+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005slh0414 started at 22:47:35 on 26-May-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005slh0414 in P2(1)/c CELL 0.71073 10.3791 17.5735 8.1030 90.000 100.512 90.000 ZERR 2.00 0.0006 0.0008 0.0003 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O P S CD UNIT 52 56 4 8 4 8 2 V = 1453.16 F(000) = 744.0 Mu = 1.19 mm-1 Cell Wt = 1470.17 Rho = 1.680 MERG 2 OMIT -3.00 55.00 FMAP 2 PLAN 5 SIZE 0.06 0.06 0.12 ACTA BOND $H L.S. 6 TEMP -153.00 WGHT 0.022500 1.244800 EXTI 0.004055 FVAR 0.44201 C1 1 -0.001746 0.642403 0.970383 11.00000 0.02043 0.02824 = 0.02314 -0.00020 -0.00839 -0.00157 AFIX 137 H1A 2 0.011214 0.588321 0.997975 11.00000 -1.50000 H1B 2 0.005308 0.672001 1.074149 11.00000 -1.50000 H1C 2 0.065313 0.659428 0.907751 11.00000 -1.50000 AFIX 0 C2 1 -0.326062 0.648588 0.621434 11.00000 0.01530 0.01547 = 0.01641 0.00116 0.00130 0.00061 C3 1 -0.359434 0.721867 0.665910 11.00000 0.01839 0.01808 = 0.01871 -0.00282 0.00032 -0.00001 AFIX 43 H3 2 -0.298883 0.750988 0.742841 11.00000 -1.20000 AFIX 0 C4 1 -0.480136 0.751848 0.598169 11.00000 0.02046 0.01641 = 0.02176 -0.00312 0.00169 0.00246 AFIX 43 H4 2 -0.502513 0.801613 0.629031 11.00000 -1.20000 AFIX 0 C5 1 -0.569411 0.709985 0.485168 11.00000 0.01429 0.01895 = 0.01822 0.00191 0.00163 0.00165 C6 1 -0.539366 0.636411 0.442464 11.00000 0.01588 0.01805 = 0.01869 -0.00275 -0.00114 -0.00147 AFIX 43 H6 2 -0.601015 0.607023 0.367601 11.00000 -1.20000 AFIX 0 C7 1 -0.417183 0.606546 0.511452 11.00000 0.01715 0.01595 = 0.02007 -0.00108 0.00076 0.00096 AFIX 43 H7 2 -0.395691 0.556313 0.482652 11.00000 -1.20000 AFIX 0 C8 1 -0.777608 0.707411 0.301279 11.00000 0.01578 0.02439 = 0.02508 -0.00204 -0.00413 0.00205 AFIX 137 H8A 2 -0.735971 0.690620 0.208289 11.00000 -1.50000 H8B 2 -0.850526 0.741698 0.258463 11.00000 -1.50000 H8C 2 -0.810734 0.663055 0.353811 11.00000 -1.50000 AFIX 0 C9 1 -0.229529 0.555288 0.180176 11.00000 0.01583 0.02416 = 0.02000 0.00293 -0.00154 -0.00278 AFIX 43 H9 2 -0.172100 0.597734 0.187259 11.00000 -1.20000 AFIX 0 C10 1 -0.347017 0.558873 0.067711 11.00000 0.01646 0.02270 = 0.01962 0.00450 -0.00166 0.00011 AFIX 43 H10 2 -0.367315 0.602240 -0.002194 11.00000 -1.20000 AFIX 0 C11 1 -0.435160 0.498785 0.057459 11.00000 0.01244 0.02029 = 0.01318 -0.00193 -0.00094 0.00174 C12 1 -0.395843 0.435974 0.159407 11.00000 0.01766 0.01964 = 0.02459 0.00200 -0.00496 -0.00195 AFIX 43 H12 2 -0.451702 0.392971 0.156258 11.00000 -1.20000 AFIX 0 C13 1 -0.274975 0.436608 0.265243 11.00000 0.02002 0.02051 = 0.02298 0.00295 -0.00525 0.00161 AFIX 43 H13 2 -0.249352 0.392712 0.331573 11.00000 -1.20000 AFIX 0 N1 3 -0.192356 0.495564 0.279244 11.00000 0.01302 0.02236 = 0.01691 0.00045 -0.00102 0.00105 O1 4 -0.129953 0.653387 0.869193 11.00000 0.01848 0.01997 = 0.01809 -0.00298 -0.00480 0.00086 O2 4 -0.683971 0.746461 0.422346 11.00000 