+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0058p21c started at 16:24:50 on 07-Sep-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0058p21c in P2(1)/c CELL 0.71073 7.5550 10.9180 8.1170 90.000 111.565 90.000 ZERR 2.00 0.0003 0.0004 0.0002 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 16 44 4 12 V = 622.67 F(000) = 264.0 Mu = 0.11 mm-1 Cell Wt = 484.55 Rho = 1.292 MERG 2 OMIT -3.00 55.00 OMIT 1 2 1 OMIT -2 2 3 EXTI 0.05378 SHEL 7 0.77 DFIX 0.84 0.02 O1W H1W O1W H2W DANG 1.35 0.02 H1W H2W HTAB N22 O1A HTAB O1W O1A EQIV_$1 -x+1, -y, -z+1 HTAB N22 O1B_$1 EQIV_$2 x, -y-1/2, z-1/2 HTAB O1W O1B_$2 FMAP 2 PLAN 10 SIZE 0.18 0.20 0.40 ACTA MPLA C1 O1A O1B MPLA C1_$1 O1A_$1 O1B_$1 BOND $H WGHT 0.04040 0.22060 L.S. 4 TEMP -153.00 FVAR 1.86278 MOLE 1 C1 1 0.585292 -0.045002 0.538072 11.00000 0.01981 0.02010 = 0.01667 -0.00152 0.00866 -0.00156 O1A 4 0.697567 -0.050582 0.455578 11.00000 0.02414 0.02610 = 0.02411 0.00443 0.01416 0.00600 O1B 4 0.597034 -0.103943 0.672129 11.00000 0.03008 0.04099 = 0.02719 0.01762 0.01622 0.01455 MOLE 2 C21 1 0.876515 0.023387 0.183104 11.00000 0.01716 0.02680 = 0.02850 -0.00072 0.00904 0.00030 AFIX 137 H21A 2 0.852512 -0.064434 0.161059 11.00000 -1.50000 H21B 2 0.976324 0.035465 0.300006 11.00000 -1.50000 H21C 2 0.917755 0.058463 0.091968 11.00000 -1.50000 AFIX 0 C23 1 0.732072 0.219296 0.212313 11.00000 0.02604 0.02220 = 0.02126 -0.00441 0.00915 -0.00443 AFIX 137 H23A 2 0.765260 0.256530 0.117634 11.00000 -1.50000 H23B 2 0.836836 0.231336 0.326197 11.00000 -1.50000 H23C 2 0.616476 0.257893 0.216003 11.00000 -1.50000 AFIX 0 C24 1 0.535505 0.065501 0.007386 11.00000 0.02005 0.02126 = 0.01488 0.00082 0.00467 -0.00212 AFIX 23 H24A 2 0.576280 0.083763 -0.092799 11.00000 -1.20000 H24B 2 0.430654 0.122193 0.000213 11.00000 -1.20000 AFIX 0 N22 3 0.698007 0.085407 0.177430 11.00000 0.01726 0.02025 = 0.01505 -0.00097 0.00667 -0.00260 AFIX 13 H22 2 0.664613 0.052659 0.267748 11.00000 0.03340 AFIX 0 MOLE 3 O1W 4 0.881467 -0.266420 0.433675 11.00000 0.02539 0.02759 = 0.03335 -0.00984 0.00057 0.00499 H1W 2 0.802435 -0.300567 0.342533 11.00000 0.04643 H2W 2 0.826714 -0.202142 0.450791 11.00000 0.05047 HKLF 4 Covalent radii and connectivity table for 06skc0058p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C1_$1 O1A - C1 O1B - C1 C21 - N22 C23 - N22 C24 - N22 C24_$3 N22 - C24 C23 C21 O1W - no bonds found Operators for generating equivalent atoms: $1 -x+1, -y, -z+1 $2 x, -y-1/2, z-1/2 $3 -x+1, -y, -z 6196 Reflections read, of which 298 rejected -8 =< h =< 8, -12 =< k =< 12, -8 =< l =< 8, Max. 2-theta = 46.64 0 Systematic absence violations 0 Inconsistent equivalents 635 Unique reflections, of which 0 suppressed R(int) = 0.0337 R(sigma) = 0.0220 Friedel opposites merged Maximum memory for data reduction = 1355 / 6831 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 = 1596 / 113690 wR2 = 0.0821 before cycle 1 for 635 data and 85 / 85 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.010 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.081; Restrained GooF = 1.078 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0404 * P )^2 + 0.