+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04mbh0603 started at 11:56:28 on 13-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04mbh0603 in C2/c CELL 0.71073 20.1042 7.6296 15.3016 90.000 129.990 90.000 ZERR 8.00 0.0040 0.0015 0.0031 0.000 0.030 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O UNIT 40 104 8 56 V = 1798.22 F(000) = 848.0 Mu = 0.14 mm-1 Cell Wt = 1593.31 Rho = 1.471 MERG 2 OMIT -3.00 55.00 OMIT 4 0 0 EXTI 0.00588 SHEL 7 0.77 DFIX 0.84 0.02 O1W H1W O1W H2W DANG 1.35 0.02 H1W H2W HTAB N22 O1A HTAB N22 O1W HTAB O1W O4A EQIV_$1 -x, -y+1, -z HTAB O2 O1W_$1 EQIV_$2 -x+1/2, -y+3/2, -z HTAB O3 O1B_$2 EQIV_$3 x, y-1, z HTAB O4B O1A_$3 EQIV_$4 -x+1/2, y+1/2, -z+1/2 HTAB N22 O3_$4 HTAB N22 O4A_$4 EQIV_$5 x, -y+1, z+1/2 HTAB O1W O1B_$5 FMAP 2 PLAN 10 SIZE 0.05 0.10 0.10 ACTA BOND $H WGHT 0.03780 2.32750 L.S. 4 TEMP -153.00 FVAR 0.46553 MOLE 1 C1 1 0.117464 0.744878 -0.085045 11.00000 0.01581 0.01798 = 0.01375 0.00073 0.00868 -0.00056 C2 1 0.097708 0.557333 -0.071029 11.00000 0.01862 0.01539 = 0.01679 -0.00017 0.01295 -0.00136 AFIX 13 H2 2 0.061286 0.497097 -0.146779 11.00000 -1.20000 AFIX 0 C3 1 0.184587 0.459402 0.011677 11.00000 0.01795 0.01561 = 0.01880 0.00067 0.01312 -0.00078 AFIX 13 H3 2 0.215648 0.459258 -0.019484 11.00000 -1.20000 AFIX 0 C4 1 0.165321 0.271096 0.023004 11.00000 0.01642 0.01719 = 0.01980 0.00152 0.01203 0.00247 O1A 4 0.107126 0.868695 -0.040178 11.00000 0.03689 0.01506 = 0.02952 -0.00135 0.02581 -0.00015 O1B 4 0.144711 0.761434 -0.138928 11.00000 0.03161 0.02047 = 0.02394 -0.00338 0.02145 -0.00680 O2 4 0.055338 0.549162 -0.025452 11.00000 0.01616 0.02555 = 0.02171 0.00353 0.01374 0.00070 AFIX 147 H2O 2 0.001426 0.555672 -0.078581 11.00000 -1.50000 AFIX 0 O3 4 0.237666 0.538985 0.120863 11.00000 0.01772 0.02150 = 0.01857 -0.00191 0.01062 -0.00506 AFIX 147 H3O 2 0.278161 0.594068 0.130609 11.00000 -1.50000 AFIX 0 O4A 4 0.177732 0.216574 0.107475 11.00000 0.02849 0.02038 = 0.02281 0.00205 0.01704 -0.00102 O4B 4 0.133577 0.178135 -0.068427 11.00000 0.03082 0.01416 = 0.02487 -0.00200 0.01955 -0.00204 AFIX 147 H4 2 0.125671 0.074496 -0.058373 11.00000 -1.50000 AFIX 0 MOLE 2 C21 1 0.066920 0.884838 0.148547 11.00000 0.02538 0.04515 = 0.02817 -0.00254 0.01763 0.00378 AFIX 137 H21A 2 0.063966 1.011402 0.135537 11.00000 -1.50000 H21B 2 0.069197 0.862671 0.213513 11.00000 -1.50000 H21C 2 0.015378 0.828209 0.080275 11.00000 -1.50000 AFIX 0 N22 3 0.145620 0.812849 0.173139 11.00000 0.02124 0.02421 = 0.02050 -0.00076 0.01258 0.00005 AFIX 137 H22A 2 0.193270 0.869847 0.234069 11.00000 -1.50000 H22B 2 0.142057 0.827804 0.111238 11.00000 -1.50000 H22C 2 0.150021 0.696539 0.189260 11.00000 -1.50000 AFIX 0 MOLE 3 O1W 4 0.122143 0.448770 0.202206 11.00000 0.02688 0.02947 = 0.02263 0.00479 0.01822 0.00267 H1W 2 0.132746 0.385649 0.254920 11.00000 0.03343 H2W 2 0.137649 0.390377 0.170811 11.00000 0.05599 HKLF 4 Covalent radii and connectivity table for 