0.000 C8A_a C7A_a H8A1_a H8A3 0.1187 0.5998 -0.4203 137 0.980 0.000 C8A_a C7A_a H8A1_a H10A 0.0478 0.4434 0.3153 137 0.980 0.000 C10A_a C9A_a H10A_a H10B -0.1300 0.5375 0.3083 137 0.980 0.000 C10A_a C9A_a H10A_a H10C 0.0205 0.5773 0.3913 137 0.980 0.000 C10A_a C9A_a H10A_a H1A -0.0063 0.4647 -0.2059 43 0.880 0.000 N1A_a C7A_a C1A_a H6B -0.0883 0.3953 0.0373 43 0.950 0.000 C6B_b C1B_b C5B_b H5B -0.0637 0.4268 -0.1421 43 0.950 0.000 C5B_b C6B_b C4B_b H3B 0.2280 0.7871 -0.0955 43 0.950 0.000 C3B_b C4B_b C2B_b H2B 0.2034 0.7556 0.0839 43 0.950 0.000 C2B_b C3B_b C1B_b H8B1 0.0962 0.6068 0.4284 137 0.980 0.000 C8B_b C7B_b H8B1_b H8B2 -0.0047 0.4790 0.3699 137 0.980 0.000 C8B_b C7B_b H8B1_b H8B3 -0.1028 0.6296 0.3872 137 0.980 0.000 C8B_b C7B_b H8B1_b H10D 0.0581 0.5601 -0.3937 137 0.980 0.000 C10B_b C9B_b H10D_b H10E -0.1225 0.5607 -0.3279 137 0.980 0.000 C10B_b C9B_b H10D_b H10F 0.0226 0.4376 -0.3093 137 0.980 0.000 C10B_b C9B_b H10D_b H1B -0.0225 0.4712 0.2000 43 0.880 0.000 N1B_b C1B_b C7B_b 2008lsh167 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1A_a 0.05866 0.57513 -0.08089 0.56988 0.03572 0.02102 0.04578 0.00252 0.00202 0.00124 0.03417 0.00637 0.00064 0.00046 0.00022 0.00612 0.00407 0.00316 0.00299 0.00241 0.00258 0.00284 0.00149 C2A_a 0.15322 0.69006 -0.03978 0.56988 0.03123 0.02091 0.04890 0.00085 0.00563 -0.00198 0.03368 0.00733 0.00088 0.00052 0.00029 0.00612 0.00435 0.00343 0.00341 0.00263 0.00298 0.00295 0.00164 H2A_a 0.20940 0.75700 -0.08468 0.56988 0.04041 0.00612 0.00000 C3A_a 0.16558 0.70704 0.06703 0.56988 0.02046 0.02520 0.04943 0.00373 -0.00532 -0.00238 0.03170 0.00552 0.00090 0.00049 0.00031 0.00612 0.00347 0.00360 0.00288 0.00257 0.00265 0.00275 0.00149 H3A_a 0.23021 0.78559 0.09513 0.56988 0.03804 0.00612 0.00000 C4A_a 0.08338 0.60909 0.13273 0.56988 0.03999 0.02765 0.03970 -0.00321 0.00425 0.00186 0.03578 0.00613 0.00071 0.00043 0.00022 0.00612 0.00389 0.00312 0.00297 0.00234 0.00280 0.00304 0.00146 C5A_a -0.01118 0.49416 0.09162 0.56988 0.02464 0.02936 0.06373 0.00808 0.00727 -0.00725 0.03925 0.00672 0.00057 0.00037 0.00027 0.00612 0.00311 0.00297 0.00346 0.00245 0.00279 0.00235 0.00140 H5A_a -0.06735 0.42722 0.13652 0.56988 0.04709 0.00612 0.00000 C6A_a -0.02354 0.47718 -0.01519 0.56988 0.01917 0.01166 0.04411 -0.00180 0.00253 -0.00319 0.02498 0.00499 0.00052 0.00038 0.00029 0.00612 0.00266 0.00229 0.00290 0.00192 0.00220 0.00195 0.00130 H6A_a -0.08817 0.39863 -0.04329 0.56988 0.02998 0.00612 0.00000 C7A_a 0.06574 0.64908 -0.26862 0.56988 0.05475 0.02804 0.04261 0.01272 -0.00654 0.00862 0.04180 0.01669 0.00174 0.00106 0.00053 0.00612 0.00603 0.00409 0.00311 0.00261 0.00309 0.00401 0.00252 C8A_a 0.01742 0.58934 -0.37304 0.56988 0.05376 0.03565 0.04864 0.00055 0.00269 0.00806 0.04602 