0.01725 0.02082 = 0.02973 -0.00431 -0.00648 0.00550 P1 5 -0.164337 0.611810 0.691731 11.00000 0.01329 0.01395 = 0.01657 -0.00037 -0.00178 -0.00009 S1 6 -0.165402 0.499110 0.718426 11.00000 0.01695 0.01337 = 0.01989 0.00198 0.00100 -0.00021 S2 6 -0.043327 0.647469 0.540918 11.00000 0.01563 0.01604 = 0.02322 0.00239 0.00153 -0.00114 CD1 7 0.000000 0.500000 0.500000 10.50000 0.01149 0.01792 = 0.01771 -0.00110 -0.00271 0.00182 HKLF 4 Covalent radii and connectivity table for 2005slh0414 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 S 1.030 CD 1.490 C1 - O1 C2 - C7 C3 P1 C3 - C4 C2 C4 - C3 C5 C5 - O2 C6 C4 C6 - C5 C7 C7 - C2 C6 C8 - O2 C9 - N1 C10 C10 - C9 C11 C11 - C10 C12 C11_$1 C12 - C13 C11 C13 - N1 C12 N1 - C9 C13 Cd1 O1 - C1 P1 O2 - C5 C8 P1 - O1 C2 S1 S2 S1 - P1 Cd1 S2 - P1 Cd1 Cd1 - N1 N1_$2 S2_$2 S2 S1 S1_$2 Operators for generating equivalent atoms: $1 -x-1, -y+1, -z $2 -x, -y+1, -z+1 h k l Fo^2 Sigma Why rejected -1 0 1 3.65 0.78 observed but should be systematically absent -3 0 1 0.98 0.21 observed but should be systematically absent 32601 Reflections read, of which 682 rejected -13 =< h =< 13, -22 =< k =< 22, -10 =< l =< 10, Max. 2-theta = 54.99 2 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -10 9 2 -0.08 0.12 7 0.77 -10 4 3 48.34 2.34 7 14.61 -9 7 4 12.41 0.96 10 5.31 3 Inconsistent equivalents 3339 Unique reflections, of which 0 suppressed R(int) = 0.0360 R(sigma) = 0.0226 Friedel opposites merged Maximum memory for data reduction = 1989 / 33123 Special position constraints for Cd1 x = 0.0000 y = 0.5000 z = 0.5000 sof = 0.50000 Input constraints retained (at least in part) for sof Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 2494 / 227876 wR2 = 0.0572 before cycle 1 for 3339 data and 181 / 181 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0225 * P )^2 + 1.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.44201 0.00057 -0.004 OSF 2 0.00406 0.00037 0.001 EXTI Mean shift/esd = 0.004 Maximum = -0.044 for U23 Cd1 Max. shift = 0.000 A for H1C Max. dU = 0.000 for C6 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2494 / 227876 wR2 = 0.0572 before cycle 2 for 3339 data and 181 / 181 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0225 * P )^2 + 1.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.44201 0.00057 0.003 OSF 2 0.00406 0.00037 0.001 EXTI Mean shift/esd = 0.001 Maximum = -0.015 for U23 Cd1 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2494 / 227876 wR2 = 0.0572 before cycle 3 for 3339 data and 181 / 181 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0225 * P )^2 + 1.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.44201 0.00057 -0.002 OSF 2 0.00406 0.00037 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for U11 Cd1 Max. shift = 0.000 A for H8C Max. dU = 0.000 for O2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2494 / 227876 wR2 = 0.0572 before cycle 4 for 3339 data and 181 / 181 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0225 * P )^2 + 1.