++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XL - CRYSTAL STRUCTURE REFINEMENT - SHELXTL Ver. 6.12 W95/98/NT/2000/ME + + Copyright(c) 2001 Bruker Analytical X-ray Solutions All Rights Reserved + + jsib001 started at 14:06:23 on 02-Nov-2005 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL jsib001 in P2(1)2(1)2(1) CELL 0.71073 10.0096 12.4633 16.4230 90.000 90.000 90.000 ZERR 4.00 0.0041 0.0050 0.0065 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O F NA P UNIT 64 104 8 12 24 4 4 V = 2048.81 F(000) = 960.0 Mu = 0.23 mm-1 Cell Wt = 1849.39 Rho = 1.499 TEMP -153 SIZE 0.08 0.10 0.20 L.S. 20 BOND $H FMAP 2 PLAN 20 ACTA 50 TWIN CONF WPDB WGHT 0.036400 0.013800 MOVE 1 1 1 -1 BASF 0.4 FVAR 0.72760 NA 6 0.002599 0.088569 0.139451 11.00000 0.02425 0.02873 = 0.02447 0.00011 -0.00076 -0.00328 O1 4 0.097751 0.025888 0.264895 11.00000 0.03261 0.04473 = 0.02789 0.00068 -0.00905 -0.00367 O2 4 0.071945 0.238775 0.219526 11.00000 0.03883 0.03981 = 0.02837 -0.00351 -0.00790 -0.00708 O3 4 0.074129 0.235777 0.053089 11.00000 0.03665 0.02148 = 0.03386 -0.00424 0.00103 -0.00120 P1 7 -0.312031 0.071653 0.197955 11.00000 0.02386 0.03153 = 0.02524 0.00686 0.00116 0.00040 F1 5 -0.427639 0.154529 0.218811 11.00000 0.04084 0.04204 = 0.03785 0.00249 0.00706 0.01246 F2 5 -0.384167 0.041214 0.114569 11.00000 0.02668 0.03471 = 0.03232 0.00502 -0.00574 -0.00189 F3 5 -0.389617 -0.022452 0.243423 11.00000 0.03657 0.04110 = 0.04260 0.01841 0.01167 -0.00279 F4 5 -0.191855 -0.010287 0.175132 11.00000 0.02714 0.03433 = 0.03490 0.00868 0.00211 0.00422 F5 5 -0.236601 0.101228 0.280625 11.00000 0.04438 0.05723 = 0.02566 0.00274 -0.00661 -0.00261 F6 5 -0.229617 0.165051 0.151408 11.00000 0.03370 0.02648 = 0.03494 0.00688 0.00107 -0.00557 N1 3 0.178982 -0.046126 0.105896 11.00000 0.02316 0.03425 = 0.02804 0.00305 -0.00706 -0.00016 N2 3 -0.012609 0.035910 -0.008205 11.00000 0.02231 0.02110 = 0.02233 0.00311 0.00055 0.00050 C1 1 0.047233 -0.069030 -0.019992 11.00000 0.01979 0.02662 = 0.02432 0.00123 0.00348 -0.00144 C2 1 0.012356 -0.130480 -0.087180 11.00000 0.02600 0.03208 = 0.03310 -0.00368 0.00031 -0.00023 AFIX 43 H2A 2 -0.043882 -0.100263 -0.127744 11.00000 -1.20000 AFIX 0 C3 1 0.057496 -0.234680 -0.096524 11.00000 0.02886 0.03719 = 0.04415 -0.01203 0.00481 -0.00051 AFIX 43 H3A 2 0.032891 -0.275477 -0.143028 11.00000 -1.20000 AFIX 0 C4 1 0.138332 -0.278303 -0.037667 11.00000 0.04401 0.02714 = 0.06307 -0.00821 0.00078 0.01025 AFIX 43 H4A 2 0.167003 -0.350696 -0.042414 11.00000 -1.20000 AFIX 0 C5 1 0.178248 -0.217744 0.028354 11.00000 0.03819 0.03300 = 0.05232 0.00297 -0.00927 0.01364 AFIX 43 H5A 2 0.236125 -0.248618 0.067759 11.00000 -1.20000 AFIX 0 C6 1 0.134872 -0.111102 0.038447 11.00000 0.02222 0.02784 = 0.03247 0.00052 -0.00117 -0.00026 C7 1 0.300403 0.013614 0.082659 11.00000 0.03144 0.05647 = 0.03712 -0.00191 -0.00134 -0.01221 AFIX 33 H7A 2 0.371545 -0.037163 0.068664 11.00000 -1.50000 H7B 2 0.329350 0.058484 0.128375 11.00000 -1.50000 H7C 2 0.280959 0.059197 0.035503 11.00000 -1.50000 AFIX 0 C8 1 0.202167 -0.106912 0.181452 11.00000 0.03340 0.04062 = 0.03880 0.00879 -0.00615 0.00707 AFIX 23 H8A 2 0.283962 -0.150799 0.175186 11.00000 -1.20000 H8B 2 0.126255 -0.156392 0.190572 11.00000 -1.20000 AFIX 0 C9 1 0.217553 -0.034654 0.255165 11.00000 0.03443 0.06225 = 0.03168 0.01177 -0.01380 0.00499 AFIX 23 H9A 2 0.234178 -0.078466 0.304416 11.00000 -1.20000 H9B 2 0.294387 0.014301 0.247376 11.00000 -1.20000 AFIX 0 C10 1 0.104767 0.111451 0.323684 11.00000 0.05212 0.05491 = 0.02558 -0.00194 -0.00755 -0.00899 AFIX 23 H10A 2 0.164259 0.089740 0.368935 11.00000 -1.20000 H10B 2 0.014665 0.124390 0.346523 11.00000 -1.20000 AFIX 0 C11 1 0.156629 0.213822 0.286245 11.00000 0.04887 0.05183 = 0.03743 -0.01045 -0.01331 -0.00914 AFIX 23 H11A 2 0.155042 0.272635 0.326752 11.00000 -1.20000 H11B 2 0.249724 0.203954 0.267317 11.00000 -1.20000 AFIX 0 C12 1 0.118189 0.329221 0.172984 11.00000 0.04219 0.02562 = 0.04447 -0.00445 -0.00140 -0.01163 AFIX 23 H12A 2 0.215106 0.322251 0.162185 11.00000 -1.20000 H12B 2 0.103141 0.396387 0.203832 11.00000 -1.20000 AFIX 0 C13 1 0.043941 0.332476 0.095497 11.00000 0.03544 0.02441 = 0.04219 -0.00670 0.00802 -0.00610 AFIX 23 H13A 2 -0.053258 0.337548 0.105958 11.00000 -1.20000 H13B 2 0.071640 0.395484 0.062903 11.00000 -1.20000 AFIX 0 C14 1 0.016968 0.230325 -0.026199 11.00000 0.05174 0.02293 = 0.02874 0.00609 0.00387 -0.00657 AFIX 23 H14A 2 0.056505 0.286018 -0.061791 11.00000 -1.20000 H14B 2 -0.080696 0.242277 -0.023316 11.00000 -1.20000 AFIX 0 C15 1 0.046111 0.120325 -0.059615 11.00000 0.03544 0.02853 = 0.02362 0.00311 0.00663 -0.00314 AFIX 23 H15A 2 0.009409 0.114591 -0.115423 11.00000 -1.20000 H15B 2 0.144011 0.109839 -0.062806 11.00000 -1.20000 AFIX 0 C16 1 -0.157914 0.031537 -0.022268 11.00000 0.02533 0.03683 = 0.03112 -0.00295 -0.00121 0.00745 AFIX 33 H16A 2 -0.175267 0.011457 -0.078984 11.00000 -1.50000 H16B 2 -0.197138 0.102110 -0.011272 11.00000 -1.50000 H16C 2 -0.197965 -0.021863 0.014101 11.00000 -1.50000 HKLF 4 Covalent radii and connectivity table for jsib001 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 NA 1.860 P 1.100 Na - F4 O2 O1 O3 N1 N2 F6 P1 O1 - C9 C10 Na O2 - C11 C12 Na O3 - C14 C13 Na P1 - F1 F3 F2 F5 F6 F4 Na F1 - P1 F2 - P1 F3 - P1 F4 - P1 Na F5 - P1 F6 - P1 Na N1 - C6 C8 C7 Na N2 - C1 C15 C16 Na C1 - C2 C6 N2 C2 - C3 C1 C3 - C4 C2 C4 - C3 C5 C5 - C4 C6 C6 - C1 C5 N1 C7 - N1 C8 - N1 C9 C9 - O1 C8 C10 - O1 C11 C11 - O2 C10 C12 - O2 C13 C13 - O3 C12 C14 - O3 C15 C15 - N2 C14 C16 - N2 17529 Reflections read, of which 54 rejected -12 =< h =< 12, -16 =< k =< 16, -19 =< l =< 20, Max. 2-theta = 56.55 0 Systematic absence violations 0 Inconsistent equivalents 4674 Unique reflections, of which 0 suppressed R(int) = 0.0644 R(sigma) = 0.0694 Friedel opposites not merged Maximum memory for data reduction = 4264 / 46054 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 = 5031 / 330089 wR2 = 0.0941 before cycle 1 for 4674 data and 263 / 263 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0364 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72759 0.00100 -0.006 OSF 2 0.37110 0.12348 -0.234 BASF 1 Mean shift/esd = 0.003 Maximum = -0.234 for BASF 1 Max. shift = 0.000 A for C8 Max. dU = 0.000 for F1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5031 / 330089 wR2 = 0.0941 before cycle 2 for 4674 data and 263 / 263 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0364 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72760 0.00100 0.003 OSF 2 0.36162 0.12348 -0.077 BASF 1 Mean shift/esd = 0.001 Maximum = -0.077 for BASF 1 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C16 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5031 / 330089 wR2 = 0.0941 before cycle 3 for 4674 data and 263 / 263 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0364 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72760 0.00100 0.001 OSF 2 0.36164 0.12348 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for C2 Max. dU = 0.000 for C16 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5031 / 330089 wR2 = 0.0941 before cycle 4 for 4674 data and 263 / 263 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0364 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72760 0.00100 0.000 OSF 2 0.36165 0.12348 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for y F3 Max. shift = 0.000 A for F3 Max. dU = 0.000 for C10 Least-squares cycle 5 Maximum vector length = 511 Memory required = 5031 / 330089 wR2 = 0.0941 before cycle 5 for 4674 data and 263 / 263 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0364 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72760 0.00100 0.001 OSF 2 0.36164 0.12348 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for C4 Max. dU = 0.000 for F3 Least-squares cycle 6 Maximum vector length = 511 Memory required = 5031 / 330089 wR2 = 0.0941 before cycle 6 for 4674 data and 263 / 263 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0364 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72760 0.00100 0.000 OSF 2 0.36164 0.12348 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for y F3 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C5 Least-squares cycle 7 Maximum vector length = 511 Memory required = 5031 / 330089 wR2 = 0.0941 before cycle 7 for 4674 data and 263 / 263 