0.01198 0.00113 0.00074 0.00045 0.00612 0.00448 0.00340 0.00316 0.00260 0.00313 0.00339 0.00169 H8A1_a -0.08510 0.64178 -0.40082 0.56988 0.06903 0.00612 0.00000 H8A2_a -0.01288 0.48745 -0.36612 0.56988 0.06903 0.00612 0.00000 H8A3_a 0.11871 0.59980 -0.42029 0.56988 0.06903 0.00612 0.00000 C9A_a 0.08582 0.63671 0.24359 0.56988 0.09189 0.04784 0.04172 -0.00805 0.01015 0.00593 0.06048 0.02046 0.00210 0.00141 0.00062 0.00612 0.00822 0.00603 0.00368 0.00339 0.00421 0.00526 0.00335 C10A_a -0.00151 0.54043 0.32135 0.56988 0.05599 0.07970 0.04031 0.00506 0.00279 -0.00504 0.05867 0.01525 0.00147 0.00104 0.00045 0.00612 0.00463 0.00637 0.00320 0.00331 0.00368 0.00476 0.00233 H10A_a 0.04780 0.44339 0.31529 0.56988 0.08800 0.00612 0.00000 H10B_a -0.12996 0.53755 0.30835 0.56988 0.08800 0.00612 0.00000 H10C_a 0.02048 0.57734 0.39134 0.56988 0.08800 0.00612 0.00000 N1A_a 0.03337 0.55006 -0.18787 0.56988 0.03809 0.02656 0.05152 -0.00085 -0.00621 -0.00366 0.03872 0.00828 0.00068 0.00052 0.00033 0.00612 0.00321 0.00253 0.00254 0.00207 0.00225 0.00242 0.00132 H1A_a -0.00628 0.46475 -0.20590 0.56988 0.04647 0.00612 0.00000 O1A_a 0.11743 0.77125 -0.25776 0.56988 0.05279 0.03012 0.06615 -0.00121 -0.01099 0.00507 0.04969 0.00872 0.00085 0.00051 0.00038 0.00612 0.00342 0.00255 0.00296 0.00200 0.00260 0.00250 0.00138 O2A_a 0.19579 0.72632 0.27789 0.56988 0.06253 0.04554 0.05640 -0.00574 -0.00879 -0.00064 0.05483 0.00956 0.00085 0.00065 0.00041 0.00612 0.00440 0.00361 0.00279 0.00252 0.00254 0.00287 0.00167 C1B_b 0.05522 0.57251 0.07749 0.43012 0.02313 0.03613 0.17750 0.00075 0.01020 0.01281 0.07892 0.01588 0.00116 0.00090 0.00072 0.00612 0.00485 0.00534 0.00796 0.00570 0.00593 0.00418 0.00300 C6B_b -0.02411 0.47487 0.01037 0.43012 0.06994 0.05923 0.14584 0.01427 -0.00632 -0.00702 0.09167 0.01551 0.00107 0.00075 0.00081 0.00612 0.00799 0.00687 0.00742 0.00585 0.00709 0.00580 0.00431 H6B_b -0.08832 0.39534 0.03733 0.43012 0.11001 0.00612 0.00000 C5B_b -0.00947 0.49358 -0.09619 0.43012 0.03212 0.03445 0.16080 0.03018 0.00178 0.01195 0.07579 0.01313 0.00096 0.00068 0.00078 0.00612 0.00525 0.00484 0.00860 0.00543 0.00578 0.00368 0.00310 H5B_b -0.06368 0.42685 -0.14206 0.43012 0.09094 0.00612 0.00000 C4B_b 0.08449 0.60994 -0.13563 0.43012 0.01905 0.02983 0.18972 0.01721 0.00110 0.00329 0.07953 0.01622 0.00116 0.00079 0.00073 0.00612 0.00482 0.00506 0.00947 0.00664 0.00748 0.00410 0.00328 C3B_b 0.16381 0.70759 -0.06852 0.43012 0.03672 0.03092 0.19440 0.01022 0.01046 0.00252 0.08735 0.01623 0.00147 0.00086 0.00087 0.00612 0.00700 0.00523 0.01063 0.00675 0.00830 0.00506 0.00409 H3B_b 0.22803 0.78712 -0.09548 0.43012 0.10482 0.00612 0.00000 C2B_b 0.14918 0.68888 0.03805 0.43012 0.03702 0.02651 0.18628 -0.01984 0.01524 -0.00192 0.08327 0.01357 