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.44201 0.00057 0.000 OSF 2 0.00406 0.00037 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y P1 Max. shift = 0.000 A for C3 Max. dU = 0.000 for O2 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2494 / 227876 wR2 = 0.0572 before cycle 5 for 3339 data and 181 / 181 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0225 * P )^2 + 1.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.44201 0.00057 0.001 OSF 2 0.00406 0.00037 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y P1 Max. shift = 0.000 A for C9 Max. dU = 0.000 for O2 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2494 / 227876 wR2 = 0.0572 before cycle 6 for 3339 data and 181 / 181 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0225 * P )^2 + 1.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.44201 0.00057 0.000 OSF 2 0.00406 0.00037 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y P1 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C4 Largest correlation matrix elements 0.603 EXTI / OSF 0.565 U33 Cd1 / OSF 0.591 U11 Cd1 / OSF 0.563 U22 Cd1 / OSF Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.0112 0.5883 0.9980 137 0.980 0.000 C1 O1 H1A H1B 0.0053 0.6720 1.0741 137 0.980 0.000 C1 O1 H1A H1C 0.0653 0.6594 0.9078 137 0.980 0.000 C1 O1 H1A H3 -0.2989 0.7510 0.7428 43 0.950 0.000 C3 C4 C2 H4 -0.5025 0.8016 0.6290 43 0.950 0.000 C4 C3 C5 H6 -0.6010 0.6070 0.3676 43 0.950 0.000 C6 C5 C7 H7 -0.3957 0.5563 0.4827 43 0.950 0.000 C7 C2 C6 H8A -0.7360 0.6906 0.2083 137 0.980 0.000 C8 O2 H8A H8B -0.8505 0.7417 0.2585 137 0.980 0.000 C8 O2 H8A H8C -0.8107 0.6631 0.3538 137 0.980 0.000 C8 O2 H8A H9 -0.1721 0.5977 0.1873 43 0.950 0.000 C9 N1 C10 H10 -0.3673 0.6022 -0.0022 43 0.950 0.000 C10 C9 C11 H12 -0.4517 0.3930 0.1563 43 0.950 0.000 C12 C13 C11 H13 -0.2494 0.3927 0.3316 43 0.950 0.000 C13 N1 C12 2005slh0414 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.00175 0.64240 0.97038 1.00000 0.02043 0.02824 0.02314 -0.00020 -0.00839 -0.00157 0.02549 0.00348 0.00018 0.00012 0.00025 0.00000 0.00094 0.00107 0.00099 0.00079 0.00076 0.00076 0.00043 H1A 0.01121 0.58832 0.99798 1.00000 0.03824 0.00000 0.00000 H1B 0.00531 0.67200 1.07415 1.00000 0.03824 0.00000 0.00000 H1C 0.06531 0.65943 0.90775 1.00000 0.03824 0.00000 0.00000 C2 -0.32606 0.64859 0.62143 1.00000 0.01530 0.01547 0.01641 0.00116 0.00130 0.00061 0.01593 0.00320 0.00017 0.00010 0.00022 0.00000 0.00079 0.00084 0.00085 0.00066 0.00065 0.00065 0.00034 C3 -0.35943 0.72187 0.66591 1.00000 0.01839 0.01808 0.01871 -0.00282 0.00032 -0.00001 0.01878 0.00331 0.00017 0.00010 0.00023 0.00000 0.00083 0.00088 0.00088 0.00070 0.00068 0.00069 0.00036 H3 -0.29888 0.75099 0.74284 1.00000 0.02254 0.00000 0.00000 C4 -0.48014 0.75185 