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0364 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72760 0.00100 0.000 OSF 2 0.36164 0.12348 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for x F3 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C9 Least-squares cycle 8 Maximum vector length = 511 Memory required = 5031 / 330089 wR2 = 0.0941 before cycle 8 for 4674 data and 263 / 263 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0364 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72760 0.00100 0.000 OSF 2 0.36164 0.12348 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z F4 Max. shift = 0.000 A for C14 Max. dU = 0.000 for C7 Least-squares cycle 9 Maximum vector length = 511 Memory required = 5031 / 330089 wR2 = 0.0941 before cycle 9 for 4674 data and 263 / 263 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0364 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72760 0.00100 0.000 OSF 2 0.36164 0.12348 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for x F3 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C16 Least-squares cycle 10 Maximum vector length = 511 Memory required = 5031 / 330089 wR2 = 0.0941 before cycle 10 for 4674 data and 263 / 263 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0364 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72760 0.00100 0.000 OSF 2 0.36164 0.12348 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z F4 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C9 Least-squares cycle 11 Maximum vector length = 511 Memory required = 5031 / 330089 wR2 = 0.0941 before cycle 11 for 4674 data and 263 / 263 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0364 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72760 0.00100 0.000 OSF 2 0.36164 0.12348 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.001 for x F3 Max. shift = 0.000 A for C14 Max. dU = 0.000 for C16 Least-squares cycle 12 Maximum vector length = 511 Memory required = 5031 / 330089 wR2 = 0.0941 before cycle 12 for 4674 data and 263 / 263 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0364 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72760 0.00100 0.000 OSF 2 0.36164 0.12348 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z C1 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C4 Least-squares cycle 13 Maximum vector length = 511 Memory required = 5031 / 330089 wR2 = 0.0941 before cycle 13 for 4674 data and 263 / 263 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0364 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72760 0.00100 0.000 OSF 2 0.36164 0.12348 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for x F3 Max. shift = 0.000 A for C14 Max. dU = 0.000 for C13 Least-squares cycle 14 Maximum vector length = 511 Memory required = 5031 / 330089 wR2 = 0.0941 before cycle 14 for 4674 data and 263 / 263 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0364 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72760 0.00100 0.000 OSF 2 0.36164 0.12348 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C4 Max. dU = 0.000 for C15 Least-squares cycle 15 Maximum vector length = 511 Memory required = 5031 / 330089 wR2 = 0.0941 before cycle 15 for 4674 data and 263 / 263 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0364 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72760 0.00100 0.000 OSF 2 0.36164 0.12348 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.001 for x F3 Max. shift = 0.000 A for F3 Max. dU = 0.000 for O2 Least-squares cycle 16 Maximum vector length = 511 Memory required = 5031 / 330089 wR2 = 0.0941 before cycle 16 for 4674 data and 263 / 263 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0364 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72760 0.00100 0.000 OSF 2 0.36164 0.12348 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z C14 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C8 Least-squares cycle 17 Maximum vector length = 511 Memory required = 5031 / 330089 wR2 = 0.0941 before cycle 17 for 4674 data and 263 / 263 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0364 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72760 0.00100 0.000 