0.00140 0.00090 0.00083 0.00612 0.00712 0.00547 0.01080 0.00834 0.01089 0.00460 0.00424 H2B_b 0.20339 0.75561 0.08392 0.43012 0.09992 0.00612 0.00000 C7B_b 0.08368 0.63634 0.27034 0.43012 0.03482 0.03077 0.16768 0.02894 -0.04625 -0.01776 0.07776 0.02125 0.00206 0.00154 0.00119 0.00612 0.00673 0.00621 0.00930 0.00739 0.00762 0.00548 0.00437 C8B_b 0.01175 0.58325 0.37303 0.43012 0.04516 0.04455 0.19837 0.01451 0.02563 -0.00403 0.09603 0.02594 0.00215 0.00137 0.00115 0.00612 0.00680 0.00647 0.01054 0.00797 0.00987 0.00520 0.00409 H8B1_b 0.09617 0.60680 0.42838 0.43012 0.14404 0.00612 0.00000 H8B2_b -0.00472 0.47896 0.36994 0.43012 0.14404 0.00612 0.00000 H8B3_b -0.10277 0.62959 0.38725 0.43012 0.14404 0.00612 0.00000 C9B_b 0.09178 0.62891 -0.24566 0.43012 0.04019 0.02781 0.19215 0.02706 -0.00827 0.01067 0.08671 0.02711 0.00256 0.00183 0.00121 0.00612 0.00651 0.00579 0.01031 0.00785 0.01049 0.00498 0.00433 C10B_b 0.00516 0.53924 -0.32590 0.43012 0.03321 0.04252 0.20530 0.02834 -0.01851 -0.00832 0.09368 0.01880 0.00149 0.00111 0.00116 0.00612 0.00527 0.00594 0.01269 0.00685 0.00818 0.00481 0.00437 H10D_b 0.05807 0.56013 -0.39368 0.43012 0.14052 0.00612 0.00000 H10E_b -0.12248 0.56069 -0.32787 0.43012 0.14052 0.00612 0.00000 H10F_b 0.02257 0.43755 -0.30925 0.43012 0.14052 0.00612 0.00000 N1B_b 0.03286 0.55134 0.18374 0.43012 0.04031 0.02487 0.18460 -0.00038 0.01307 0.00899 0.08326 0.01592 0.00112 0.00082 0.00081 0.00612 0.00504 0.00398 0.00749 0.00505 0.00576 0.00395 0.00288 H1B_b -0.02249 0.47120 0.20005 0.43012 0.09991 0.00612 0.00000 O1B_b 0.12008 0.76633 0.26290 0.43012 0.06743 0.02479 0.23710 -0.00187 0.04272 -0.01144 0.10977 0.02089 0.00148 0.00081 0.00109 0.00612 0.00639 0.00408 0.01191 0.00483 0.00709 0.00460 0.00447 O2B_b 0.19698 0.72855 -0.27108 0.43012 0.05156 0.02740 0.19690 -0.00301 0.01664 -0.01224 0.09195 0.01558 0.00119 0.00081 0.00089 0.00612 0.00537 0.00417 0.00915 0.00473 0.00553 0.00357 0.00334 Final Structure Factor Calculation for 2008lsh167 in P2(1)2(1)2(1) Total number of l.s. parameters = 218 Maximum vector length = 511 Memory required = 3373 / 25046 wR2 = 0.1537 before cycle 23 for 1993 data and 2 / 218 parameters Disagreeable restraints before cycle 23 Observed Target Error Sigma Restraint -0.0315 0.0100 DELU C6B_b C2B_b 0.0301 0.0100 DELU C6B_b N1B_b 0.0324 0.0100 ISOR U22 C6B_b -0.0542 0.0100 ISOR U33 C6B_b Summary of restraints applied in cycle 23 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 30. 0. 0. 0. 60. 0. 6. 