++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XL - CRYSTAL STRUCTURE REFINEMENT - SHELXTL Ver. 6.12 W95/98/NT/2000/ME + + Copyright(c) 2001 Bruker Analytical X-ray Solutions All Rights Reserved + + b started at 12:27:50 on 30-Mar-2009 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL g in P2(1)/c CELL 0.71073 12.0632 17.4713 11.7628 90.000 105.363 90.000 ZERR 4.00 0.0015 0.0023 0.0011 0.000 0.007 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 108 116 12 12 V = 2390.54 F(000) = 944.0 Mu = 0.08 mm-1 Cell Wt = 1774.13 Rho = 1.232 TEMP -153 L.S. 6 BOND $H FMAP 2 PLAN 20 ACTA SIZE 0.2 0.1 0.03 OMIT -3 55 SHEL 7 0.77 WGHT 0.0459 2.6476 FVAR 0.23057 N1 3 0.12684 0.37135 -0.28651 11.00000 0.02968 0.03154 = 0.02810 -0.00132 0.00727 -0.00004 N2 3 0.04323 0.25884 -0.38246 11.00000 0.03793 0.03290 = 0.02952 -0.00552 0.01031 0.00603 AFIX 43 H2 2 0.06080 0.21474 -0.40940 11.00000 -1.20000 AFIX 0 N3 3 0.23032 0.25907 -0.25524 11.00000 0.03179 0.03711 = 0.03015 -0.00320 0.00835 0.00559 O1 4 0.53505 0.43641 -0.25079 11.00000 0.03979 0.08261 = 0.06321 -0.01217 0.02127 -0.01388 O2 4 0.05222 0.38714 0.00773 11.00000 0.06367 0.03726 = 0.05041 0.00444 0.03653 0.00610 O3 4 0.19143 0.36788 -0.07784 11.00000 0.04243 0.03325 = 0.02819 0.00128 0.01432 0.00747 C1 1 0.31185 0.32059 -0.19473 11.00000 0.03116 0.04502 = 0.02328 -0.00361 0.00542 0.00172 C2 1 0.39015 0.29482 -0.07616 11.00000 0.04160 0.05424 = 0.02733 -0.00542 0.00493 0.01056 AFIX 137 H2A 2 0.34311 0.28035 -0.02325 11.00000 -1.50000 H2B 2 0.44158 0.33688 -0.04095 11.00000 -1.50000 H2C 2 0.43588 0.25073 -0.08835 11.00000 -1.50000 AFIX 0 C3 1 0.38085 0.34627 -0.28121 11.00000 0.02886 0.05464 = 0.02819 -0.00452 0.00883 0.00106 AFIX 13 H3 2 0.32419 0.35382 -0.35955 11.00000 -1.20000 AFIX 0 C4 1 0.46860 0.28801 -0.29934 11.00000 0.03360 0.07554 = 0.04039 -0.00969 0.01188 0.01176 AFIX 137 H4A 2 0.49683 0.30339 -0.36677 11.00000 -1.50000 H4B 2 0.43227 0.23752 -0.31458 11.00000 -1.50000 H4C 2 0.53311 0.28563 -0.22835 11.00000 -1.50000 AFIX 0 C5 1 0.43698 0.42320 -0.24463 11.00000 0.03385 0.06987 = 0.03110 0.00234 0.00676 -0.00666 C6 1 0.37117 0.48333 -0.20173 11.00000 0.03264 0.04603 = 0.03695 -0.00114 0.00888 -0.00700 C7 1 0.42888 0.56090 -0.18982 11.00000 0.04601 0.06151 = 0.06047 0.00250 0.01208 -0.01299 AFIX 137 H7A 2 0.42957 0.57982 -0.26806 11.00000 -1.50000 H7B 2 0.50803 0.55628 -0.14059 11.00000 -1.50000 H7C 2 0.38643 0.59684 -0.15309 11.00000 -1.50000 AFIX 0 C8 1 0.27001 0.46598 -0.17886 11.00000 0.04167 0.03918 = 0.02208 0.00130 0.00426 0.00150 C9 1 0.19256 0.52276 -0.13637 11.00000 0.03918 0.03213 = 0.03429 0.00010 0.01039 0.00307 C10 1 0.25170 0.55202 -0.01122 11.00000 0.05518 0.04090 = 0.04458 -0.00922 0.00971 -0.00040 AFIX 137 H10A 2 0.27232 0.50841 0.04265 11.00000 -1.50000 H10B 2 0.19899 0.58577 0.01582 11.00000 -1.50000 H10C 2 0.32134 0.58045 -0.01265 11.00000 -1.50000 AFIX 0 C11 1 0.15515 0.59036 -0.22283 11.00000 0.04793 0.04255 = 0.06061 0.01005 0.01373 -0.00593 AFIX 137 H11A 2 0.22163 0.62321 -0.22028 11.00000 -1.50000 H11B 2 0.09564 0.62017 -0.20004 11.00000 -1.50000 H11C 2 0.12448 0.57057 -0.30298 11.00000 -1.50000 AFIX 0 C12 1 0.08040 0.48271 -0.12976 11.00000 0.04170 0.03241 = 0.03314 -0.00099 0.01460 0.00628 AFIX 23 H12A 2 0.03589 0.51754 -0.09216 11.00000 -1.20000 H12B 2 0.03316 0.47152 -0.21061 11.00000 -1.20000 AFIX 0 C13 1 0.10394 0.41009 -0.06128 11.00000 0.04520 0.03287 = 0.03143 -0.00493 0.01423 0.00700 C14 1 0.22681 0.38437 -0.18841 11.00000 0.03429 0.03991 = 0.02522 -0.00237 0.01101 0.00183 C15 1 0.12977 0.29879 -0.30796 11.00000 0.03299 0.03727 = 0.02385 0.00096 0.01319 0.00410 C16 1 -0.07245 0.28299 -0.41956 11.00000 0.03754 0.03412 = 0.03395 0.00569 0.01101 -0.00534 C17 1 -0.12490 0.32200 -0.34565 11.00000 