04mbh0603 in C2/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - O2 C1 C3 C3 - O3 C4 C2 C4 - O4A O4B C3 O1A - C1 O1B - C1 O2 - C2 O3 - C3 O4A - C4 O4B - C4 C21 - N22 N22 - C21 O1W - no bonds found Operators for generating equivalent atoms: $1 -x, -y+1, -z $2 -x+1/2, -y+3/2, -z $3 x, y-1, z $4 -x+1/2, y+1/2, -z+1/2 $5 x, -y+1, z+1/2 10029 Reflections read, of which 410 rejected -26 =< h =< 26, -8 =< k =< 9, -19 =< l =< 19, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 2044 Unique reflections, of which 0 suppressed R(int) = 0.0586 R(sigma) = 0.0493 Friedel opposites merged Maximum memory for data reduction = 1758 / 25391 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 = 2121 / 166941 wR2 = 0.1124 before cycle 1 for 2044 data and 132 / 132 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 0.006 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.060; Restrained GooF = 1.059 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0378 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.46553 0.00144 -0.002 OSF 2 0.00588 0.00096 -0.003 EXTI Mean shift/esd = 0.003 Maximum = -0.008 for U22 O4B Max. shift = 0.000 A for H2W Max. dU = 0.000 for H1W Least-squares cycle 2 Maximum vector length = 511 Memory required = 2121 / 166941 wR2 = 0.1124 before cycle 2 for 2044 data and 132 / 132 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 0.006 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.060; Restrained GooF = 1.059 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0378 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.46553 0.00144 -0.002 OSF 2 0.00588 0.00096 -0.002 EXTI Mean shift/esd = 0.001 Maximum = -0.003 for U22 O4B Max. shift = 0.000 A for H2W Max. dU = 0.000 for H1W Least-squares cycle 3 Maximum vector length = 511 Memory required = 2121 / 166941 wR2 = 0.1124 before cycle 3 for 2044 data and 132 / 132 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 0.006 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.060; Restrained GooF = 1.059 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0378 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.46553 0.00144 0.000 OSF 2 0.00588 0.00096 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y H1W Max. shift = 0.000 A for H1W Max. dU = 0.000 for H1W Least-squares cycle 4 Maximum vector length = 511 Memory required = 2121 / 166941 wR2 = 0.1124 before cycle 4 for 2044 data and 132 / 132 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 0.006 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.060; Restrained GooF = 1.059 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0378 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.46553 0.00144 0.000 OSF 2 0.00588 0.00096 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x O4A Max. shift = 0.000 A for H1W Max. dU = 0.000 for H1W Largest correlation matrix elements 0.820 z H2W / x H2W 0.759 U13 C2 / U33 C2 0.744 U13 O3 / U33 O3 0.787 U13 O1A / U33 O1A 0.759 U13 O4B / U33 O4B 0.739 U13 C4 / U33 C4 0.779 U13 O1B / U33 O1B 0.755 U13 O2 / U11 O2 0.738 U13 O4A / U33 O4A 0.773 U13 O1A / U11 O1A 0.755 U13 C2 / U11 C2 0.735 U13 N22 / U33 N22 0.768 U13 O2 / U33 O2 0.749 U13 C3 / U11 C3 0.731 U13 C21 / U11 C21 0.766 U13 C3 / U33 C3 0.749 U13 O4B / U11 O4B 0.731 U13 O4A / U11 O4A 0.761 U13 O1W / U33 O1W 0.748 U13 C21 / U33 C21 0.725 U13 C1 / U33 C1 0.760 U13 O1B / U11 O1B 0.746 U13 O1W / U11 O1W 0.725 z H1W / x H1W Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.0613 0.4971 -0.1468 13 1.000 0.000 C2 O2 C1 C3 H3 0.2156 0.4593 -0.0195 13 1.000 0.000 C3 O3 C4 C2 H2O 0.0014 0.5557 -0.0786 147 0.840 0.000 O2 C2 H2O H3O 0.2782 0.5941 0.1306 147 0.840 0.000 O3 C3 H3O H4 0.1257 0.0745 -0.0584 147 0.840 0.000 O4B C4 H4 H21A 0.0640 1.0114 0.1355 137 0.980 0.000 C21 N22 H21A H21B 0.0692 0.8627 0.2135 137 0.980 0.000 C21 N22 H21A H21C 0.0154 0.8282 0.0803 137 0.980 0.000 C21 N22 H21A H22A 0.1933 0.8698 0.2341 137 0.910 0.000 N22 C21 H22A H22B 0.1421 0.8278 0.1112 137 0.910 0.000 N22 C21 H22A H22C 0.1500 0.6965 0.1893 137 0.910 0.000 N22 C21 H22A 04mbh0603 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.11746 0.74488 -0.08505 1.00000 0.01580 0.01798 0.01375 0.00072 0.00868 -0.00056 0.01644 0.00415 0.00010 0.00022 0.00014 0.00000 0.00077 0.00084 0.00081 0.00063 0.00068 0.00061 0.00036 C2 0.09771 0.55733 -0.07103 1.00000 0.01861 0.01539 0.01678 -0.00017 0.01295 -0.00136 0.01578 0.00431 0.00011 0.00021 0.00015 0.00000 0.00081 0.00084 0.00085 0.00062 0.00073 0.00060 0.00036 H2 0.06129 0.49710 -0.14678 1.00000 0.01894 0.00000 0.00000 C3 0.18459 0.45940 0.01168 1.00000 0.01795 0.01561 0.01880 0.00067 0.01312 -0.00078 0.01649 0.00423 0.00011 0.00021 0.00014 0.00000 0.00081 0.00087 0.00090 0.00062 0.00075 0.00060 0.00037 H3 0.21565 0.45926 -0.01948 1.00000 0.01979 0.00000 0.00000 C4 0.16532 0.27110 0.02300 1.00000 0.01642 0.01719 0.01980 0.00152 0.01203 0.00247 0.01752 0.00429 0.00010 0.00022 0.00014 0.00000 0.00079 0.00087 0.00091 0.00065 0.00073 0.00061 0.00037 O1A 0.10713 0.86870 -0.04018 1.00000 0.03689 0.01505 0.02952 -0.00135 0.02581 -0.00015 0.02390 0.00335 0.00008 0.00015 0.00011 0.00000 0.00075 0.00066 0.00076 0.00050 0.00066 0.00050 0.00032 O1B 0.14471 0.76143 -0.13893 1.00000 0.03161 0.02047 0.02394 -0.00338 0.02145 -0.00680 0.02271 0.00318 0.00008 0.00016 0.00011 0.00000 0.00070 0.00065 0.00070 0.00050 0.00061 0.00050 0.00031 O2 0.05534 0.54916 -0.02545 1.00000 0.01616 0.02556 0.02170 0.00353 0.01374 0.00070 0.01999 0.00312 0.00008 0.00016 0.00011 0.00000 0.00060 0.00069 0.00069 0.00050 0.00056 0.00047 0.00031 H2O 0.00143 0.55567 -0.07858 1.00000 0.02999 0.00000 0.00000 O3 0.23767 0.53898 0.12086 1.00000 0.01772 0.02150 0.01856 -0.00191 0.01062 -0.00506 0.02002 0.00290 0.00007 0.00015 0.00010 0.00000 0.00061 0.00069 0.00067 0.00047 0.00055 0.00045 0.00030 H3O 0.27816 0.59408 0.13061 1.00000 0.03003 0.00000 0.00000 O4A 0.17773 