0.59817 1.00000 0.02046 0.01641 0.02176 -0.00312 0.00169 0.00246 0.01981 0.00333 0.00017 0.00010 0.00023 0.00000 0.00085 0.00087 0.00092 0.00071 0.00071 0.00071 0.00037 H4 -0.50251 0.80161 0.62903 1.00000 0.02378 0.00000 0.00000 C5 -0.56941 0.70998 0.48517 1.00000 0.01429 0.01895 0.01822 0.00191 0.00163 0.00165 0.01732 0.00328 0.00017 0.00010 0.00022 0.00000 0.00079 0.00088 0.00087 0.00069 0.00066 0.00067 0.00035 C6 -0.53937 0.63641 0.44246 1.00000 0.01588 0.01805 0.01869 -0.00275 -0.00114 -0.00147 0.01808 0.00327 0.00017 0.00010 0.00023 0.00000 0.00081 0.00088 0.00087 0.00070 0.00068 0.00068 0.00036 H6 -0.60101 0.60702 0.36760 1.00000 0.02169 0.00000 0.00000 C7 -0.41718 0.60655 0.51145 1.00000 0.01715 0.01595 0.02007 -0.00108 0.00076 0.00096 0.01806 0.00326 0.00017 0.00010 0.00023 0.00000 0.00082 0.00086 0.00089 0.00070 0.00068 0.00067 0.00036 H7 -0.39569 0.55631 0.48265 1.00000 0.02167 0.00000 0.00000 C8 -0.77761 0.70741 0.30128 1.00000 0.01578 0.02439 0.02508 -0.00204 -0.00413 0.00205 0.02274 0.00333 0.00017 0.00011 0.00024 0.00000 0.00083 0.00096 0.00098 0.00078 0.00072 0.00073 0.00039 H8A -0.73597 0.69062 0.20829 1.00000 0.03410 0.00000 0.00000 H8B -0.85053 0.74170 0.25846 1.00000 0.03410 0.00000 0.00000 H8C -0.81073 0.66306 0.35381 1.00000 0.03410 0.00000 0.00000 C9 -0.22953 0.55529 0.18018 1.00000 0.01583 0.02416 0.02000 0.00293 -0.00154 -0.00278 0.02060 0.00342 0.00017 0.00011 0.00023 0.00000 0.00081 0.00095 0.00092 0.00074 0.00069 0.00071 0.00038 H9 -0.17210 0.59773 0.18726 1.00000 0.02473 0.00000 0.00000 C10 -0.34702 0.55887 0.06771 1.00000 0.01646 0.02270 0.01962 0.00450 -0.00166 0.00011 0.02022 0.00336 0.00017 0.00011 0.00023 0.00000 0.00083 0.00095 0.00093 0.00072 0.00069 0.00071 0.00038 H10 -0.36732 0.60224 -0.00219 1.00000 0.02426 0.00000 0.00000 C11 -0.43516 0.49879 0.05746 1.00000 0.01244 0.02029 0.01318 -0.00193 -0.00094 0.00174 0.01572 0.00315 0.00017 0.00010 0.00022 0.00000 0.00084 0.00091 0.00083 0.00065 0.00068 0.00063 0.00036 C12 -0.39584 0.43597 0.15941 1.00000 0.01766 0.01964 0.02459 0.00200 -0.00496 -0.00195 0.02174 0.00339 0.00018 0.00011 0.00024 0.00000 0.00085 0.00092 0.00099 0.00074 0.00073 0.00071 0.00039 H12 -0.45170 0.39297 0.15626 1.00000 0.02608 0.00000 0.00000 C13 -0.27497 0.43661 0.26524 1.00000 0.02002 0.02051 0.02298 0.00295 -0.00525 0.00161 0.02232 0.00343 0.00018 0.00011 0.00024 0.00000 0.00089 0.00093 0.00097 0.00074 0.00073 0.00073 0.00039 H13 -0.24935 0.39271 0.33157 1.00000 0.02679 0.00000 0.00000 N1 -0.19236 0.49556 0.27924 1.00000 0.01302 0.02236 0.01691 0.00045 -0.00102 0.00105 0.01790 0.00279 0.00015 0.00008 0.00020 0.00000 0.00070 0.00083 0.00078 0.00058 0.00058 0.00056 0.00032 O1 -0.12995 0.65339 0.86919 1.00000 0.01848 0.01997 0.01809 -0.00298 -0.00480 0.00086 0.01987 0.00222 0.00012 0.00007 0.00016 0.00000 0.00061 0.00065 0.00064 0.00051 0.00050 0.00050 0.00027 O2 -0.68397 