0.03771 0.04191 = 0.04150 -0.00080 0.01227 -0.00200 AFIX 43 H17 2 -0.08141 0.33601 -0.26872 11.00000 -1.20000 AFIX 0 C18 1 -0.24108 0.34089 -0.38327 11.00000 0.03957 0.04117 = 0.07214 0.00423 0.02229 0.00130 AFIX 43 H18 2 -0.27685 0.36784 -0.33241 11.00000 -1.20000 AFIX 0 C19 1 -0.30374 0.32018 -0.49491 11.00000 0.02768 0.06768 = 0.07458 0.02123 0.00546 -0.00798 AFIX 43 H19 2 -0.38313 0.33258 -0.52082 11.00000 -1.20000 AFIX 0 C20 1 -0.25203 0.28172 -0.56879 11.00000 0.04117 0.08420 = 0.04708 0.00720 -0.00099 -0.02338 AFIX 43 H20 2 -0.29547 0.26816 -0.64594 11.00000 -1.20000 AFIX 0 C21 1 -0.13616 0.26257 -0.53096 11.00000 0.03942 0.05609 = 0.03636 -0.00055 0.01067 -0.01253 AFIX 43 H21 2 -0.10085 0.23537 -0.58195 11.00000 -1.20000 AFIX 0 C22 1 0.22230 0.18592 -0.19955 11.00000 0.03815 0.03723 = 0.03032 -0.00270 0.00843 0.00647 C23 1 0.14911 0.17621 -0.12742 11.00000 0.04730 0.03071 = 0.03460 -0.00299 0.00960 0.00929 AFIX 43 H23 2 0.10335 0.21791 -0.11458 11.00000 -1.20000 AFIX 0 C24 1 0.14203 0.10680 -0.07421 11.00000 0.04875 0.04668 = 0.03554 -0.00321 0.00938 0.00092 AFIX 43 H24 2 0.09097 0.10054 -0.02574 11.00000 -1.20000 AFIX 0 C25 1 0.20906 0.04674 -0.09152 11.00000 0.06752 0.04302 = 0.06244 0.00909 0.01497 0.00773 AFIX 43 H25 2 0.20550 -0.00084 -0.05357 11.00000 -1.20000 AFIX 0 C26 1 0.28150 0.05513 -0.16369 11.00000 0.08412 0.04472 = 0.12222 0.02007 0.05546 0.03062 AFIX 43 H26 2 0.32676 0.01305 -0.17615 11.00000 -1.20000 AFIX 0 C27 1 0.28876 0.12502 -0.21853 11.00000 0.06873 0.04975 = 0.08363 0.00577 0.04300 0.02015 AFIX 43 H27 2 0.33868 0.13080 -0.26831 11.00000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for g in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 N1 - C15 C14 N2 - C15 C16 N3 - C15 C22 C1 O1 - C5 O2 - C13 O3 - C13 C14 C1 - N3 C14 C2 C3 C2 - C1 C3 - C5 C4 C1 C4 - C3 C5 - O1 C6 C3 C6 - C8 C5 C7 C7 - C6 C8 - C6 C14 C9 C9 - C8 C10 C12 C11 C10 - C9 C11 - C9 C12 - C13 C9 C13 - O2 O3 C12 C14 - N1 O3 C8 C1 C15 - N1 N2 N3 C16 - C21 C17 N2 C17 - C16 C18 C18 - C19 C17 C19 - C20 C18 C20 - C19 C21 C21 - C16 C20 C22 - C27 C23 N3 C23 - C24 C22 C24 - C25 C23 C25 - C24 C26 C26 - C25 C27 C27 - C22 C26 46433 Reflections read, of which 981 rejected -15 =< h =< 15, -21 =< k =< 21, -14 =< l =< 14, Max. 2-theta = 53.26 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 4 17 0 5.21 2.02 6 26.99 -11 8 1 3.37 1.48 6 28.22 -10 10 1 10.36 1.98 6 18.78 -3 10 1 6.45 1.07 8 6.50 7 14 1 2.12 2.44 4 17.44 -6 16 1 3.60 1.87 6 12.16 1 18 1 2.74 2.00 5 20.98 -11 8 2 1.47 1.34 6 16.81 -4 17 2 0.70 1.85 6 12.06 -12 5 3 4.32 2.81 3 53.72 -1 17 4 7.71 2.40 4 15.24 3 15 5 4.22 2.58 3 30.74 -10 14 6 3.23 3.30 3 24.86 10 2 7 5.38 5.40 2 32.72 5 11 7 6.40 1.91 5 11.23 2 12 8 3.39 2.41 5 27.84 -10 5 9 8.82 1.81 5 22.48 -2 12 9 3.88 2.70 4 16.70 -3 10 10 2.25 1.94 6 22.05 5 1 11 7.01 2.99 3 16.74 -7 4 11 3.77 1.35 7 11.17 -2 7 11 3.55 1.68 6 20.77 3 2 12 2.09 1.08 4 18.17 23 Inconsistent equivalents 4937 Unique reflections, of which 0 suppressed R(int) = 0.1872 R(sigma) = 0.1310 Friedel opposites merged Maximum memory for data reduction = 3052 / 48958 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 = 3925 / 379323 wR2 = 0.1954 before cycle 1 for 4937 data and 303 / 303 parameters GooF = S = 1.114; Restrained GooF = 1.114 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0459 * P )^2 + 2.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23035 0.00061 -0.363 OSF Mean shift/esd = 0.020 Maximum = -0.363 for OSF Max. shift = 0.001 A for H2B Max. dU = 0.000 for C26 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3925 / 379323 wR2 = 0.1953 before cycle 2 for 4937 data and 303 / 303 parameters GooF = S = 1.113; Restrained GooF = 1.113 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0459 * P )^2 + 2.