OSF 2 0.36165 0.12348 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for x F3 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C11 Least-squares cycle 18 Maximum vector length = 511 Memory required = 5031 / 330089 wR2 = 0.0941 before cycle 18 for 4674 data and 263 / 263 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0364 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72760 0.00100 0.000 OSF 2 0.36165 0.12348 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z F4 Max. shift = 0.000 A for C14 Max. dU = 0.000 for C9 Least-squares cycle 19 Maximum vector length = 511 Memory required = 5031 / 330089 wR2 = 0.0941 before cycle 19 for 4674 data and 263 / 263 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0364 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72760 0.00100 0.000 OSF 2 0.36164 0.12348 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for x F3 Max. shift = 0.000 A for F3 Max. dU = 0.000 for F4 Least-squares cycle 20 Maximum vector length = 511 Memory required = 5031 / 330089 wR2 = 0.0941 before cycle 20 for 4674 data and 263 / 263 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0364 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72760 0.00100 -0.001 OSF 2 0.36164 0.12348 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for C4 Max. dU = 0.000 for C9 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 1.0439 1.1003 1.1277 43 0.950 0.000 C2 C3 C1 H3A 0.9671 1.2755 1.1430 43 0.950 0.000 C3 C4 C2 H4A 0.8330 1.3507 1.0424 43 0.950 0.000 C4 C3 C5 H5A 0.7639 1.2486 0.9322 43 0.950 0.000 C5 C4 C6 H7A 0.6285 1.0372 0.9313 33 0.980 0.000 C7 N1 H7A H7B 0.7190 0.9408 0.9645 33 0.980 0.000 C7 N1 H7A H7C 0.6707 0.9415 0.8716 33 0.980 0.000 C7 N1 H7A H8A 0.8737 1.1564 0.8094 23 0.990 0.000 C8 N1 C9 H8B 0.7160 1.1508 0.8248 23 0.990 0.000 C8 N1 C9 H9A 0.7056 0.9857 0.7526 23 0.990 0.000 C9 O1 C8 H9B 0.7658 1.0785 0.6956 23 0.990 0.000 C9 O1 C8 H10A 0.9853 0.8756 0.6535 23 0.990 0.000 C10 O1 C11 H10B 0.8357 0.9103 0.6311 23 0.990 0.000 C10 O1 C11 H11A 0.7503 0.7960 0.7327 23 0.990 0.000 C11 O2 C10 H11B 0.8450 0.7274 0.6732 23 0.990 0.000 C11 O2 C10 H12A 0.8969 0.6036 0.7962 23 0.990 0.000 C12 O2 C13 H12B 0.7849 0.6777 0.8378 23 0.990 0.000 C12 O2 C13 H13A 0.9284 0.6045 0.9371 23 0.990 0.000 C13 O3 C12 H13B 1.0533 0.6625 0.8940 23 0.990 0.000 C13 O3 C12 H14A 1.0807 0.7577 1.0233 23 0.990 0.000 C14 O3 C15 H14B 0.9435 0.7140 1.0618 23 0.990 0.000 C14 O3 C15 H15A 0.8560 0.8902 1.0628 23 0.990 0.000 C15 N2 C14 H15B 0.9906 0.8854 1.1154 23 0.990 0.000 C15 N2 C14 H16A 1.1753 0.9885 1.0790 33 0.980 0.000 C16 N2 H16A H16B 1.1980 1.0219 0.9859 33 0.980 0.000 C16 N2 H16A H16C 1.1971 0.8979 1.0113 33 0.980 0.000 C16 N2 H16A jsib001 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Na 0.99740 0.91143 0.86055 1.00000 0.02425 0.02873 0.02447 0.00011 -0.00076 -0.00328 0.02582 0.00170 0.00010 0.00008 0.00006 0.00000 0.00054 0.00056 0.00058 0.00050 0.00046 0.00049 0.00025 O1 0.90225 0.97411 0.73510 1.00000 0.03261 0.04473 0.02789 0.00068 -0.00905 -0.00367 0.03508 0.00322 0.00018 0.00016 0.00012 0.00000 0.00107 0.00131 0.00115 0.00101 0.00091 0.00099 0.00051 O2 0.92805 0.76122 0.78047 1.00000 0.03883 0.03981 0.02837 -0.00351 -0.00790 -0.00708 0.03567 0.00326 0.00020 0.00016 0.00012 0.00000 0.00115 0.00125 0.00118 0.00096 0.00097 0.00101 0.00051 O3 0.92587 0.76422 0.94691 1.00000 0.03665 0.02148 0.03386 -0.00424 0.00103 -0.00120 0.03066 0.00322 0.00019 0.00014 0.00012 0.00000 0.00114 0.00102 0.00121 0.00090 0.00096 0.00094 0.00048 P1 1.31203 0.92835 0.80205 1.00000 0.02386 0.03153 0.02524 0.00686 0.00116 0.00040 0.02688 0.00133 0.00007 0.00006 0.00004 0.00000 0.00035 0.00040 0.00038 0.00033 0.00031 0.00032 0.00017 F1 1.42764 0.84547 0.78119 1.00000 0.04084 0.04204 0.03785 0.00249 0.00706 0.01246 0.04025 0.00305 0.00017 0.00014 0.00010 0.00000 0.00101 0.00106 0.00109 0.00084 0.00086 0.00086 0.00046 F2 1.38417 0.95879 0.88543 1.00000 0.02668 0.03471 0.03232 0.00502 -0.00574 -0.00189 0.03124 0.00256 0.00014 0.00012 0.00009 0.00000 0.00083 0.00096 0.00094 0.00076 0.00072 0.00073 0.00040 F3 1.38962 1.02245 0.75658 1.00000 0.03657 0.04110 0.04260 0.01841 0.01167 -0.00279 