0.74646 0.42235 1.00000 0.01725 0.02082 0.02973 -0.00431 -0.00648 0.00550 0.02395 0.00234 0.00012 0.00007 0.00017 0.00000 0.00061 0.00068 0.00075 0.00056 0.00053 0.00052 0.00030 P1 -0.16434 0.61181 0.69173 1.00000 0.01329 0.01395 0.01657 -0.00037 -0.00178 -0.00009 0.01517 0.00081 0.00004 0.00003 0.00006 0.00000 0.00020 0.00022 0.00022 0.00017 0.00016 0.00016 0.00011 S1 -0.16540 0.49911 0.71843 1.00000 0.01695 0.01337 0.01989 0.00198 0.00100 -0.00021 0.01703 0.00083 0.00004 0.00002 0.00006 0.00000 0.00022 0.00022 0.00023 0.00016 0.00017 0.00015 0.00011 S2 -0.04333 0.64747 0.54092 1.00000 0.01563 0.01604 0.02322 0.00239 0.00153 -0.00114 0.01855 0.00082 0.00004 0.00002 0.00006 0.00000 0.00021 0.00022 0.00024 0.00017 0.00017 0.00016 0.00011 Cd1 0.00000 0.50000 0.50000 0.50000 0.01149 0.01792 0.01771 -0.00110 -0.00271 0.00182 0.01638 0.00000 0.00000 0.00000 0.00000 0.00000 0.00010 0.00011 0.00011 0.00007 0.00007 0.00006 0.00007 Final Structure Factor Calculation for 2005slh0414 in P2(1)/c Total number of l.s. parameters = 181 Maximum vector length = 511 Memory required = 2313 / 26061 wR2 = 0.0572 before cycle 7 for 3339 data and 0 / 181 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0225 * P )^2 + 1.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0236 for 2952 Fo > 4sig(Fo) and 0.0291 for all 3339 data wR2 = 0.0572, GooF = S = 1.046, Restrained GooF = 1.046 for all data Occupancy sum of asymmetric unit = 19.50 for non-hydrogen and 14.00 for hydrogen atoms Principal mean square atomic displacements U 0.0371 0.0282 0.0112 C1 0.0181 0.0160 0.0137 C2 0.0234 0.0182 0.0148 C3 0.0259 0.0192 0.0144 C4 0.0205 0.0181 0.0134 C5 0.0232 0.0188 0.0123 C6 0.0226 0.0162 0.0154 C7 0.0325 0.0233 0.0124 C8 0.0286 0.0199 0.0133 C9 0.0276 0.0201 0.0129 C10 0.0219 0.0152 0.0100 C11 0.0332 0.0190 0.0130 C12 0.0330 0.0214 0.0126 C13 0.0225 0.0200 0.0112 N1 0.0292 0.0192 0.0112 O1 0.0410 0.0192 0.0117 O2 0.0207 0.0140 0.0108 P1 0.0222 0.0161 0.0128 S1 0.0251 0.0160 0.0146 S2 0.0229 0.0172 0.0091 Cd1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.030 0.048 0.066 0.090 0.117 0.151 0.195 0.263 1.000 Number in group 352. 333. 334. 318. 339. 326. 337. 337. 328. 335. GooF 1.047 1.032 1.026 1.047 1.060 1.063 1.085 0.944 1.047 1.106 K 1.423 0.934 0.961 0.957 0.966 0.987 0.992 1.003 1.013 1.008 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.65 inf Number in group 346. 326. 337. 326. 338. 329. 336. 334. 333. 334. GooF 1.080 0.995 0.953 0.965 0.890 0.951 0.921 0.871 1.066 1.585 K 0.979 1.003 1.001 1.007 1.017 1.019 1.022 1.018 1.007 0.991 R1 0.062 0.053 0.041 0.036 0.029 0.027 0.021 0.017 0.018 0.021 Recommended weighting scheme: WGHT 0.0214 1.2964 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) -2 3 1 604.24 777.25 4.88 0.122 3.67 3 5 2 1071.07 878.37 4.47 0.130 1.97 3 6 0 461.71 584.47 4.08 0.106 2.22 2 4 3 2678.45 2359.10 3.74 0.213 