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23030 0.00060 -0.091 OSF Mean shift/esd = 0.007 Maximum = -0.091 for OSF Max. shift = 0.000 A for H2B Max. dU = 0.000 for O2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3925 / 379323 wR2 = 0.1953 before cycle 3 for 4937 data and 303 / 303 parameters GooF = S = 1.113; Restrained GooF = 1.113 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0459 * P )^2 + 2.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23029 0.00060 -0.004 OSF Mean shift/esd = 0.001 Maximum = -0.004 for OSF Max. shift = 0.000 A for H10B Max. dU = 0.000 for C7 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3925 / 379323 wR2 = 0.1953 before cycle 4 for 4937 data and 303 / 303 parameters GooF = S = 1.113; Restrained GooF = 1.113 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0459 * P )^2 + 2.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23029 0.00060 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y C2 Max. shift = 0.000 A for H2A Max. dU = 0.000 for C7 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3925 / 379323 wR2 = 0.1953 before cycle 5 for 4937 data and 303 / 303 parameters GooF = S = 1.113; Restrained GooF = 1.113 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0459 * P )^2 + 2.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23029 0.00060 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H7A Max. dU = 0.000 for C16 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3925 / 379323 wR2 = 0.1953 before cycle 6 for 4937 data and 303 / 303 parameters GooF = S = 1.113; Restrained GooF = 1.113 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0459 * P )^2 + 2.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23029 0.00060 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H2A Max. dU = 0.000 for C4 Largest correlation matrix elements 0.505 U13 C27 / U33 C27 0.503 U13 C26 / U11 C26 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.0608 0.2147 -0.4094 43 0.880 0.000 N2 C15 C16 H2A 0.3431 0.2803 -0.0233 137 0.980 0.000 C2 C1 H2A H2B 0.4415 0.3369 -0.0409 137 0.980 0.000 C2 C1 H2A H2C 0.4359 0.2508 -0.0884 137 0.980 0.000 C2 C1 H2A H3 0.3242 0.3538 -0.3595 13 1.000 0.000 C3 C5 C4 C1 H4A 0.4968 0.3034 -0.3668 137 0.980 0.000 C4 C3 H4A H4B 0.4323 0.2375 -0.3145 137 0.980 0.000 C4 C3 H4A H4C 0.5331 0.2856 -0.2284 137 0.980 0.000 C4 C3 H4A H7A 0.4296 0.5798 -0.2680 137 0.980 0.000 C7 C6 H7A H7B 0.5080 0.5563 -0.1406 137 0.980 0.000 C7 C6 H7A H7C 0.3864 0.5968 -0.1531 137 0.980 0.000 C7 C6 H7A H10A 0.2723 0.5084 0.0426 137 0.980 0.000 C10 C9 H10A H10B 0.1990 0.5858 0.0158 137 0.980 0.000 C10 C9 H10A H10C 0.3213 0.5805 -0.0127 137 0.980 0.000 C10 C9 H10A H11A 0.2216 0.6232 -0.2203 137 0.980 0.000 C11 C9 H11A H11B 0.0956 0.6202 -0.2001 137 0.980 0.000 C11 C9 H11A H11C 0.1245 0.5706 -0.3030 137 0.980 0.000 C11 C9 H11A H12A 0.0359 0.5175 -0.0921 23 0.990 0.000 C12 C13 C9 H12B 0.0331 0.4715 -0.2106 23 0.990 0.000 C12 C13 C9 H17 -0.0814 0.3360 -0.2687 43 0.950 0.000 C17 C16 C18 H18 -0.2769 0.3678 -0.3324 43 0.950 0.000 C18 C19 C17 H19 -0.3831 0.3326 -0.5208 43 0.950 0.000 C19 C20 C18 H20 -0.2955 0.2681 -0.6459 43 0.950 0.000 C20 C19 C21 H21 -0.1008 0.2354 -0.5819 43 0.950 0.000 C21 C16 C20 H23 0.1033 0.2179 -0.1146 43 0.950 0.000 C23 C24 C22 H24 0.0910 0.1006 -0.0257 43 0.950 0.000 C24 C25 C23 H25 0.2055 -0.0008 -0.0535 43 0.950 0.000 C25 C24 C26 H26 0.3268 0.0130 -0.1762 43 0.950 0.000 C26 C25 C27 H27 0.3387 0.1308 -0.2683 43 0.950 0.000 C27 C22 C26 g in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq N1 0.12682 0.37135 -0.28651 1.00000 0.02956 0.03139 0.02801 -0.00130 0.00724 -0.00001 0.02973 0.00560 0.00025 0.00018 0.00024 0.00000 0.00180 0.00200 0.00165 0.00144 0.00140 0.00153 0.00075 N2 0.04323 0.25883 -0.38248 1.00000 0.03782 0.03279 0.02944 -0.00552 0.01026 0.00602 0.03309 0.00593 0.00027 0.00018 0.00024 0.00000 0.00203 0.00194 0.00165 0.00147 0.00152 0.00163 0.00079 H2 0.06080 0.21474 -0.40942 1.00000 0.03971 0.00000 0.00000 N3 0.23033 0.25906 -0.25524 1.00000 0.03167 0.03700 0.03010 -0.00322 0.00836 0.00557 0.03289 0.00582 0.00026 0.00018 0.00025 0.00000 0.00190 0.00202 0.00163 0.00151 0.00145 0.00159 0.00079 O1 0.53505 0.43640 -0.25080 1.00000 0.03964 0.08244 0.06311 -0.01221 0.02121 -0.01384 0.06029 0.00583 0.00026 0.00019 0.00026 0.00000 0.00195 0.00255 0.00199 0.00180 0.00162 0.00177 0.00092 O2 0.05222 0.38714 0.00774 1.00000 0.06349 0.03718 0.05025 0.00448 0.03648 0.00611 0.04624 0.00570 0.00025 0.00016 0.00024 0.00000 0.00201 0.00176 0.00170 0.00140 0.00161 0.00151 0.00077 O3 0.19144 0.36788 -0.07785 1.00000 0.04232 0.03311 0.02811 0.00126 0.01431 0.00747 0.03357 0.00483 0.00022 0.00014 0.00020 0.00000 0.00162 0.00161 0.00134 0.00116 0.00119 0.00133 0.00066 C1 0.31187 0.32059 -0.19472 1.00000 0.03110 0.04495 0.02315 -0.00363 0.00538 0.00177 0.03341 0.00701 0.00032 0.00023 0.00029 0.00000 0.00216 0.00255 0.00186 0.00182 0.00165 0.00198 0.00095 C2 0.39015 0.29482 -0.07616 1.00000 0.04142 0.05412 0.02721 -0.00540 0.00485 0.01050 0.04172 0.00764 0.00035 0.00025 0.00030 0.00000 0.00247 0.00283 0.00199 0.00198 0.00182 0.00221 0.00107 H2A 0.34310 0.28032 -0.02327 1.00000 0.06258 0.00000 0.00000 H2B 0.44154 0.33690 -0.04091 1.00000 0.06258 0.00000 0.00000 H2C 0.43593 0.25076 -0.08835 1.00000 0.06258 0.00000 0.00000 C3 0.38085 0.34627 -0.28120 1.00000 0.02876 0.05453 0.02814 -0.00453 0.00884 0.00110 0.03690 0.00746 0.00032 0.00024 0.00032 0.00000 0.00219 0.00287 0.00200 0.00193 0.00171 0.00206 0.00101 H3 0.32419 0.35382 -0.35954 1.00000 0.04428 0.00000 0.00000 C4 0.46860 0.28799 -0.29933 1.00000 0.03356 0.07544 0.04032 -0.00971 0.01184 0.01175 0.04938 0.00832 0.00034 0.00028 0.00035 0.00000 0.00247 0.00341 0.00232 0.00232 0.00194 0.00240 0.00120 H4A 0.49681 0.30336 -0.36678 1.00000 0.07408 0.00000 0.00000 H4B 0.43228 0.23751 -0.31453 1.00000 0.07408 0.00000 0.00000 H4C 0.53313 0.28563 -0.22836 1.00000 0.07408 0.00000 0.00000 C5 0.43700 0.42319 -0.24462 1.00000 0.03383 0.06977 0.03099 0.00232 0.00671 -0.00667 0.04522 0.00811 0.00037 0.00027 0.00033 0.00000 0.00261 0.00341 0.00215 0.00221 0.00190 0.00239 0.00115 C6 0.37116 0.48332 -0.20173 1.00000 0.03255 0.04586 0.03687 -0.00118 0.00884 -0.00698 0.03850 0.00743 0.00034 0.00024 0.00033 0.00000 0.00236 0.00269 0.00222 0.00199 0.00188 0.00211 0.00101 C7 0.42888 0.56090 -0.18981 1.00000 0.04585 0.06143 0.06035 0.00250 0.01205 -0.01302 0.05626 0.00847 0.00039 0.00026 0.00040 0.00000 0.00290 0.00335 0.00290 0.00256 0.00234 0.00256 0.00129 H7A 0.42956 0.57983 -0.26805 1.00000 0.08439 0.00000 0.00000 H7B 0.50803 0.55629 -0.14059 1.00000 0.08439 0.00000 0.00000 H7C 0.38643 0.59684 -0.15306 1.00000 0.08439 0.00000 0.00000 C8 0.27003 0.46598 -0.17887 1.00000 0.04153 0.03909 0.02200 0.00131 0.00425 0.00154 0.03500 0.00724 0.00034 0.00023 0.00030 0.00000 0.00248 0.00250 0.00189 0.00178 0.00173 0.00207 0.00097 C9 0.19257 0.52277 -0.13637 1.00000 0.03916 0.03200 0.03415 0.00010 0.01030 0.00305 0.03499 0.00740 0.00033 0.00023 0.00032 0.00000 0.00244 0.00234 0.00211 0.00184 0.00184 0.00195 0.00097 C10 0.25170 0.55202 -0.01123 1.00000 0.05511 0.04085 0.04449 -0.00923 0.00971 -0.00044 0.04748 0.00782 0.00039 0.00025 0.00035 0.00000 0.00294 0.00271 0.00246 0.00209 0.00216 0.00227 0.00116 H10A 0.27234 0.50840 0.04263 1.00000 0.07121 0.00000 0.00000 H10B 0.19899 0.58575 0.01584 1.00000 0.07121 0.00000 0.00000 H10C 0.32133 0.58047 -0.01265 1.00000 0.07121 0.00000 0.00000 C11 0.15515 0.59037 -0.22283 1.00000 0.04780 0.04244 0.06055 0.01008 0.01372 -0.00590 0.05038 0.00871 