0. rms sigma 0.000 0.020 0.000 0.033 0.000 0.000 0.000 0.010 0.000 0.010 0.000 rms deviation 0.000 0.012 0.000 0.033 0.000 0.000 0.000 0.011 0.000 0.028 0.000 GooF = S = 1.162; Restrained GooF = 1.172 for 97 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0131 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0785 for 1414 Fo > 4sig(Fo) and 0.1192 for all 1993 data wR2 = 0.1537, GooF = S = 1.162, Restrained GooF = 1.172 for all data Occupancy sum of asymmetric unit = 13.00 for non-hydrogen and 11.00 for hydrogen atoms Principal mean square atomic displacements U 0.0465 0.0354 0.0207 C1A_a 0.0505 0.0301 0.0204 C2A_a 0.0510 0.0251 0.0190 C3A_a 0.0441 0.0370 0.0262 C4A_a 0.0663 0.0345 0.0169 C5A_a 0.0445 0.0200 0.0105 C6A_a 0.0581 0.0498 0.0176 C7A_a 0.0576 0.0478 0.0326 C8A_a 0.0943 0.0534 0.0338 C9A_a 0.0812 0.0558 0.0390 C10A_a 0.0540 0.0370 0.0252 N1A_a 0.0726 0.0474 0.0290 O1A_a 0.0691 0.0533 0.0421 O2A_a 0.1782 0.0437 0.0148 C1B_b 0.1488 0.0716 0.0546 C6B_b 0.1678 0.0413 0.0183 C5B_b 0.1916 0.0290 0.0180 C4B_b 0.1957 0.0366 0.0297 C3B_b 0.1902 0.0355 0.0241 C2B_b 0.1891 0.0304 0.0138 C7B_b 0.2037 0.0486 0.0358 C8B_b may be split into 0.0159 0.5851 0.3881 and 0.0076 0.5814 0.3580 0.1968 0.0461 0.0173 C9B_b 0.2122 0.0405 0.0283 C10B_b may be split into 0.0022 0.5430 -0.3102 and 0.0082 0.5355 -0.3416 0.1858 0.0435 0.0205 N1B_b 0.2473 0.0605 0.0215 O1B_b may be split into 0.1268 0.7659 0.2792 and 0.1134 0.7668 0.2466 0.1989 0.0548 0.0222 O2B_b Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.014 0.024 0.032 0.041 0.052 0.068 0.086 0.118 0.173 1.000 Number in group 203. 203. 198. 219. 190. 195. 191. 200. 194. 200. GooF 1.281 1.232 1.464 1.176 1.087 1.176 0.927 1.094 0.873 1.180 K 5.447 2.172 1.598 1.201 1.029 1.029 0.994 1.016 0.991 1.006 Resolution(A) 0.77 0.80 0.83 0.88 0.92 0.98 1.05 1.16 1.32 1.67 inf Number in group 200. 205. 196. 201. 196. 201. 196. 198. 204. 196. GooF 1.263 1.339 1.252 1.125 1.060 1.078 1.171 1.021 1.104 1.168 K 1.256 1.298 1.190 1.048 1.003 0.988 1.019 0.993 1.022 1.005 R1 0.348 0.365 0.274 0.185 0.140 0.110 0.071 0.057 0.066 0.033 Recommended weighting scheme: WGHT 0.0190 0.4179 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) 0 6 8 20.11 2.36 6.42 0.031 1.12 3 0 10 127.98 85.90 3.98 0.187 1.15 -1 2 10 55.67 30.06 3.84 0.111 1.23 1 3 15 13.37 3.01 3.52 0.035 0.82 -5 1 12 11.42 0.90 3.36 0.019 0.87 6 2 11 11.68 1.43 3.35 0.024 0.84 -5 8 7 15.29 0.08 3.33 0.006 0.82 -1 3 16 7.05 0.03 3.30 0.003 0.78 0 6 14 13.06 4.04 3.15 0.041 0.79 3 4 14 27.84 1.66 3.09 0.026 0.81 0 1 6 276.61 212.02 3.08 0.294 2.09 0 2 0 225.05 274.57 3.04 0.335 4.66 -2 1 16 9.21 1.34 2.94 0.023 0.79 1 2 10 58.49 29.84 2.90 0.110 1.23 4 4 12 11.22 3.48 2.89 0.038 0.87 2 1 11 5.91 0.47 2.86 0.014 1.11 -2 1 11 5.02 0.49 2.83 0.014 1.11 1 2 11 20.58 10.95 2.81 0.067 1.12 1 0 9 24.71 13.49 2.78 0.074 1.41 -5 2 12 8.98 1.75 2.77 0.027 0.86 -1 3 15 11.05 3.04 2.76 0.035 0.82 0 4 1 30.11 18.78 2.74 0.087 2.29 4 3 0 2267.61 2095.45 2.72 0.924 1.61 -4 2 15 8.16 1.21 