0.04009 0.00303 0.00016 0.00014 0.00010 0.00000 0.00091 0.00105 0.00108 0.00087 0.00081 0.00081 0.00045 F4 1.19186 1.01029 0.82487 1.00000 0.02714 0.03433 0.03490 0.00868 0.00211 0.00422 0.03212 0.00277 0.00015 0.00013 0.00009 0.00000 0.00082 0.00091 0.00095 0.00075 0.00075 0.00075 0.00040 F5 1.23660 0.89877 0.71938 1.00000 0.04438 0.05723 0.02566 0.00274 -0.00661 -0.00261 0.04243 0.00289 0.00017 0.00015 0.00010 0.00000 0.00098 0.00119 0.00097 0.00085 0.00081 0.00092 0.00046 F6 1.22962 0.83495 0.84859 1.00000 0.03370 0.02648 0.03494 0.00688 0.00107 -0.00557 0.03171 0.00273 0.00016 0.00012 0.00010 0.00000 0.00094 0.00085 0.00099 0.00076 0.00076 0.00075 0.00041 N1 0.82102 1.04613 0.89410 1.00000 0.02316 0.03425 0.02804 0.00305 -0.00706 -0.00016 0.02848 0.00376 0.00021 0.00018 0.00014 0.00000 0.00116 0.00138 0.00131 0.00107 0.00105 0.00109 0.00055 N2 1.01261 0.96409 1.00820 1.00000 0.02231 0.02110 0.02233 0.00311 0.00055 0.00050 0.02191 0.00365 0.00020 0.00017 0.00013 0.00000 0.00111 0.00118 0.00121 0.00096 0.00096 0.00097 0.00049 C1 0.95277 1.06903 1.01999 1.00000 0.01979 0.02662 0.02432 0.00123 0.00348 -0.00143 0.02358 0.00458 0.00024 0.00022 0.00016 0.00000 0.00129 0.00149 0.00152 0.00128 0.00112 0.00116 0.00060 C2 0.98764 1.13048 1.08718 1.00000 0.02600 0.03208 0.03310 -0.00368 0.00031 -0.00023 0.03040 0.00489 0.00028 0.00022 0.00019 0.00000 0.00149 0.00163 0.00176 0.00136 0.00134 0.00128 0.00068 H2A 1.04388 1.10026 1.12774 1.00000 0.03648 0.00000 0.00000 C3 0.94250 1.23468 1.09652 1.00000 0.02886 0.03720 0.04415 -0.01203 0.00481 -0.00051 0.03674 0.00541 0.00030 0.00024 0.00020 0.00000 0.00160 0.00178 0.00200 0.00159 0.00145 0.00144 0.00075 H3A 0.96711 1.27548 1.14303 1.00000 0.04408 0.00000 0.00000 C4 0.86167 1.27830 1.03767 1.00000 0.04400 0.02714 0.06307 -0.00821 0.00078 0.01025 0.04474 0.00586 0.00032 0.00026 0.00021 0.00000 0.00197 0.00173 0.00252 0.00171 0.00183 0.00150 0.00090 H4A 0.83300 1.35070 1.04241 1.00000 0.05369 0.00000 0.00000 C5 0.82175 1.21774 0.97165 1.00000 0.03819 0.03300 0.05232 0.00297 -0.00927 0.01364 0.04117 0.00567 0.00032 0.00024 0.00020 0.00000 0.00177 0.00179 0.00219 0.00157 0.00166 0.00152 0.00082 H5A 0.76387 1.24862 0.93224 1.00000 0.04941 0.00000 0.00000 C6 0.86513 1.11110 0.96155 1.00000 0.02222 0.02784 0.03247 0.00052 -0.00117 -0.00026 0.02751 0.00484 0.00026 0.00022 0.00017 0.00000 0.00140 0.00157 0.00171 0.00134 0.00125 0.00116 0.00066 C7 0.69960 0.98639 0.91734 1.00000 0.03144 0.05647 0.03712 -0.00191 -0.00134 -0.01221 0.04168 0.00520 0.00029 0.00026 0.00019 0.00000 0.00161 0.00216 0.00189 0.00168 0.00149 0.00162 0.00081 H7A 0.62846 1.03716 0.93134 1.00000 0.06252 0.00000 0.00000 H7B 0.71904 0.94080 0.96450 1.00000 0.06252 0.00000 0.00000 H7C 0.67065 0.94152 0.87162 1.00000 0.06252 0.00000 0.00000 C8 0.79783 1.10691 0.81855 1.00000 0.03340 0.04062 0.03880 0.00879 -0.00615 0.00707 0.03761 0.00533 0.00030 0.00025 0.00018 0.00000 0.00166 0.00184 0.00190 0.00147 0.00144 0.00144 0.00076 H8A 0.87374 1.15639 0.80943 1.00000 0.04513 0.00000 0.00000 H8B 0.71604 1.15080 0.82481 1.00000 0.04513 0.00000 0.00000 C9 0.78245 1.03465 0.74483 1.00000 0.03443 0.06225 0.03168 0.01177 -0.01380 0.00499 0.04279 0.00547 0.00029 0.00028 0.00019 0.00000 0.00169 0.00233 0.00181 0.00164 0.00143 0.00161 0.00085 H9A 0.70561 0.98570 0.75262 1.00000 0.05135 0.00000 0.00000 H9B 0.76582 1.07847 0.69558 1.00000 0.05135 0.00000 0.00000 C10 0.89523 0.88855 0.67632 1.00000 0.05212 0.05491 0.02558 -0.00194 -0.00755 -0.00899 0.04420 0.00541 0.00035 0.00026 0.00019 0.00000 0.00208 0.00225 0.00179 0.00156 0.00151 0.00179 0.00088 H10A 0.98534 0.87561 0.65348 1.00000 0.05304 0.00000 0.00000 H10B 0.83574 0.91026 0.63107 1.00000 0.05304 0.00000 0.00000 C11 0.84337 0.78618 0.71375 1.00000 0.04887 0.05183 0.03743 -0.01045 -0.01331 -0.00914 0.04604 0.00541 0.00034 0.00028 0.00020 0.00000 0.00209 0.00215 0.00196 0.00165 0.00165 0.00172 0.00089 H11A 0.75028 0.79605 0.73268 1.00000 0.05525 0.00000 0.00000 H11B 0.84496 0.72737 0.67325 1.00000 0.05525 0.00000 0.00000 C12 0.88181 0.67078 0.82702 1.00000 0.04219 0.02562 0.04447 -0.00445 -0.00140 -0.01163 0.03743 0.00505 0.00032 0.00024 0.00019 0.00000 