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.86277 0.00948 -0.001 OSF 2 0.05378 0.01198 0.000 EXTI Mean shift/esd = 0.002 Maximum = -0.005 for U23 O1W Max. shift = 0.000 A for H1W Max. dU = 0.000 for O1W Least-squares cycle 2 Maximum vector length = 511 Memory required = 1596 / 113690 wR2 = 0.0821 before cycle 2 for 635 data and 85 / 85 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.010 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.081; Restrained GooF = 1.078 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0404 * P )^2 + 0.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.86278 0.00948 0.001 OSF 2 0.05378 0.01198 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.002 for U23 O1W Max. shift = 0.000 A for H23B Max. dU = 0.000 for H2W Least-squares cycle 3 Maximum vector length = 511 Memory required = 1596 / 113690 wR2 = 0.0821 before cycle 3 for 635 data and 85 / 85 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.010 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.081; Restrained GooF = 1.078 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0404 * P )^2 + 0.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.86278 0.00948 0.000 OSF 2 0.05378 0.01198 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x N22 Max. shift = 0.000 A for H2W Max. dU = 0.000 for H2W Least-squares cycle 4 Maximum vector length = 511 Memory required = 1596 / 113690 wR2 = 0.0821 before cycle 4 for 635 data and 85 / 85 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.010 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.081; Restrained GooF = 1.078 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0404 * P )^2 + 0.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.86278 0.00948 0.000 OSF 2 0.05378 0.01198 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x C21 Max. shift = 0.000 A for H1W Max. dU = 0.000 for H2W Largest correlation matrix elements 0.693 U13 O1B / U11 O1B 0.602 U13 C1 / U11 C1 0.567 U13 C24 / U33 C24 0.678 U13 N22 / U11 N22 0.601 U13 N22 / U33 N22 0.560 U12 O1B / U23 O1B 0.666 U13 O1A / U11 O1A 0.597 U13 C21 / U33 C21 0.556 U12 N22 / U23 N22 0.652 U13 C24 / U11 C24 0.597 U13 C23 / U33 C23 0.553 U12 O1A / U23 O1A 0.652 U13 C21 / U11 C21 0.594 U13 O1W / U11 O1W 0.552 z O1B / x O1B 0.650 U13 C23 / U11 C23 0.590 U13 O1W / U33 O1W 0.548 U12 C24 / U23 C24 0.631 EXTI / OSF 0.589 U13 O1B / U33 O1B 0.547 U12 C21 / U23 C21 0.622 U13 O1A / U33 O1A 0.585 U12 C1 / U23 C1 0.536 z C23 / x C23 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H21A 0.8525 -0.0644 0.1611 137 0.980 0.000 C21 N22 H21A H21B 0.9763 0.0355 0.3000 137 0.980 0.000 C21 N22 H21A H21C 0.9178 0.0585 0.0920 137 0.980 0.000 C21 N22 H21A H23A 0.7653 0.2565 0.1176 137 0.980 0.000 C23 N22 H23A H23B 0.8368 0.2313 0.3262 137 0.980 0.000 C23 N22 H23A H23C 0.6165 0.2579 0.2160 137 0.980 0.000 C23 N22 H23A H24A 0.5763 0.0838 -0.0928 23 0.990 0.000 C24 N22 C24_$3 H24B 0.4307 0.1222 0.0002 23 0.990 0.000 C24 N22 C24_$3 H22 0.6646 0.0527 0.2677 13 0.930 0.000 N22 C24 C23 C21 06skc0058p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.58529 -0.04500 