0.21657 0.10748 1.00000 0.02849 0.02038 0.02281 0.00206 0.01704 -0.00102 0.02349 0.00323 0.00008 0.00016 0.00011 0.00000 0.00068 0.00068 0.00070 0.00050 0.00059 0.00049 0.00031 O4B 0.13358 0.17813 -0.06843 1.00000 0.03082 0.01415 0.02487 -0.00200 0.01955 -0.00204 0.02207 0.00313 0.00008 0.00015 0.00011 0.00000 0.00070 0.00061 0.00071 0.00050 0.00061 0.00050 0.00031 H4 0.12567 0.07450 -0.05837 1.00000 0.03310 0.00000 0.00000 C21 0.06692 0.88484 0.14855 1.00000 0.02538 0.04515 0.02817 -0.00254 0.01763 0.00378 0.03259 0.00531 0.00012 0.00029 0.00018 0.00000 0.00099 0.00129 0.00114 0.00089 0.00093 0.00084 0.00049 H21A 0.06396 1.01140 0.13553 1.00000 0.04889 0.00000 0.00000 H21B 0.06920 0.86267 0.21351 1.00000 0.04889 0.00000 0.00000 H21C 0.01538 0.82821 0.08028 1.00000 0.04889 0.00000 0.00000 N22 0.14562 0.81285 0.17314 1.00000 0.02124 0.02421 0.02050 -0.00076 0.01258 0.00005 0.02259 0.00381 0.00009 0.00020 0.00013 0.00000 0.00075 0.00081 0.00081 0.00061 0.00067 0.00060 0.00035 H22A 0.19327 0.86985 0.23407 1.00000 0.03388 0.00000 0.00000 H22B 0.14206 0.82781 0.11124 1.00000 0.03388 0.00000 0.00000 H22C 0.15002 0.69654 0.18926 1.00000 0.03388 0.00000 0.00000 O1W 0.12214 0.44877 0.20221 1.00000 0.02688 0.02947 0.02263 0.00479 0.01822 0.00267 0.02464 0.00355 0.00009 0.00017 0.00012 0.00000 0.00071 0.00078 0.00075 0.00056 0.00064 0.00053 0.00032 H1W 0.13275 0.38565 0.25493 1.00000 0.03347 0.05647 0.00142 0.00272 0.00159 0.00000 0.00624 H2W 0.13764 0.39036 0.17081 1.00000 0.05599 0.06659 0.00169 0.00318 0.00201 0.00000 0.00830 Final Structure Factor Calculation for 04mbh0603 in C2/c Total number of l.s. parameters = 132 Maximum vector length = 511 Memory required = 1989 / 22995 wR2 = 0.1124 before cycle 5 for 2044 data and 0 / 132 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 0.006 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.060; Restrained GooF = 1.059 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0378 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0433 for 1617 Fo > 4sig(Fo) and 0.0595 for all 2044 data wR2 = 0.1124, GooF = S = 1.060, Restrained GooF = 1.059 for all data Occupancy sum of asymmetric unit = 13.00 for non-hydrogen and 13.00 for hydrogen atoms Principal mean square atomic displacements U 0.0192 0.0165 0.0136 C1 0.0193 0.0156 0.0125 C2 0.0192 0.0169 0.0133 C3 0.0205 0.0182 0.0138 C4 0.0373 0.0198 0.0145 O1A 0.0349 0.0185 0.0147 O1B 0.0279 0.0197 0.0124 O2 0.0258 0.0200 0.0142 O3 0.0293 0.0238 0.0174 O4A 0.0311 0.0214 0.0138 O4B 0.0477 0.0278 0.0223 C21 0.0248 0.0228 0.0202 N22 0.0323 0.0253 0.0163 O1W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.010 0.022 0.034 0.048 0.061 0.079 0.101 0.131 0.195 1.000 Number in group 215. 208. 195. 211. 193. 212. 203. 203. 198. 206. GooF 0.852 1.041 1.017 1.165 1.070 1.119 1.113 1.103 0.955 1.127 K 2.128 1.178 0.919 0.955 0.964 0.992 0.992 1.029 1.022 1.009 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.66 inf Number in group 212. 