0.00183 0.00167 0.00201 0.00147 0.00156 0.00145 0.00078 H12A 0.89686 0.60361 0.79617 1.00000 0.04491 0.00000 0.00000 H12B 0.78489 0.67775 0.83781 1.00000 0.04491 0.00000 0.00000 C13 0.95606 0.66752 0.90450 1.00000 0.03544 0.02441 0.04219 -0.00670 0.00802 -0.00610 0.03401 0.00494 0.00030 0.00022 0.00018 0.00000 0.00169 0.00159 0.00195 0.00146 0.00147 0.00134 0.00074 H13A 0.92836 0.60452 0.93710 1.00000 0.04082 0.00000 0.00000 H13B 1.05326 0.66245 0.89404 1.00000 0.04082 0.00000 0.00000 C14 0.98303 0.76968 1.02620 1.00000 0.05174 0.02293 0.02874 0.00609 0.00387 -0.00657 0.03447 0.00516 0.00034 0.00022 0.00018 0.00000 0.00194 0.00157 0.00178 0.00130 0.00150 0.00147 0.00074 H14A 1.08070 0.75772 1.02332 1.00000 0.04137 0.00000 0.00000 H14B 0.94349 0.71398 1.06179 1.00000 0.04137 0.00000 0.00000 C15 0.95389 0.87967 1.05961 1.00000 0.03544 0.02853 0.02362 0.00311 0.00663 -0.00314 0.02920 0.00505 0.00030 0.00021 0.00017 0.00000 0.00161 0.00159 0.00161 0.00123 0.00130 0.00131 0.00068 H15A 0.85599 0.89016 1.06281 1.00000 0.03504 0.00000 0.00000 H15B 0.99059 0.88541 1.11542 1.00000 0.03504 0.00000 0.00000 C16 1.15791 0.96846 1.02227 1.00000 0.02533 0.03683 0.03112 -0.00295 -0.00121 0.00745 0.03110 0.00478 0.00025 0.00024 0.00017 0.00000 0.00145 0.00173 0.00167 0.00143 0.00126 0.00131 0.00069 H16A 1.17527 0.98854 1.07898 1.00000 0.04664 0.00000 0.00000 H16B 1.19796 1.02186 0.98590 1.00000 0.04664 0.00000 0.00000 H16C 1.19714 0.89789 1.01127 1.00000 0.04664 0.00000 0.00000 Final Structure Factor Calculation for jsib001 in P2(1)2(1)2(1) Total number of l.s. parameters = 263 Maximum vector length = 511 Memory required = 4770 / 28112 wR2 = 0.0941 before cycle 21 for 4674 data and 2 / 263 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0364 * P )^2 + 0.01 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0471 for 3502 Fo > 4sig(Fo) and 0.0718 for all 4674 data wR2 = 0.0941, GooF = S = 1.025, Restrained GooF = 1.025 for all data Occupancy sum of asymmetric unit = 29.00 for non-hydrogen and 26.00 for hydrogen atoms Principal mean square atomic displacements U 0.0305 0.0246 0.0223 Na 0.0465 0.0380 0.0208 O1 0.0470 0.0383 0.0217 O2 0.0375 0.0344 0.0201 O3 0.0360 0.0240 0.0207 P1 0.0564 0.0367 0.0276 F1 0.0406 0.0301 0.0230 F2 0.0621 0.0404 0.0177 F3 0.0445 0.0275 0.0244 F4 0.0583 0.0456 0.0235 F5 0.0396 0.0351 0.0204 F6 0.0364 0.0311 0.0180 N1 0.0251 0.0221 0.0185 N2 0.0272 0.0260 0.0175 C1 0.0363 0.0289 0.0260 C2 0.0539 0.0306 0.0257 C3 0.0650 0.0484 0.0209 C4 0.0576 0.0463 0.0196 C5 0.0327 0.0278 0.0221 C6 0.0615 0.0374 0.0261 C7 0.0487 0.0414 0.0227 C8 0.0663 0.0461 0.0160 C9 0.0629 0.0467 0.0230 C10 0.0597 0.0562 0.0222 C11 0.0484 0.0451 0.0188 C12 0.0506 0.0303 0.0212 C13 0.0534 0.0326 0.0174 C14 0.0387 0.0300 0.0189 C15 0.0415 0.0301 0.0217 C16 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.029 0.042 0.056 0.069 0.084 0.102 0.127 0.168 0.238 1.000 Number in group 499. 443. 504. 445. 460. 460. 461. 465. 467. 470. GooF 0.846 0.979 0.989 0.973 1.082 1.132 1.103 1.109 1.116 0.893 K 1.404 1.141 1.073 1.038 1.060 1.053 1.033 1.019 0.993 0.998 Resolution(A) 0.75 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.66 inf Number in group 467. 478. 462. 464. 472. 466. 463. 473. 461. 468. GooF 1.083 0.996 0.935 0.945 0.946 0.959 0.967 1.004 1.085 1.284 K 1.197 1.136 1.065 1.023 1.030 1.004 0.982 0.986 0.992 1.007 R1 0.224 0.176 0.168 0.149 0.088 0.060 0.047 0.037 0.027 0.020 Recommended weighting scheme: WGHT 0.0300 0.1628 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 0 5 2 511.81 396.38 4.90 0.147 2.39 -3 1 3 697.22 846.48 4.35 0.215 2.78 2 0 16 248.81 3.89 4.10 0.015 1.01 1 6 5 150.02 113.38 3.97 0.079 1.73 0 5 3 894.11 756.53 3.78 0.204 2.27 0 3 3 568.73 669.47 3.74 0.191 3.31 0 4 9 35.17 70.34 3.71 0.062 1.57 3 3 1 506.02 604.25 3.61 0.182 2.57 0 6 2 1249.85 1068.39 3.51 0.242 2.01 -8 3 3 352.94 467.94 3.50 0.160 1.17 0 6 9 827.53 992.45 3.34 0.233 1.37 -2 15 5 274.14 156.46 3.29 0.093 0.80 3 1 3 728.53 843.22 3.28 0.215 2.78 4 8 5 232.23 160.93 3.28 0.094 1.23 -3 6 2 429.70 361.16 3.22 0.141 1.72 -4 9 17 327.09 108.55 3.18 0.077 0.76 5 0 2 56.39 33.52 3.16 0.043 1.94 3 3 6 335.80 280.45 