0.53807 1.00000 0.01981 0.02010 0.01667 -0.00152 0.00866 -0.00156 0.01831 0.00377 0.00027 0.00015 0.00023 0.00000 0.00101 0.00085 0.00095 0.00076 0.00088 0.00076 0.00048 O1A 0.69757 -0.05058 0.45558 1.00000 0.02414 0.02610 0.02411 0.00443 0.01416 0.00600 0.02328 0.00276 0.00019 0.00011 0.00017 0.00000 0.00085 0.00070 0.00077 0.00052 0.00074 0.00054 0.00044 O1B 0.59703 -0.10394 0.67213 1.00000 0.03008 0.04099 0.02719 0.01762 0.01622 0.01455 0.03114 0.00306 0.00020 0.00012 0.00017 0.00000 0.00086 0.00083 0.00079 0.00064 0.00069 0.00065 0.00045 C21 0.87651 0.02339 0.18310 1.00000 0.01716 0.02680 0.02850 -0.00072 0.00904 0.00030 0.02397 0.00397 0.00026 0.00017 0.00025 0.00000 0.00109 0.00101 0.00106 0.00078 0.00097 0.00078 0.00051 H21A 0.85251 -0.06443 0.16106 1.00000 0.03595 0.00000 0.00000 H21B 0.97632 0.03547 0.30001 1.00000 0.03595 0.00000 0.00000 H21C 0.91776 0.05846 0.09197 1.00000 0.03595 0.00000 0.00000 C23 0.73207 0.21930 0.21231 1.00000 0.02604 0.02220 0.02126 -0.00441 0.00915 -0.00443 0.02304 0.00393 0.00028 0.00015 0.00025 0.00000 0.00107 0.00093 0.00092 0.00072 0.00091 0.00078 0.00050 H23A 0.76526 0.25653 0.11763 1.00000 0.03456 0.00000 0.00000 H23B 0.83684 0.23134 0.32620 1.00000 0.03456 0.00000 0.00000 H23C 0.61648 0.25789 0.21600 1.00000 0.03456 0.00000 0.00000 C24 0.53551 0.06550 0.00739 1.00000 0.02005 0.02126 0.01488 0.00082 0.00467 -0.00212 0.01923 0.00369 0.00027 0.00015 0.00023 0.00000 0.00107 0.00091 0.00092 0.00071 0.00091 0.00074 0.00047 H24A 0.57628 0.08376 -0.09280 1.00000 0.02307 0.00000 0.00000 H24B 0.43065 0.12219 0.00021 1.00000 0.02307 0.00000 0.00000 N22 0.69801 0.08541 0.17743 1.00000 0.01726 0.02025 0.01505 -0.00097 0.00667 -0.00260 0.01732 0.00294 0.00021 0.00012 0.00018 0.00000 0.00090 0.00077 0.00079 0.00059 0.00074 0.00064 0.00044 H22 0.66461 0.05266 0.26775 1.00000 0.03340 0.00000 0.00551 O1W 0.88147 -0.26642 0.43368 1.00000 0.02539 0.02759 0.03335 -0.00984 0.00057 0.00499 0.03167 0.00291 0.00019 0.00013 0.00019 0.00000 0.00086 0.00079 0.00089 0.00067 0.00081 0.00066 0.00045 H1W 0.80243 -0.30057 0.34253 1.00000 0.04643 0.03533 0.00328 0.00191 0.00259 0.00000 0.00751 H2W 0.82671 -0.20214 0.45079 1.00000 0.05047 0.04935 0.00355 0.00178 0.00319 0.00000 0.00713 Final Structure Factor Calculation for 06skc0058p21c in P2(1)/c Total number of l.s. parameters = 85 Maximum vector length = 511 Memory required = 1511 / 22995 wR2 = 0.0821 before cycle 5 for 635 data and 0 / 85 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.010 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.081; Restrained GooF = 1.078 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0404 * P )^2 + 0.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0323 for 573 Fo > 4sig(Fo) and 0.0373 for all 635 data wR2 = 0.0821, GooF = S = 1.081, Restrained GooF = 1.078 for all data Occupancy sum of asymmetric unit = 8.00 for non-hydrogen and 11.00 for hydrogen atoms Principal mean square atomic displacements U 0.0220 0.0184 0.0145 C1 0.0335 0.0209 0.0155 O1A 0.0568 0.0215 0.0151 O1B 0.0290 0.0265 0.0164 C21 0.0292 0.0228 0.0172 C23 0.0242 0.0188 0.0147 C24 0.0218 0.0158 0.0144 N22 0.0534 0.0215 0.0202 O1W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.025 0.045 0.064 0.087 0.114 0.138 0.170 0.211 0.287 1.000 Number in group 67. 