0.00038 0.00025 0.00038 0.00000 0.00283 0.00284 0.00281 0.00227 0.00229 0.00227 0.00119 H11A 0.22162 0.62322 -0.22027 1.00000 0.07558 0.00000 0.00000 H11B 0.09562 0.62016 -0.20006 1.00000 0.07558 0.00000 0.00000 H11C 0.12451 0.57058 -0.30298 1.00000 0.07558 0.00000 0.00000 C12 0.08039 0.48271 -0.12975 1.00000 0.04155 0.03226 0.03310 -0.00095 0.01451 0.00634 0.03476 0.00754 0.00033 0.00022 0.00032 0.00000 0.00246 0.00243 0.00209 0.00181 0.00185 0.00195 0.00098 H12A 0.03589 0.51754 -0.09214 1.00000 0.04171 0.00000 0.00000 H12B 0.03314 0.47154 -0.21060 1.00000 0.04171 0.00000 0.00000 C13 0.10392 0.41008 -0.06127 1.00000 0.04512 0.03279 0.03139 -0.00491 0.01410 0.00694 0.03568 0.00749 0.00036 0.00023 0.00032 0.00000 0.00258 0.00245 0.00209 0.00184 0.00196 0.00209 0.00098 C14 0.22681 0.38437 -0.18840 1.00000 0.03420 0.03976 0.02512 -0.00243 0.01097 0.00184 0.03244 0.00712 0.00032 0.00022 0.00030 0.00000 0.00227 0.00249 0.00193 0.00180 0.00170 0.00197 0.00094 C15 0.12976 0.29879 -0.30797 1.00000 0.03286 0.03728 0.02378 0.00101 0.01318 0.00411 0.03022 0.00732 0.00032 0.00023 0.00029 0.00000 0.00226 0.00253 0.00185 0.00180 0.00171 0.00199 0.00091 C16 -0.07246 0.28299 -0.41957 1.00000 0.03741 0.03396 0.03383 0.00568 0.01093 -0.00536 0.03479 0.00739 0.00033 0.00023 0.00032 0.00000 0.00246 0.00247 0.00215 0.00186 0.00188 0.00201 0.00098 C17 -0.12489 0.32200 -0.34565 1.00000 0.03761 0.04181 0.04142 -0.00078 0.01220 -0.00199 0.03995 0.00794 0.00035 0.00024 0.00035 0.00000 0.00248 0.00260 0.00227 0.00205 0.00196 0.00212 0.00102 H17 -0.08139 0.33600 -0.26872 1.00000 0.04794 0.00000 0.00000 C18 -0.24108 0.34090 -0.38326 1.00000 0.03950 0.04104 0.07206 0.00423 0.02225 0.00129 0.04945 0.00913 0.00037 0.00026 0.00043 0.00000 0.00275 0.00282 0.00323 0.00238 0.00248 0.00219 0.00118 H18 -0.27685 0.36784 -0.33240 1.00000 0.05934 0.00000 0.00000 C19 -0.30374 0.32018 -0.49491 1.00000 0.02762 0.06753 0.07450 0.02120 0.00542 -0.00796 0.05809 0.00947 0.00038 0.00029 0.00045 0.00000 0.00248 0.00357 0.00344 0.00292 0.00253 0.00248 0.00136 H19 -0.38313 0.33261 -0.52083 1.00000 0.06971 0.00000 0.00000 C20 -0.25203 0.28172 -0.56880 1.00000 0.04110 0.08412 0.04697 0.00716 -0.00099 -0.02345 0.05980 0.00891 0.00040 0.00031 0.00041 0.00000 0.00291 0.00396 0.00266 0.00266 0.00230 0.00274 0.00140 H20 -0.29548 0.26814 -0.64595 1.00000 0.07176 0.00000 0.00000 C21 -0.13615 0.26256 -0.53096 1.00000 0.03927 0.05597 0.03627 -0.00052 0.01065 -0.01241 0.04372 0.00770 0.00036 0.00025 0.00034 0.00000 0.00270 0.00299 0.00226 0.00211 0.00201 0.00222 0.00111 H21 -0.10083 0.23537 -0.58195 1.00000 0.05246 0.00000 0.00000 C22 0.22230 0.18592 -0.19955 1.00000 0.03806 0.03717 0.03022 -0.00271 0.00838 0.00648 0.03528 0.00727 0.00033 0.00023 0.00031 0.00000 0.00238 0.00253 0.00200 0.00189 0.00183 0.00201 0.00097 C23 0.14911 0.17622 -0.12742 1.00000 0.04715 0.03067 0.03447 -0.00296 0.00953 0.00931 0.03767 0.00744 0.00035 0.00023 0.00032 0.00000 0.00258 0.00240 0.00209 0.00189 0.00192 0.00205 0.00099 H23 0.10335 0.21792 -0.11458 1.00000 0.04521 0.00000 0.00000 C24 0.14203 0.10681 -0.07421 1.00000 0.04862 0.04657 0.03548 -0.00324 0.00938 0.00090 0.04389 0.00776 0.00038 0.00025 0.00034 0.00000 0.00272 0.00289 0.00227 0.00210 0.00200 0.00236 0.00110 H24 0.09096 0.10055 -0.02574 1.00000 0.05267 0.00000 0.00000 C25 0.20906 0.04674 -0.09151 1.00000 0.06737 0.04309 0.06231 0.00916 0.01495 0.00774 0.05801 0.00931 0.00043 0.00028 0.00042 0.00000 0.00348 0.00307 0.00302 0.00242 0.00269 0.00266 0.00132 H25 0.20551 -0.00084 -0.05354 1.00000 0.06961 0.00000 0.00000 C26 0.28151 0.05512 -0.16370 1.00000 0.08400 0.04462 0.12200 0.02007 0.05534 0.03059 0.07821 0.01189 0.00049 0.00029 0.00053 0.00000 0.00415 0.00329 0.00485 0.00327 0.00388 0.00306 0.00176 H26 0.32677 