1.97 0 6 3 678.13 557.63 3.73 0.103 1.97 2 2 3 -1.08 13.41 3.67 0.016 2.13 -6 3 4 23.70 6.12 3.64 0.011 1.39 1 6 2 2663.44 3003.65 3.61 0.240 2.25 -4 6 3 947.31 1107.24 3.54 0.146 1.67 0 2 2 267.47 204.90 3.40 0.063 3.63 2 9 1 3113.05 3463.85 3.31 0.258 1.75 -2 5 1 3684.38 4083.04 3.27 0.280 2.82 -2 9 1 157.59 113.29 3.24 0.047 1.80 -1 10 2 137.81 189.17 3.23 0.060 1.61 3 4 1 1415.81 1244.46 3.19 0.154 2.44 -4 5 1 2976.95 3296.45 3.15 0.251 2.07 4 16 0 720.39 871.19 3.09 0.129 1.01 -2 3 3 1348.02 1524.40 3.09 0.171 2.34 3 4 0 887.68 1021.97 3.06 0.140 2.69 -9 8 7 43.51 83.62 3.05 0.040 0.82 5 7 4 13.22 0.34 3.05 0.003 1.16 -5 0 2 1860.41 2097.46 3.02 0.200 1.97 9 13 3 192.47 280.73 3.01 0.073 0.79 7 2 1 15.93 3.46 2.99 0.008 1.37 5 1 0 1196.51 1057.30 2.95 0.142 2.03 -4 19 4 169.43 240.95 2.93 0.068 0.82 -2 7 2 200.11 255.10 2.89 0.070 2.03 -6 9 7 143.64 196.16 2.88 0.061 0.92 -4 0 4 94.57 62.83 2.88 0.035 1.73 -2 1 1 2.42 12.94 2.83 0.016 4.54 3 7 0 180.77 138.09 2.82 0.051 2.02 5 5 0 21.09 8.19 2.82 0.013 1.76 0 5 3 1705.67 1891.95 2.78 0.190 2.12 -3 2 7 12.22 0.21 2.78 0.002 1.13 2 5 2 332.35 272.99 2.76 0.072 2.23 2 4 0 25.70 10.57 2.75 0.014 3.33 -8 13 3 773.65 897.59 2.74 0.131 0.91 -5 14 5 395.70 474.96 2.72 0.095 0.93 4 1 0 543.61 466.58 2.70 0.095 2.52 -2 8 1 16.55 33.67 2.70 0.025 1.99 -2 6 3 615.62 532.12 2.69 0.101 1.93 -4 7 1 6056.94 6542.36 2.66 0.354 1.80 4 2 2 630.71 722.95 2.66 0.118 1.94 3 9 6 -4.13 13.82 2.64 0.016 1.00 -11 13 1 259.20 340.52 2.63 0.081 0.77 10 1 3 3589.94 3267.14 2.61 0.250 0.90 4 1 2 342.87 407.77 2.61 0.088 1.98 6 12 5 45.49 83.83 2.61 0.040 0.86 -6 18 1 397.74 519.23 2.58 0.100 0.85 1 9 0 460.08 393.64 2.57 0.087 1.92 Bond lengths and angles C1 - Distance Angles O1 1.4430 (0.0021) H1A 0.9800 109.47 H1B 0.9800 109.47 109.47 H1C 0.9800 109.47 109.47 109.47 C1 - O1 H1A H1B C2 - Distance Angles C7 1.3882 (0.0024) C3 1.3978 (0.0024) 118.95 (0.16) P1 1.7919 (0.0018) 120.07 (0.13) 120.81 (0.13) C2 - C7 C3 C3 - Distance Angles C4 1.3775 (0.0025) C2 1.3978 (0.0024) 119.99 (0.17) H3 0.9500 120.01 120.01 C3 - C4 C2 C4 - Distance Angles C3 1.3775 (0.0025) C5 1.3888 (0.0025) 120.60 (0.17) H4 0.9500 119.70 119.70 C4 - C3 C5 C5 - Distance Angles O2 1.3649 (0.0021) C6 1.3885 (0.0025) 124.36 (0.16) C4 1.3888 (0.0025) 115.35 (0.16) 120.29 (0.16) C5 - O2 C6 C6 - Distance Angles C5 1.3885 (0.0025) C7 1.3919 (0.0024) 118.72 (0.16) H6 0.9500 120.64 120.64 C6 - C5 C7 C7 - Distance Angles C2 1.3882 (0.0024) C6 1.3919 (0.0024) 121.41 (0.17) H7 0.9500 119.29 119.29 C7 - C2 C6 C8 - Distance Angles O2 1.4248 (0.0022) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - O2 H8A H8B C9 - Distance Angles N1 1.3349 (0.0023) C10 1.3842 (0.0025) 123.71 (0.17) H9 0.9500 118.15 118.15 C9 - N1 C10 C10 - Distance Angles C9 1.3842 (0.0025) C11 1.3897 (0.0025) 119.74 (0.17) H10 0.9500 120.13 120.13 C10 - C9 C11 C11 - Distance