65. 61. 65. 61. 65. 61. 63. 63. 64. GooF 0.984 1.197 1.156 1.001 1.013 0.999 0.971 0.961 1.410 1.035 K 1.415 0.955 0.899 0.996 0.987 1.006 0.994 1.020 1.001 1.012 Resolution(A) 0.90 0.93 0.96 0.99 1.04 1.09 1.16 1.26 1.40 1.77 inf Number in group 67. 61. 65. 62. 65. 63. 63. 64. 61. 64. GooF 0.859 1.126 1.009 0.932 1.128 1.311 0.824 0.822 1.075 1.517 K 0.999 1.031 1.008 1.026 1.013 0.989 1.011 1.023 1.016 1.000 R1 0.071 0.061 0.048 0.043 0.044 0.044 0.026 0.026 0.026 0.026 Recommended weighting scheme: WGHT 0.0404 0.2206 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 1 7 117.23 235.05 6.76 0.271 1.12 -1 4 3 7.99 1.91 3.95 0.024 1.92 2 2 0 181.72 223.59 3.79 0.265 2.95 2 1 0 221.74 259.67 2.98 0.285 3.34 2 0 4 8.28 4.01 2.95 0.035 1.45 2 10 0 4.75 8.79 2.65 0.052 1.04 1 1 0 6.90 2.62 2.58 0.029 5.91 0 0 8 341.64 296.96 2.56 0.305 0.94 4 7 2 17.12 23.97 2.49 0.087 1.04 -4 2 1 41.45 51.06 2.45 0.126 1.77 -2 3 3 2.51 4.95 2.44 0.039 2.08 -3 4 6 23.82 18.16 2.42 0.075 1.20 5 7 0 18.31 24.41 2.40 0.087 1.04 0 1 1 91.74 78.24 2.40 0.156 6.21 -4 4 2 58.92 70.10 2.33 0.148 1.55 2 1 7 58.61 48.78 2.27 0.124 0.94 -7 5 1 144.87 124.59 2.23 0.197 0.94 -6 4 3 223.82 198.24 2.21 0.249 1.14 2 10 1 1.38 3.54 2.16 0.033 1.02 -1 3 3 76.26 65.73 2.15 0.143 2.17 1 3 0 113.39 99.46 2.14 0.176 3.23 0 6 2 20.92 26.47 2.13 0.091 1.64 5 2 2 62.42 22.73 2.13 0.084 1.16 -6 2 4 5.89 9.04 2.10 0.053 1.19 1 11 0 5.60 8.61 2.10 0.052 0.98 3 7 3 174.94 148.43 2.08 0.216 1.07 0 2 4 133.84 118.53 2.07 0.193 1.78 2 1 6 201.87 179.76 2.04 0.237 1.06 0 8 5 -1.13 0.49 2.02 0.012 1.01 2 3 7 12.97 6.53 1.98 0.045 0.91 2 0 0 397.67 439.98 1.98 0.371 3.51 0 1 3 403.03 442.88 1.96 0.372 2.45 6 7 0 -1.06 0.39 1.93 0.011 0.94 -3 0 4 4.73 7.18 1.91 0.047 1.84 -3 1 2 49.81 42.73 1.89 0.116 2.37 0 6 0 2966.70 2738.05 1.87 0.926 1.82 2 11 0 111.89 98.36 1.87 0.175 0.96 1 5 0 38.22 44.84 1.85 0.118 2.09 6 1 3 0.93 3.75 1.84 0.034 0.93 -3 6 5 23.31 28.34 1.83 0.094 1.18 4 4 0 58.57 50.77 1.83 0.126 1.48 -4 8 2 1.24 3.22 1.81 0.032 1.10 7 0 0 628.99 561.73 1.78 0.419 1.00 0 1 2 853.64 924.41 1.78 0.538 3.57 3 10 0 1.89 3.82 1.77 0.035 0.99 5 8 0 9.66 13.07 1.75 0.064 0.98 1 12 0 5.30 8.23 1.74 0.051 0.90 0 3 2 315.47 343.71 1.73 0.328 2.62 2 11 1 6.42 2.41 1.73 0.027 0.94 1 2 7 29.52 35.14 1.73 0.105 0.99 Bond lengths and angles C1 - Distance Angles O1B 1.2390 (0.0021) O1A 1.2606 (0.0021) 126.62 (0.16) C1_$1 1.5566 (0.0036) 117.27 (0.17) 116.11 (0.17) C1 - O1B O1A O1A - Distance Angles C1 1.2606 (0.0021) O1A - O1B - Distance Angles C1 1.2390 (0.0021) O1B - C21 - Distance Angles N22 1.4946 (0.0022) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C21 - N22 H21A H21B C23 - Distance Angles N22 1.4932 (0.0021) H23A 0.9800 109.47 H23B 0.9800 109.47 109.47 H23C 0.9800 109.47 109.47 109.47 C23 - N22 H23A H23B C24 - Distance Angles N22 1.4879 (0.0024) C24_$3 1.5168 (0.0033) 111.00 (0.17) H24A 0.9900 109.44 109.44 H24B 0.9900 109.44 109.44 