3.15 0.124 1.89 -7 2 4 509.93 648.71 3.15 0.188 1.32 -4 7 14 83.19 29.84 3.14 0.040 0.91 -1 12 1 109.28 168.44 3.05 0.096 1.03 7 1 3 134.63 94.65 3.04 0.072 1.38 4 2 2 310.55 257.33 3.04 0.119 2.23 0 0 10 178.82 120.38 2.94 0.081 1.64 1 0 9 39.21 57.52 2.92 0.056 1.80 11 6 4 114.32 48.22 2.91 0.051 0.82 5 1 9 216.18 168.65 2.90 0.096 1.34 0 5 1 480.57 415.85 2.88 0.151 2.46 11 6 3 422.58 310.97 2.83 0.130 0.82 8 6 5 85.25 124.21 2.80 0.082 1.02 -5 11 1 237.14 162.70 2.80 0.094 0.98 12 5 1 244.71 153.53 2.79 0.092 0.79 -5 4 5 257.77 186.07 2.78 0.101 1.50 -2 9 18 454.87 217.91 2.76 0.109 0.75 -1 9 17 77.60 24.03 2.76 0.036 0.79 -4 7 18 135.10 51.94 2.76 0.053 0.77 2 0 10 316.90 264.93 2.74 0.120 1.56 1 3 7 331.36 286.04 2.74 0.125 2.00 1 7 6 146.22 194.54 2.73 0.103 1.48 -4 14 5 230.55 150.84 2.73 0.091 0.81 -1 6 15 100.74 58.37 2.73 0.057 0.96 2 0 4 93.12 114.79 2.72 0.079 3.17 -7 1 2 190.16 248.21 2.71 0.117 1.40 -4 10 12 385.11 281.31 2.70 0.124 0.86 -11 6 3 418.55 311.56 2.70 0.131 0.82 3 1 0 173.54 145.69 2.70 0.089 3.22 -11 4 10 574.77 402.19 2.67 0.148 0.77 11 0 1 -9.58 29.28 2.67 0.040 0.91 -11 4 9 165.93 81.14 2.66 0.067 0.79 -1 11 14 109.82 53.06 2.66 0.054 0.81 Bond lengths and angles Na - Distance Angles F4 2.3770 (0.0020) O2 2.3908 (0.0023) 120.53 (0.08) O1 2.4004 (0.0023) 86.83 (0.07) 70.58 (0.08) O3 2.4270 (0.0022) 141.03 (0.07) 69.14 (0.08) 129.09 (0.08) N1 2.4978 (0.0026) 106.55 (0.08) 116.26 (0.08) 71.95 (0.08) 99.82 (0.08) N2 2.5168 (0.0025) 93.03 (0.07) 138.74 (0.08) 140.00 (0.09) 69.63 (0.07) 69.81 (0.07) F6 2.5199 (0.0021) 54.66 (0.06) 85.91 (0.07) 114.97 (0.07) 91.82 (0.07) 157.43 (0.08) 96.77 (0.07) P1 3.2994 (0.0017) 27.56 (0.04) 99.61 (0.06) 96.20 (0.06) 120.00 (0.06) 134.11 (0.07) 101.90 (0.06) 28.48 (0.04) Na - F4 O2 O1 O3 N1 N2 F6 O1 - Distance Angles C9 1.4258 (0.0034) C10 1.4402 (0.0035) 115.21 (0.23) Na 2.4004 (0.0023) 114.19 (0.16) 110.72 (0.17) O1 - C9 C10 O2 - Distance Angles C11 1.4198 (0.0036) C12 1.4385 (0.0035) 112.93 (0.23) Na 2.3908 (0.0022) 115.23 (0.18) 114.50 (0.16) O2 - C11 C12 O3 - Distance Angles C14 1.4239 (0.0033) C13 1.4244 (0.0031) 113.72 (0.22) Na 2.4270 (0.0022) 112.32 (0.16) 106.94 (0.16) O3 - C14 C13 P1 - Distance Angles F1 1.5885 (0.0018) F3 1.5926 (0.0017) 91.29 (0.10) F2 1.5940 (0.0017) 90.57 (0.09) 90.38 (0.09) F5 1.5966 (0.0018) 90.63 (0.10) 90.11 (0.10) 178.69 (0.10) F6 1.6186 (0.0017) 90.31 (0.10) 178.38 (0.10) 89.79 (0.09) 89.69 (0.10) F4 1.6219 (0.0017) 178.34 (0.10) 90.36 (0.10) 89.29 (0.09) 89.49 (0.09) 88.03 (0.09) Na 3.2994 (0.0017) 135.77 (0.08) 130.47 (0.07) 101.39 (0.07) 77.38 (0.07) 47.94 (0.06) 42.69 (0.06) P1 - F1 F3 F2 F5 F6 F4 F1 - Distance Angles P1 1.5885 (0.0018) F1 - F2 - Distance Angles P1 1.5940 (0.0017) F2 - F3 - Distance Angles P1 1.5926 (0.0017) F3 - F4 - Distance Angles P1 1.6219 (0.0017) Na 2.3770 (0.0020) 109.75 (0.09) F4 - P1 F5 - Distance Angles P1 1.5966 (0.0018) F5 - F6 - Distance Angles P1 1.6186 (0.0017) Na 2.5199 (0.0021) 103.58 (0.08) F6 - P1 N1 - Distance Angles C6 1.4415 (0.0034) C8 1.4723 (0.0035) 114.01 (0.22) C7 1.4755 (0.0033) 109.70 (0.22) 110.35 (0.22) Na 2.4978 (0.0025) 109.31 (0.15) 105.74 (0.17) 107.47 (0.17) N1 - C6 C8 C7 N2 - Distance Angles C1 1.4515 (0.0034) C15 1.4715 (0.0032) 113.76 (0.20) C16 1.4737 (0.0032) 110.68 (0.22) 109.31 (0.22) Na 2.5168 (0.0025) 109.79 (0.16) 110.01 (0.16) 102.73 (0.16) N2 - C1 C15 C16 C1 - Distance Angles C2 1.3878 (0.0037) C6 1.4020 (0.0036) 119.69 (0.26) N2 1.4515 (0.0034) 119.97 (0.23) 120.26 (0.24) C1 - C2 C6 C2 - Distance Angles C3 1.3836 (0.0039) C1 1.3878 (0.0037) 121.60 (0.29) H2A 0.9500 119.20 119.20 C2 - C3 C1 C3 - Distance Angles C4 1.3728 (0.0045) C2 1.3836 (0.0039) 119.09 (0.31) H3A 0.9500 120.46 120.46 C3 - C4 C2 C4 - Distance Angles C3 1.3728 (0.0045) C5 1.3802 (0.0041) 120.48 (0.29) H4A 0.9500 119.76 119.76 C4 - C3 C5 C5 - Distance Angles C4 1.3802 (0.0041) C6 1.4080 (0.0039) 121.29 (0.29) H5A 0.9500 119.35 119.35 C5 - C4 C6 C6 - Distance Angles C1 1.4020 (0.0036) C5 1.4080 (0.0039) 117.74 (0.28) N1 1.4415 (0.0034) 120.50 (0.24) 121.76 (0.26) C6 - C1 C5 C7 - Distance Angles N1 1.4755 (0.0033) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - N1 