0.01304 -0.17617 1.00000 0.09385 0.00000 0.00000 C27 0.28876 0.12502 -0.21854 1.00000 0.06863 0.04969 0.08349 0.00578 0.04293 0.02017 0.06294 0.01035 0.00044 0.00028 0.00046 0.00000 0.00347 0.00321 0.00357 0.00278 0.00293 0.00272 0.00142 H27 0.33867 0.13081 -0.26832 1.00000 0.07553 0.00000 0.00000 Final Structure Factor Calculation for g in P2(1)/c Total number of l.s. parameters = 303 Maximum vector length = 511 Memory required = 3622 / 22995 wR2 = 0.1953 before cycle 7 for 4937 data and 0 / 303 parameters GooF = S = 1.113; Restrained GooF = 1.113 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0459 * P )^2 + 2.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1086 for 2829 Fo > 4sig(Fo) and 0.1906 for all 4937 data wR2 = 0.1953, GooF = S = 1.113, Restrained GooF = 1.113 for all data Occupancy sum of asymmetric unit = 33.00 for non-hydrogen and 29.00 for hydrogen atoms Principal mean square atomic displacements U 0.0319 0.0297 0.0276 N1 0.0431 0.0341 0.0220 N2 0.0420 0.0308 0.0259 N3 0.0909 0.0572 0.0327 O1 0.0760 0.0360 0.0267 O2 0.0468 0.0299 0.0240 O3 0.0461 0.0315 0.0225 C1 0.0633 0.0357 0.0262 C2 0.0555 0.0294 0.0258 C3 0.0820 0.0397 0.0264 C4 0.0715 0.0337 0.0304 C5 0.0489 0.0371 0.0295 C6 0.0718 0.0590 0.0381 C7 0.0443 0.0390 0.0218 C8 0.0403 0.0339 0.0307 C9 0.0585 0.0507 0.0333 C10 0.0670 0.0501 0.0340 C11 0.0451 0.0337 0.0255 C12 0.0483 0.0367 0.0221 C13 0.0406 0.0343 0.0224 C14 0.0400 0.0318 0.0189 C15 0.0431 0.0368 0.0245 C16 0.0432 0.0408 0.0359 C17 0.0729 0.0405 0.0349 C18 0.0988 0.0496 0.0259 C19 0.1011 0.0491 0.0292 C20 0.0628 0.0364 0.0320 C21 0.0455 0.0324 0.0279 C22 0.0529 0.0353 0.0249 C23 0.0506 0.0465 0.0346 C24 0.0698 0.0659 0.0383 C25 0.1397 0.0676 0.0274 C26 0.0997 0.0582 0.0309 C27 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.017 0.026 0.035 0.046 0.058 0.076 0.103 0.158 1.000 Number in group 546. 487. 493. 455. 516. 479. 486. 496. 483. 496. GooF 1.288 1.227 1.257 1.196 1.070 1.039 0.959 1.000 0.998 1.019 K 38.865 7.403 3.776 2.419 1.470 1.224 1.066 0.978 0.988 0.979 Resolution(A) 0.79 0.83 0.86 0.90 0.95 1.00 1.08 1.19 1.36 1.71 inf Number in group 501. 504. 479. 491. 503. 492. 486. 495. 491. 495. GooF 1.041 1.055 1.103 1.193 1.157 1.133 1.045 1.130 1.085 1.177 K 1.524 1.641 1.569 1.463 1.234 1.021 0.983 1.020 1.058 0.976 R1 0.497 0.459 0.404 0.349 0.277 0.167 0.117 0.107 0.083 0.046 Recommended weighting scheme: WGHT 0.0452 2.6934 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) 1 13 1 88.34 1.46 4.12 0.008 1.32 11 3 2 94.88 2.29 3.45 0.011 0.98 6 8 0 59.91 0.86 3.28 0.006 1.45 -7 5 1 75.95 14.20 3.26 0.026 1.54 -10 1 5 976.79 1386.10 3.24 0.258 1.17 -2 0 14 99.12 6.22 3.22 0.017 0.83 0 19 7 -23.19 57.22 3.18 0.053 0.80 -3 17 6 154.28 24.89 3.15 0.035 0.91 -11 10 5 183.09 40.61 3.14 0.044 0.91 -10 7 3 71.63 4.52 3.07 0.015 1.09 -11 5 3 88.11 2.06 3.05 0.010 1.05 -8 11 4 259.86 139.72 3.03 0.082 1.08 -6 7 12 95.00 8.18 3.03 0.020 0.89 -12 9 5 120.84 17.64 2.98 0.029 0.88 -3 13 4 281.91 413.66 2.94 0.141 1.20 2 1 0 123.32 66.51 2.88 0.057 5.52 -12 10 4 146.62 21.69 2.87 0.032 0.87 -9 2 1 61.01 10.56 2.86 0.023 1.31 -4 14 9 104.13 0.73 2.86 0.006 0.90 -2 1 9 34.72 0.05 2.84 0.002 1.30 2 18 1 100.65 0.06 2.82 0.002 0.95 10 8 1 114.30 18.26 2.81 0.030 1.00 -7 7 11 479.64 312.99 2.79 0.123 0.93 -4 7 9 44.48 0.22 2.76 0.003 1.14 0 16 7 100.15 4.09 2.76 0.014 0.91 -10 5 5 65.41 0.53 2.74 0.005 1.11 -3 12 5 49.11 1.97 2.74 0.010 1.22 -1 11 5 42.11 0.42 2.73 0.005 1.32 -5 14 2 74.30 0.31 2.73 0.004 1.11 1 6 2 -13.08 17.25 2.72 0.029 2.47 2 7 0 1697.82 1404.86 2.72 0.260 2.29 2 16 4 94.55 11.06 2.70 0.023 0.99 6 4 7 63.60 133.04 2.68 0.080 1.07 2 2 11 78.25 13.17 2.66 0.025 0.97 6 13 8 140.06 13.23 2.66 0.025 0.81 -13 9 2 102.24 0.00 2.66 0.000 0.83 -7 