2.67 0.022 0.77 -7 5 6 -1.26 3.90 2.64 0.040 0.85 -2 1 13 4.90 0.98 2.63 0.020 0.95 3 5 13 9.81 2.12 2.58 0.029 0.83 0 4 2 4.52 0.99 2.58 0.020 2.19 -2 11 3 20.51 11.33 2.55 0.068 0.81 4 1 11 10.97 4.82 2.53 0.044 0.99 1 0 16 3.81 0.06 2.52 0.005 0.80 4 8 0 11.40 5.80 2.50 0.049 0.99 4 0 10 73.58 94.95 2.50 0.197 1.06 -1 10 5 6.48 1.88 2.48 0.028 0.87 3 1 8 3.08 0.50 2.48 0.014 1.34 -5 6 8 4.82 0.07 2.45 0.005 0.90 3 3 11 6.95 1.94 2.44 0.028 1.00 0 8 12 10.03 0.99 2.41 0.020 0.79 5 1 12 10.65 0.90 2.40 0.019 0.87 1 0 13 6.16 0.62 2.39 0.016 0.98 0 0 12 17.47 9.58 2.39 0.063 1.07 3 9 6 21.96 10.44 2.38 0.065 0.87 2 5 0 146.28 171.17 2.38 0.264 1.67 8 3 7 14.22 0.48 2.37 0.014 0.81 -1 2 13 9.60 3.84 2.36 0.040 0.96 -7 6 7 9.27 3.03 2.35 0.035 0.80 3 0 6 5.84 0.02 2.34 0.003 1.63 3 1 14 6.09 0.13 2.34 0.007 0.86 3 0 12 26.71 17.42 2.33 0.084 0.99 0 1 13 1.95 6.72 2.32 0.052 0.99 Bond lengths and angles C1A_a - Distance Angles C2A_a 1.3900 C6A_a 1.3900 120.00 N1A_a 1.4125 (0.0051) 124.67 (0.33) 115.31 (0.33) C1A_a - C2A_a C6A_a C2A_a - Distance Angles C3A_a 1.3900 C1A_a 1.3900 120.00 H2A_a 0.9500 120.00 120.00 C2A_a - C3A_a C1A_a C3A_a - Distance Angles C2A_a 1.3900 C4A_a 1.3900 120.00 H3A_a 0.9500 120.00 120.00 C3A_a - C2A_a C4A_a C4A_a - Distance Angles C3A_a 1.3900 C5A_a 1.3900 120.00 C9A_a 1.4531 (0.0081) 118.57 (0.55) 121.21 (0.56) C4A_a - C3A_a C5A_a C5A_a - Distance Angles C6A_a 1.3900 C4A_a 1.3900 120.00 H5A_a 0.9500 120.00 120.00 C5A_a - C6A_a C4A_a C6A_a - Distance Angles C5A_a 1.3900 C1A_a 1.3900 120.00 H6A_a 0.9500 120.00 120.00 C6A_a - C5A_a C1A_a C7A_a - Distance Angles O1A_a 1.2106 (0.0099) N1A_a 1.4124 (0.0090) 125.72 (0.66) C8A_a 1.5019 (0.0093) 121.98 (0.67) 112.20 (0.71) C7A_a - O1A_a N1A_a C8A_a - Distance Angles C7A_a 1.5019 (0.0093) H8A1_a 0.9800 109.47 H8A2_a 0.9800 109.47 109.47 H8A3_a 0.9800 109.47 109.47 109.47 C8A_a - C7A_a H8A1_a H8A2_a C9A_a - Distance Angles O2A_a 1.2552 (0.0127) C4A_a 1.4531 (0.0081) 118.23 (0.87) C10A_a 1.4970 (0.0119) 116.79 (0.77) 123.23 (0.87) C9A_a - O2A_a C4A_a C10A_a - Distance Angles C9A_a 1.4970 (0.0119) H10A_a 0.9800 109.47 H10B_a 0.9800 109.47 109.47 H10C_a 0.9800 109.47 109.47 109.47 C10A_a - C9A_a H10A_a H10B_a N1A_a - Distance Angles C7A_a 1.4124 (0.0090) C1A_a 1.4125 (0.0051) 126.12 (0.53) H1A_a 0.8800 116.94 116.94 N1A_a - C7A_a C1A_a O1A_a - Distance Angles C7A_a 1.2106 (0.0099) O1A_a - O2A_a - Distance Angles C9A_a 1.2552 (0.0128) O2A_a - C1B_b - Distance Angles C6B_b 1.3900 C2B_b 1.3900 120.00 N1B_b 1.3949 (0.0104) 117.90 (0.67) 122.08 (0.67) C1B_b - C6B_b C2B_b C6B_b - Distance Angles C1B_b 1.3900 C5B_b 1.3900 120.00 H6B_b 0.9500 120.00 120.00 C6B_b - C1B_b C5B_b C5B_b - Distance Angles C6B_b 1.3900 C4B_b 1.3900 120.00 H5B_b 0.9500 120.00 120.00 