Angles C10 1.3897 (0.0025) C12 1.3944 (0.0025) 116.60 (0.16) C11_$1 1.4910 (0.0034) 121.67 (0.20) 121.73 (0.20) C11 - C10 C12 C12 - Distance Angles C13 1.3845 (0.0025) C11 1.3944 (0.0025) 119.66 (0.17) H12 0.9500 120.17 120.17 C12 - C13 C11 C13 - Distance Angles N1 1.3365 (0.0024) C12 1.3845 (0.0025) 123.62 (0.17) H13 0.9500 118.19 118.19 C13 - N1 C12 N1 - Distance Angles C9 1.3349 (0.0023) C13 1.3365 (0.0024) 116.61 (0.16) Cd1 2.4267 (0.0015) 121.78 (0.12) 121.09 (0.12) N1 - C9 C13 O1 - Distance Angles C1 1.4430 (0.0021) P1 1.5943 (0.0013) 118.86 (0.12) O1 - C1 O2 - Distance Angles C5 1.3649 (0.0021) C8 1.4248 (0.0022) 117.97 (0.14) O2 - C5 P1 - Distance Angles O1 1.5943 (0.0013) C2 1.7919 (0.0018) 99.44 (0.08) S1 1.9926 (0.0006) 111.25 (0.05) 111.69 (0.06) S2 2.0059 (0.0007) 110.14 (0.05) 110.37 (0.06) 113.15 (0.03) P1 - O1 C2 S1 S1 - Distance Angles P1 1.9926 (0.0006) Cd1 2.6812 (0.0005) 84.59 (0.02) S1 - P1 S2 - Distance Angles P1 2.0059 (0.0007) Cd1 2.6613 (0.0005) 84.87 (0.02) S2 - P1 Cd1 - Distance Angles N1 2.4267 (0.0015) N1_$2 2.4267 (0.0015) 180.00 S2_$2 2.6613 (0.0005) 90.68 (0.04) 89.32 (0.04) S2 2.6613 (0.0005) 89.32 (0.04) 90.68 (0.04) 180.00 (0.02) S1 2.6812 (0.0005) 86.94 (0.04) 93.06 (0.04) 102.69 (0.01) 77.31 (0.01) S1_$2 2.6812 (0.0005) 93.06 (0.04) 86.94 (0.04) 77.31 (0.01) 102.69 (0.01) 180.00 Cd1 - N1 N1_$2 S2_$2 S2 S1 FMAP and GRID set by program FMAP 2 2 22 GRID -1.316 -2 -2 1.316 2 2 R1 = 0.0287 for 3339 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.54 at 0.9544 0.1479 0.0435 [ 1.24 A from S2 ] Deepest hole -0.45 at 0.9744 0.0243 0.9203 [ 0.78 A from CD1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2307 / 18165 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0456 0.6479 0.4565 1.00000 0.05 0.54 1.24 S2 1.86 H8C 2.57 H13 2.62 C8 Q2 1 -0.8337 0.6114 0.3067 1.00000 0.05 0.52 1.00 H8C 1.79 C8 1.95 S1 1.97 H8A Q3 1 -0.5000 0.5000 0.0000 0.50000 0.05 0.44 0.75 C11 1.89 C10 1.90 C12 2.27 H10 Q4 1 0.1063 0.5011 0.4336 1.00000 0.05 0.33 1.31 CD1 1.47 S1 2.34 N1 2.36 P1 Q5 1 0.0046 0.6014 0.4824 1.00000 0.05 0.32 1.10 S2 1.79 CD1 2.58 H8C 2.66 P1 Shortest distances between peaks (including symmetry equivalents) 1 5 0.96 1 2 2.00 4 5 2.13 4 5 2.31 2 4 2.33 2 5 2.40 4 4 2.63 1 4 2.67 Time profile in seconds ----------------------- 0.04: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.01: Analyse DFIX/DANG restraints 0.00: 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. 1.67: 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 1.26: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.16: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.07: Analysis of variance 0.04: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.04: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005slh0414 finished at 22:47:39 Total CPU time: 4.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++