10 2 46.54 1.25 2.66 0.008 1.23 -11 11 4 126.56 12.38 2.66 0.024 0.90 -3 13 8 80.24 14.66 2.61 0.027 0.99 3 7 2 2020.64 1689.42 2.61 0.285 1.88 13 2 1 81.46 0.06 2.61 0.002 0.87 -5 4 6 35.21 2.37 2.61 0.011 1.59 8 10 7 103.15 0.43 2.60 0.005 0.84 -9 8 9 89.40 5.44 2.58 0.016 0.95 -9 14 1 139.52 14.08 2.58 0.026 0.91 9 6 3 73.07 9.70 2.57 0.022 1.06 6 3 0 257.14 175.93 2.56 0.092 1.84 -1 2 1 74.45 37.20 2.56 0.042 6.42 3 11 11 134.70 14.14 2.56 0.026 0.81 6 4 5 456.22 610.03 2.56 0.171 1.26 Bond lengths and angles N1 - Distance Angles C15 1.2950 (0.0046) C14 1.4494 (0.0045) 104.41 (0.30) N1 - C15 N2 - Distance Angles C15 1.3640 (0.0046) C16 1.4119 (0.0048) 124.83 (0.32) H2 0.8800 117.59 117.59 N2 - C15 C16 N3 - Distance Angles C15 1.3927 (0.0046) C22 1.4509 (0.0049) 119.05 (0.31) C1 1.5030 (0.0048) 103.77 (0.30) 121.99 (0.28) N3 - C15 C22 O1 - Distance Angles C5 1.2261 (0.0046) O1 - O2 - Distance Angles C13 1.2153 (0.0044) O2 - O3 - Distance Angles C13 1.3436 (0.0044) C14 1.5002 (0.0040) 115.80 (0.28) O3 - C13 C1 - Distance Angles N3 1.5030 (0.0048) C14 1.5298 (0.0052) 100.41 (0.28) C2 1.5302 (0.0049) 112.93 (0.33) 115.46 (0.29) C3 1.5418 (0.0050) 107.19 (0.28) 107.84 (0.31) 112.11 (0.32) C1 - N3 C14 C2 C2 - Distance Angles C1 1.5302 (0.0049) H2A 0.9800 109.47 H2B 0.9800 109.47 109.47 H2C 0.9800 109.47 109.47 109.47 C2 - C1 H2A H2B C3 - Distance Angles C5 1.5151 (0.0058) C4 1.5239 (0.0054) 110.95 (0.34) C1 1.5418 (0.0050) 110.46 (0.31) 114.47 (0.35) H3 1.0000 106.84 106.84 106.84 C3 - C5 C4 C1 C4 - Distance Angles C3 1.5239 (0.0054) H4A 0.9800 109.47 H4B 0.9800 109.47 109.47 H4C 0.9800 109.47 109.47 109.47 C4 - C3 H4A H4B C5 - Distance Angles O1 1.2261 (0.0046) C6 1.4837 (0.0059) 119.90 (0.42) C3 1.5151 (0.0058) 121.05 (0.41) 119.04 (0.35) C5 - O1 C6 C6 - Distance Angles C8 1.3514 (0.0053) C5 1.4837 (0.0059) 120.11 (0.38) C7 1.5133 (0.0057) 126.86 (0.40) 113.03 (0.36) C6 - C8 C5 C7 - Distance Angles C6 1.5133 (0.0057) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - C6 H7A H7B C8 - Distance Angles C6 1.3514 (0.0053) C14 1.5121 (0.0055) 120.55 (0.36) C9 1.5346 (0.0054) 125.42 (0.37) 113.96 (0.33) C8 - C6 C14 C9 - Distance Angles C8 1.5346 (0.0054) C10 1.5429 (0.0052) 110.94 (0.32) C12 1.5437 (0.0053) 109.93 (0.32) 106.97 (0.31) C11 1.5458 (0.0054) 112.12 (0.31) 110.82 (0.34) 105.82 (0.31) C9 - C8 C10 C12 C10 - Distance Angles C9 1.5429 (0.0052) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - C9 H10A H10B C11 - Distance Angles C9 1.5458 (0.0054) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - C9 H11A H11B C12 - Distance Angles C13 1.4895 (0.0052) C9 1.5437 (0.0054) 111.69 (0.32) H12A 0.9900 109.28 109.28 H12B 0.9900 109.28 109.28 107.95 C12 - C13 C9 H12A C13 - Distance Angles O2 1.2153 (0.0043) O3 1.3436 (0.0044) 118.55 (0.35) C12 1.4895 (0.0052) 125.75 (0.36) 115.70 (0.33) C13 - O2 O3 C14 - Distance Angles N1 1.4494 (0.0045) O3 1.5002 (0.0040) 106.99 (0.28) C8 1.5121 (0.0055) 113.88 (0.31) 106.77 (0.28) C1 1.5298 (0.0052) 105.93 (0.29) 104.52 (0.28) 117.90 (0.32) C14 - N1 O3 C8 C15 - Distance Angles N1 1.2950 (0.0046) N2 1.3640 (0.0046) 124.78 (0.34) N3 1.3927 (0.0046) 117.82 (0.34) 117.33 (0.33) C15 - N1 N2 C16 - Distance Angles C21 1.3788 (0.0052) C17 1.3827 (0.0053) 119.51 (0.38) N2 1.4119 (0.0048) 118.20 (0.36) 122.17 (0.33) C16 - C21 C17 C17 - Distance Angles C16 1.3827 (0.0053) C18 1.3931 (0.0056) 120.43 (0.39) H17 0.9500 119.79 119.79 C17 - C16 C18 C18 - Distance Angles C19 1.3788 (0.0062) C17 1.3931 (0.0057) 119.46 (0.43) H18 0.9500 120.27 120.27 C18 - C19 C17 C19 - Distance Angles C20 1.3723 (0.0067) C18 1.3788 (0.0062) 120.35 (0.43) H19 0.9500 119.83 119.83 C19 - C20 C18 C20 - Distance Angles C19 1.3723 (0.0067) C21 1.3909 (0.0060) 120.14 (0.42) H20 0.9500 119.93 119.93 