202. 205. 202. 200. 209. 202. 203. 205. 204. GooF 1.084 0.916 1.008 1.159 0.936 0.936 1.051 1.001 0.921 1.468 K 0.977 1.035 1.016 1.041 1.041 1.013 1.018 1.008 1.013 1.003 R1 0.162 0.116 0.117 0.096 0.072 0.050 0.048 0.034 0.028 0.033 Recommended weighting scheme: WGHT 0.0377 2.3394 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 0 1681.18 2921.98 5.26 0.243 6.84 -3 3 6 88.06 5.60 5.19 0.011 1.75 0 6 3 86.73 24.97 4.95 0.022 1.21 -12 0 6 215.40 65.77 4.84 0.036 1.68 0 0 6 965.48 465.62 4.32 0.097 1.95 12 0 0 377.23 126.88 4.17 0.051 1.28 -1 1 3 498.56 707.84 4.16 0.120 3.91 -6 8 4 119.19 284.42 4.10 0.076 0.91 -12 8 9 856.91 544.81 3.66 0.105 0.81 14 0 0 335.28 186.58 3.65 0.061 1.10 12 6 0 90.39 30.46 3.64 0.025 0.90 -3 9 7 115.13 343.23 3.62 0.083 0.78 -15 3 9 58.52 15.90 3.60 0.018 1.17 -12 2 11 121.22 59.27 3.56 0.035 1.27 3 7 6 33.83 108.87 3.53 0.047 0.89 -6 6 6 381.68 276.32 3.16 0.075 1.14 -3 1 2 2669.66 3121.38 2.95 0.251 4.91 8 4 6 70.52 128.25 2.93 0.051 0.93 -3 1 1 1671.74 1978.94 2.92 0.200 4.94 -24 0 12 15.50 89.35 2.91 0.043 0.84 11 1 8 159.13 367.98 2.87 0.086 0.79 -9 7 4 47.89 91.32 2.79 0.043 0.98 -9 1 4 7404.00 6482.48 2.79 0.362 2.14 6 6 0 14.16 0.69 2.76 0.004 1.14 -8 2 1 521.15 649.98 2.75 0.115 1.86 1 7 7 -4.67 19.15 2.73 0.020 0.89 11 7 3 307.49 537.97 2.71 0.104 0.78 -5 3 15 1331.35 1005.30 2.71 0.143 0.86 -9 3 9 388.28 289.28 2.70 0.077 1.40 0 2 1 7390.73 8478.74 2.65 0.414 3.63 -1 3 13 155.62 265.37 2.61 0.073 0.88 -2 2 9 253.50 338.60 2.59 0.083 1.35 -12 0 12 292.85 182.72 2.58 0.061 1.26 -12 6 10 50.84 92.41 2.58 0.043 0.95 -5 9 7 11.54 128.92 2.57 0.051 0.79 -3 7 2 174.23 261.53 2.55 0.073 1.07 5 9 1 38.89 115.92 2.52 0.048 0.81 -19 5 15 224.10 328.42 2.52 0.082 0.80 13 3 0 2.15 22.70 2.50 0.021 1.07 -13 3 17 67.44 121.54 2.48 0.050 0.85 -22 4 6 161.41 91.75 2.47 0.043 0.78 -8 0 2 957.15 797.33 2.47 0.127 2.33 -8 2 18 179.03 293.32 2.46 0.077 0.77 -2 2 15 41.39 109.04 2.45 0.047 0.81 -18 2 18 147.16 225.37 2.44 0.068 0.82 -6 2 4 3704.46 3276.18 2.38 0.258 2.45 -9 7 7 1120.98 941.34 2.35 0.138 0.96 -24 2 11 152.16 82.27 2.35 0.041 0.82 -19 1 1 64.10 19.49 2.35 0.020 0.84 -18 0 10 4172.31 3639.09 2.35 0.271 1.11 Bond lengths and angles C1 - Distance Angles O1B 1.2555 (0.0020) O1A 1.2611 (0.0020) 125.19 (0.15) C2 1.5364 (0.0023) 116.51 (0.14) 118.28 (0.14) C1 - O1B O1A C2 - Distance Angles O2 1.4069 (0.0019) C1 1.5364 (0.0023) 113.81 (0.13) C3 1.5393 (0.0024) 107.43 (0.13) 107.96 (0.13) H2 1.0000 109.18 109.18 109.18 C2 - O2 C1 C3 C3 - Distance Angles O3 1.4168 (0.0021) C4 1.5266 (0.0023) 108.86 (0.13) C2 1.5393 (0.0024) 110.99 (0.13) 108.27 (0.13) H3 1.0000 109.56 109.56 109.56 C3 - O3 C4 C2 C4 - Distance Angles O4A 1.2212 (0.0021) O4B 1.3115 (0.0021) 124.97 (0.16) C3 1.5266 (0.0023) 123.13 (0.15) 111.89 (0.14) C4 - O4A O4B O1A - Distance Angles C1 1.2611 (0.0020) O1A - O1B - Distance Angles C1 1.2555 (0.0020) O1B - O2 - Distance Angles C2 1.4069 (0.0019) H2O 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4168 (0.0021) H3O 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.2212 (0.0021) O4A - O4B - Distance Angles C4 1.3115 (0.0021) H4 0.8400 109.47 O4B - C4 C21 - Distance Angles N22 1.4770 (0.0023) 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 N22 - Distance Angles C21 1.4770 (0.0023) H22A 0.9100 109.47 H22B 0.9100 109.47 109.47 H22C 0.9100 109.47 109.47 109.47 N22 - C21 H22A H22B O1W - Distance Angles H1W 0.8409 (0.0151) H2W 0.8479 (0.0158) 106.48 (1.93) O1W - H1W Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.91 1.97 2.861(2) 167.4 N22-H22B...O1A 0.91 2.02 2.899(2) 162.9 N22-H22C...O1W 0.848(16) 2.086(17) 2.9276(19) 172(2) O1W-H2W...O4A 0.84 1.93 2.765(2) 175.5 O2-H2O...O1W_$1 0.84 1.84 2.6734(17) 171.9 O3-H3O...O1B_$2 0.84 1.68 2.5177(17) 178.5 O4B-H4...O1A_$3 0.91 2.14 2.985(2) 155.1 N22-H22A...O3_$4 0.91 2.43 3.016(3) 122.6 N22-H22A...O4A_$4 0.841(15) 1.858(16) 2.6962(19) 174(2) O1W-H1W...O1B_$5 FMAP and GRID set by program FMAP 2 1 39 GRID -0.694 -2 -1 0.694 2 1 R1 = 0.0595 for 2044 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.33 at 0.1778 0.3651 0.0220 [ 0.76 A from C4 ] Deepest hole -0.25 at 0.1699 0.4659 0.0485 [ 0.79 A from C3 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2160 / 31515 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1778 0.3651 0.0220 1.00000 0.05 0.33 0.76 C4 0.77 C3 1.46 H3 1.73 O4A Q2 1 0.1140 0.6576 -0.0633 1.00000 0.05 0.26 0.77 C1 0.81 C2 1.59 H2 1.67 O1A Q3 1 0.1265 -0.0175 -0.0330 1.00000 0.05 0.26 0.80 H4 0.93 O1A 1.62 O4B 1.94 C1 Q4 1 0.1390 0.5034 -0.0300 1.00000 0.05 0.24 0.76 C2 0.78 C3 1.43 H2 1.48 H3 Q5 1 0.1157 0.9638 0.0214 1.00000 0.05 0.23 1.11 O1A 1.52 H22B 1.60 H4 2.21 O4A Q6 1 0.0138 0.8922 0.0602 1.00000 0.05 0.22 0.57 H21C 1.06 C21 1.30 H21A 1.85 H21B Q7 1 0.1866 -0.0210 0.0335 1.00000 0.05 0.21 1.34 H4 1.49 O1A 1.93 O4B 2.16 H3 Q8 1 0.0526 0.0765 -0.1692 1.00000 0.05 0.21 1.35 H4 1.55 O4B 2.08 H21B 2.13 H21B Q9 1 -0.0294 0.8648 -0.0388 1.00000 0.05 0.20 1.45 H21C 1.50 H21A 2.20 C21 2.33 C21 Q10 1 0.1045 0.9653 0.2406 1.00000 0.05 0.20 0.95 H21B 1.25 C21 1.30 H21A 1.99 H22A Shortest distances between peaks (including symmetry equivalents) 3 7 0.96 3 5 1.00 6 9 1.18 1 4 1.25 2 4 1.25 5 7 1.32 3 8 1.76 6 9 1.94 8 8 1.97 6 10 2.19 8 10 2.22 6 6 2.26 9 9 2.29 5 6 2.32 5 9 2.32 5 8 2.47 1 2 2.48 2 3 2.50 5 6 2.53 5 9 2.54 7 8 2.59 8 10 2.62 2 5 2.66 6 8 2.73 9 10 2.74 3 6 2.74 2 7 2.75 1 7 2.95 Time profile in seconds ----------------------- 0.08: 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. 0.48: 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 0.31: Structure factors and derivatives 0.27: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.02: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04mbh0603 finished at 11:56:29 Total CPU time: 1.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++