C5B_b - C6B_b C4B_b C4B_b - Distance Angles C3B_b 1.3900 C5B_b 1.3900 120.00 C9B_b 1.4314 (0.0149) 121.36 (0.81) 118.60 (0.81) C4B_b - C3B_b C5B_b C3B_b - Distance Angles C4B_b 1.3900 C2B_b 1.3900 120.00 H3B_b 0.9500 120.00 120.00 C3B_b - C4B_b C2B_b C2B_b - Distance Angles C3B_b 1.3900 C1B_b 1.3900 120.00 H2B_b 0.9500 120.00 120.00 C2B_b - C3B_b C1B_b C7B_b - Distance Angles O1B_b 1.2450 (0.0138) N1B_b 1.4215 (0.0139) 122.69 (1.39) C8B_b 1.5138 (0.0154) 117.62 (1.30) 114.19 (0.98) C7B_b - O1B_b N1B_b C8B_b - Distance Angles C7B_b 1.5138 (0.0154) H8B1_b 0.9800 109.47 H8B2_b 0.9800 109.47 109.47 H8B3_b 0.9800 109.47 109.47 109.47 C8B_b - C7B_b H8B1_b H8B2_b C9B_b - Distance Angles O2B_b 1.2624 (0.0154) C4B_b 1.4314 (0.0149) 111.86 (1.25) C10B_b 1.4807 (0.0161) 120.56 (1.32) 127.35 (1.26) C9B_b - O2B_b C4B_b C10B_b - Distance Angles C9B_b 1.4807 (0.0161) H10D_b 0.9800 109.47 H10E_b 0.9800 109.47 109.47 H10F_b 0.9800 109.47 109.47 109.47 C10B_b - C9B_b H10D_b H10E_b N1B_b - Distance Angles C1B_b 1.3949 (0.0104) C7B_b 1.4215 (0.0139) 131.39 (0.93) H1B_b 0.8800 114.31 114.31 N1B_b - C1B_b C7B_b O1B_b - Distance Angles C7B_b 1.2450 (0.0139) O1B_b - O2B_b - Distance Angles C9B_b 1.2624 (0.0154) O2B_b - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.04 2.919(7) 175.3 N1A_a-H1A_a...O1A_$1a 0.88 2.10 2.974(12) 172.1 N1B_b-H1B_b...O1B_$2b FMAP and GRID set by program FMAP 2 1 12 GRID -2.778 -2 -2 2.778 2 2 R1 = 0.1099 for 1195 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.13 at 0.0327 0.2678 0.5057 [ 1.63 A from C2A ] Deepest hole -0.15 at -0.0087 0.7200 0.6777 [ 1.11 A from C7A ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 3374 / 16179 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0327 0.7678 -0.0057 1.00000 0.05 0.13 1.63 C2A 1.65 C2B 1.77 C3B 1.85 C3A Q2 1 0.0667 0.6348 -0.1576 1.00000 0.05 0.13 0.39 C4B 0.92 N1A 1.14 C1A 1.15 C9B Q3 1 -0.0332 0.4774 0.0731 1.00000 0.05 0.13 0.33 C5A 0.81 C6B 0.98 H5A 0.98 H6B Q4 1 0.0979 0.8155 -0.1776 1.00000 0.05 0.12 1.12 O1A 1.46 H10F 1.47 H3B 1.56 H2A Q5 1 0.0770 0.6275 0.1589 1.00000 0.05 0.12 0.38 C4A 0.85 N1B 1.10 C9A 1.18 C1B Shortest distances between peaks (including symmetry equivalents) 2 4 1.72 3 5 1.97 1 2 2.44 1 4 2.46 1 5 2.63 1 3 2.89 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 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.38: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.08: Set up l.s. refinement 0.00: Generate idealized H-atoms 7.89: Structure factors and derivatives 3.17: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.17: Apply other restraints 0.73: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxl finished at 09:34:58 Total CPU time: 12.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++