C20 - C19 C21 C21 - Distance Angles C16 1.3788 (0.0052) C20 1.3909 (0.0060) 120.10 (0.42) H21 0.9500 119.95 119.95 C21 - C16 C20 C22 - Distance Angles C27 1.3855 (0.0057) C23 1.3875 (0.0053) 119.60 (0.39) N3 1.4509 (0.0049) 119.53 (0.37) 120.87 (0.34) C22 - C27 C23 C23 - Distance Angles C24 1.3777 (0.0055) C22 1.3875 (0.0053) 120.76 (0.39) H23 0.9500 119.62 119.62 C23 - C24 C22 C24 - Distance Angles C25 1.3726 (0.0061) C23 1.3777 (0.0055) 119.72 (0.43) H24 0.9500 120.14 120.14 C24 - C25 C23 C25 - Distance Angles C24 1.3726 (0.0060) C26 1.3782 (0.0066) 120.32 (0.46) H25 0.9500 119.84 119.84 C25 - C24 C26 C26 - Distance Angles C25 1.3782 (0.0066) C27 1.3946 (0.0066) 120.38 (0.46) H26 0.9500 119.81 119.81 C26 - C25 C27 C27 - Distance Angles C22 1.3855 (0.0057) C26 1.3946 (0.0066) 119.21 (0.44) H27 0.9500 120.40 120.40 C27 - C22 C26 FMAP and GRID set by program FMAP 2 2 23 GRID -1.250 -2 -2 1.250 2 2 R1 = 0.1904 for 4937 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.20 at 0.0819 0.2142 0.3996 [ 1.23 A from H23 ] Deepest hole -0.28 at 0.2528 0.1711 0.2354 [ 0.95 A from C1 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 3536 / 24069 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0819 0.2858 -0.1004 1.00000 0.05 0.20 1.23 H23 1.92 O3 2.14 C23 2.22 C13 Q2 1 0.0512 0.2272 -0.5210 1.00000 0.05 0.20 1.31 H2 1.70 H23 1.75 N2 1.79 H21 Q3 1 0.1798 0.4761 0.0421 1.00000 0.05 0.20 1.25 H10A 1.75 C13 1.79 C10 1.96 H10B Q4 1 0.1004 0.3347 -0.2326 1.00000 0.05 0.19 1.01 N1 1.21 C15 1.71 C14 1.95 O3 Q5 1 0.3991 0.6133 -0.1048 1.00000 0.05 0.19 0.62 H7C 1.47 C7 1.71 H10C 1.79 H7B Q6 1 0.1056 0.1853 0.0016 1.00000 0.05 0.18 1.47 H23 1.52 H24 1.74 C23 1.75 C24 Q7 1 -0.2447 0.4254 -0.3823 1.00000 0.05 0.18 1.28 H18 1.48 C18 1.63 H25 2.04 H26 Q8 1 0.0776 0.4089 -0.2740 1.00000 0.05 0.18 0.92 N1 1.50 H12B 1.86 C14 2.10 C15 Q9 1 0.2737 0.2884 -0.2193 1.00000 0.05 0.17 0.74 C1 0.77 N3 1.78 C15 1.84 C14 Q10 1 0.3460 0.3118 -0.1404 1.00000 0.05 0.17 0.68 C1 0.85 C2 1.47 H2B 1.49 H2A Q11 1 -0.0628 0.1587 -0.4342 1.00000 0.05 0.17 1.74 H2 1.85 H11B 1.88 O2 2.10 H10B Q12 1 0.2822 0.2974 0.0389 1.00000 0.05 0.17 1.20 H2A 1.95 O3 2.11 C2 2.23 H4B Q13 1 -0.1997 0.3349 -0.2252 1.00000 0.05 0.17 1.47 H18 1.64 H17 1.80 C18 1.88 C17 Q14 1 0.3113 0.5992 -0.2164 1.00000 0.05 0.17 1.01 H7C 1.15 H11A 1.52 C7 1.73 H7A Q15 1 0.3218 -0.0108 -0.0208 1.00000 0.05 0.16 1.36 H25 1.72 C25 1.89 H26 1.99 C26 Q16 1 0.1616 0.2723 -0.2442 1.00000 0.05 0.16 0.88 C15 0.90 N3 1.70 C22 1.82 N1 Q17 1 0.0088 0.3162 -0.2241 1.00000 0.05 0.16 1.13 H17 1.85 C17 1.99 C15 2.01 N1 Q18 1 0.2746 0.0402 0.0619 1.00000 0.05 0.16 1.57 H25 1.77 C25 2.09 H3 2.26 C24 Q19 1 0.2262 0.1841 -0.1118 1.00000 0.05 0.16 0.91 C23 1.02 C22 1.59 H23 1.81 C24 Q20 1 -0.0214 0.3660 -0.2747 1.00000 0.05 0.16 0.91 H17 1.51 C17 1.83 N1 2.03 H12B Shortest distances between peaks (including symmetry equivalents) 17 20 1.06 1 2 1.11 9 10 1.17 4 17 1.18 9 16 1.34 4 16 1.34 4 8 1.39 8 20 1.41 5 14 1.47 4 20 1.52 15 18 1.54 1 17 1.58 2 6 1.66 7 15 1.69 1 4 1.84 8 17 1.98 16 17 2.07 1 6 2.10 1 16 2.17 16 19 2.18 4 9 2.21 6 19 2.22 2 11 2.26 10 16 2.34 9 19 2.37 7 13 2.38 2 17 2.43 13 20 2.43 10 12 2.44 1 19 2.52 1 20 2.52 13 17 2.53 1 12 2.54 8 16 2.58 12 19 2.62 16 20 2.70 2 12 2.72 10 19 2.73 6 12 2.84 7 20 2.85 7 18 2.87 4 10 2.90 2 4 2.92 1 8 2.96 6 16 2.98 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: 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. 0.22: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.34: Structure factors and derivatives 2.79: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.19: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + b finished at 12:27:56 Total CPU time: 4.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++