108.04 C24 - N22 C24_$3 H24A N22 - Distance Angles C24 1.4879 (0.0024) C23 1.4932 (0.0021) 110.17 (0.14) C21 1.4946 (0.0022) 112.95 (0.13) 110.30 (0.13) H22 0.9300 107.74 107.74 107.74 N22 - C24 C23 C21 O1W - Distance Angles H1W 0.8474 (0.0164) H2W 0.8516 (0.0167) 106.04 (2.01) O1W - H1W Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.93 1.84 2.7032(17) 153.7 N22-H22...O1A 0.852(17) 1.929(18) 2.7743(17) 172(2) O1W-H2W...O1A 0.93 2.27 2.9158(18) 125.7 N22-H22...O1B_$1 0.847(16) 1.957(18) 2.7883(19) 167(2) O1W-H1W...O1B_$2 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 2.7866 (0.0185) x + 7.9570 (0.0250) y + 3.2544 (0.0070) z = 3.0240 (0.0149) * 0.0000 (0.0000) C1 * 0.0000 (0.0000) O1A * 0.0000 (0.0000) O1B Rms deviation of fitted atoms = 0.0000 2.7867 (0.0185) x + 7.9570 (0.0250) y + 3.2544 (0.0071) z = 3.0170 (0.0065) Angle to previous plane (with approximate esd) = 0.00 ( 0.39 ) * 0.0000 (0.0000) C1_$1 * 0.0000 (0.0000) O1A_$1 * 0.0000 (0.0000) O1B_$1 Rms deviation of fitted atoms = 0.0000 FMAP and GRID set by program FMAP 2 3 12 GRID -2.778 -2 -2 2.778 2 2 R1 = 0.0373 for 635 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.10 at 0.8776 0.4262 0.0543 [ 1.76 A from H21B ] Deepest hole -0.11 at 0.6380 0.4686 0.0969 [ 0.97 A from C1 ] Mean = 0.00, Rms deviation from mean = 0.03 e/A^3, Highest memory used = 1596 / 12348 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.1224 -0.0738 0.4457 1.00000 0.05 0.10 1.76 H21B 1.88 O1A 2.18 H23A 2.30 H22 Q2 1 0.5182 -0.2320 0.6410 1.00000 0.05 0.10 1.50 O1B 1.82 H23C 2.08 H24B 2.12 H24A Q3 1 0.6562 -0.0261 0.6723 1.00000 0.05 0.10 0.96 O1B 1.04 C1 1.92 O1A 2.13 C1 Q4 1 0.3228 0.0357 -0.0816 1.00000 0.05 0.10 1.26 H24B 1.28 H21A 1.50 C24 1.51 N22 Q5 1 0.6471 0.0741 0.0893 1.00000 0.05 0.09 0.69 N22 0.87 C24 1.38 H24A 1.42 H22 Q6 1 0.5000 0.0000 0.5000 0.50000 0.05 0.09 0.78 C1 1.74 O1B 1.75 O1A 2.67 H22 Q7 1 0.5947 0.1588 -0.0610 1.00000 0.05 0.09 0.85 H24A 1.31 C24 1.55 H24B 1.88 H23A Q8 1 0.7956 0.0603 0.1705 1.00000 0.05 0.09 0.71 C21 0.81 N22 1.30 H21C 1.41 H21B Q9 1 0.7161 0.1511 0.2040 1.00000 0.05 0.08 0.75 N22 0.75 C23 1.31 H22 1.39 H23B Q10 1 0.4426 0.2188 -0.0520 1.00000 0.05 0.08 1.15 H24B 1.81 C24 1.88 H24A 2.13 H23C Shortest distances between peaks (including symmetry equivalents) 2 10 1.03 5 8 1.08 5 9 1.22 4 5 1.23 8 9 1.24 7 10 1.35 4 8 1.39 5 7 1.46 2 7 1.47 3 6 1.49 7 9 2.01 4 10 2.17 7 8 2.21 5 10 2.21 4 9 2.24 4 5 2.37 4 7 2.39 4 7 2.41 9 10 2.45 2 3 2.45 1 3 2.47 4 4 2.63 2 9 2.67 5 5 2.70 2 6 2.76 1 9 2.78 2 5 2.80 1 1 2.83 1 6 2.84 2 4 2.92 1 8 2.95 3 10 2.95 3 3 2.98 2 9 2.99 Time profile in seconds ----------------------- 0.06: 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 0.02: Analyse other restraints etc. 0.39: 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 0.08: Structure factors and derivatives 0.03: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.03: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.00: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0058p21c finished at 16:24:51 Total CPU time: 0.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++