H7A H7B C8 - Distance Angles N1 1.4723 (0.0035) C9 1.5167 (0.0041) 112.53 (0.24) H8A 0.9900 109.09 109.09 H8B 0.9900 109.09 109.09 107.84 C8 - N1 C9 H8A C9 - Distance Angles O1 1.4258 (0.0034) C8 1.5167 (0.0041) 108.56 (0.23) H9A 0.9900 109.98 109.98 H9B 0.9900 109.98 109.98 108.36 C9 - O1 C8 H9A C10 - Distance Angles O1 1.4402 (0.0035) C11 1.5084 (0.0045) 111.70 (0.25) H10A 0.9900 109.28 109.28 H10B 0.9900 109.28 109.28 107.94 C10 - O1 C11 H10A C11 - Distance Angles O2 1.4198 (0.0036) C10 1.5084 (0.0045) 107.12 (0.26) H11A 0.9900 110.29 110.29 H11B 0.9900 110.29 110.29 108.55 C11 - O2 C10 H11A C12 - Distance Angles O2 1.4385 (0.0034) C13 1.4743 (0.0041) 108.54 (0.23) H12A 0.9900 109.98 109.98 H12B 0.9900 109.98 109.98 108.36 C12 - O2 C13 H12A C13 - Distance Angles O3 1.4244 (0.0031) C12 1.4743 (0.0041) 106.97 (0.25) H13A 0.9900 110.33 110.33 H13B 0.9900 110.33 110.33 108.57 C13 - O3 C12 H13A C14 - Distance Angles O3 1.4239 (0.0033) C15 1.5052 (0.0038) 107.40 (0.24) H14A 0.9900 110.23 110.23 H14B 0.9900 110.23 110.23 108.51 C14 - O3 C15 H14A C15 - Distance Angles N2 1.4715 (0.0032) C14 1.5052 (0.0038) 111.38 (0.22) H15A 0.9900 109.35 109.35 H15B 0.9900 109.35 109.35 107.99 C15 - N2 C14 H15A C16 - Distance Angles N2 1.4737 (0.0032) H16A 0.9800 109.47 H16B 0.9800 109.47 109.47 H16C 0.9800 109.47 109.47 109.47 C16 - N2 H16A H16B Selected torsion angles -120.68 ( 0.19) F4 - Na - O1 - C9 115.33 ( 0.19) O2 - Na - O1 - C9 75.95 ( 0.21) O3 - Na - O1 - C9 -12.13 ( 0.18) N1 - Na - O1 - C9 -29.75 ( 0.24) N2 - Na - O1 - C9 -169.00 ( 0.18) F6 - Na - O1 - C9 -146.63 ( 0.18) P1 - Na - O1 - C9 107.32 ( 0.19) F4 - Na - O1 - C10 -16.67 ( 0.18) O2 - Na - O1 - C10 -56.05 ( 0.22) O3 - Na - O1 - C10 -144.13 ( 0.20) N1 - Na - O1 - C10 -161.75 ( 0.18) N2 - Na - O1 - C10 59.00 ( 0.20) F6 - Na - O1 - C10 81.37 ( 0.18) P1 - Na - O1 - C10 -87.68 ( 0.20) F4 - Na - O2 - C11 -13.71 ( 0.19) O1 - Na - O2 - C11 134.48 ( 0.20) O3 - Na - O2 - C11 43.59 ( 0.21) N1 - Na - O2 - C11 132.38 ( 0.20) N2 - Na - O2 - C11 -132.00 ( 0.20) F6 - Na - O2 - C11 -106.94 ( 0.19) P1 - Na - O2 - C11 138.83 ( 0.18) F4 - Na - O2 - C12 -147.20 ( 0.20) O1 - Na - O2 - C12 1.00 ( 0.18) O3 - Na - O2 - C12 -89.90 ( 0.20) N1 - Na - O2 - C12 -1.11 ( 0.24) N2 - Na - O2 - C12 94.51 ( 0.19) F6 - Na - O2 - C12 119.57 ( 0.18) P1 - Na - O2 - C12 43.27 ( 0.22) F4 - Na - O3 - C14 156.43 ( 0.19) O2 - Na - O3 - C14 -163.75 ( 0.17) O1 - Na - O3 - C14 -89.08 ( 0.18) N1 - Na - O3 - C14 -25.05 ( 0.17) N2 - Na - O3 - C14 71.50 ( 0.18) F6 - Na - O3 - C14 67.22 ( 0.18) P1 - Na - O3 - C14 -82.15 ( 0.20) F4 - Na - O3 - C13 31.01 ( 0.17) O2 - Na - O3 - C13 70.83 ( 0.20) O1 - Na - O3 - C13 145.50 ( 0.17) N1 - Na - O3 - C13 -150.47 ( 0.18) N2 - Na - O3 - C13 -53.92 ( 0.17) F6 - Na - O3 - C13 -58.20 ( 0.18) P1 - Na - O3 - C13 179.09 ( 0.14) F4 - Na - P1 - F1 -38.80 ( 0.12) O2 - Na - P1 - F1 -110.09 ( 0.11) O1 - Na - P1 - F1 32.58 ( 0.13) O3 - Na - P1 - F1 179.10 ( 0.12) N1 - Na - P1 - F1 105.77 ( 0.12) N2 - Na - P1 - F1 23.57 ( 0.12) F6 - Na - P1 - F1 -24.12 ( 0.12) F4 - Na - P1 - F3 117.98 ( 0.11) O2 - Na - P1 - F3 46.69 ( 0.11) O1 - Na - P1 - F3 -170.64 ( 0.11) O3 - Na - P1 - F3 -24.11 ( 0.14) N1 - Na - P1 - F3 -97.44 ( 0.11) N2 - Na - P1 - F3 -179.64 ( 0.13) F6 - Na - P1 - F3 76.29 ( 0.10) F4 - Na - P1 - F2 -141.60 ( 0.09) O2 - Na - P1 - F2 147.11 ( 0.09) O1 - Na - P1 - F2 -70.22 ( 0.09) O3 - Na - P1 - F2 76.30 ( 0.11) N1 - Na - P1 - F2 2.97 ( 0.09) N2 - Na - P1 - F2 -79.23 ( 0.11) F6 - Na - P1 - F2 -103.26 ( 0.11) F4 - Na - P1 - F5 38.85 ( 0.09) O2 - Na - P1 - F5 -32.44 ( 0.09) O1 - Na - P1 - F5 110.23 ( 0.10) O3 - Na - P1 - F5 -103.25 ( 0.11) N1 - Na - P1 - F5 -176.58 ( 0.09) N2 - Na - P1 - F5 101.22 ( 0.11) F6 - Na - P1 - F5 155.52 ( 0.12) F4 - Na - P1 - F6 -62.37 ( 0.10) O2 - Na - P1 - F6 -133.66 ( 0.10) O1 - Na - P1 - F6 9.01 ( 0.10) O3 - Na - P1 - F6 155.53 ( 0.12) N1 - Na - P1 - F6 82.20 ( 0.10) N2 - Na - P1 - F6 142.11 ( 0.11) O2 - Na - P1 - F4 70.82 ( 0.10) O1 - Na - P1 - F4 -146.51 ( 0.10) O3 - Na - P1 - F4 0.01 ( 0.12) N1 - Na - P1 - F4 -73.32 ( 0.10) N2 - Na - P1 - F4 -155.52 ( 0.12) F6 - Na - P1 - F4 -22.54 ( 3.60) F1 - P1 - F4 - Na 161.89 ( 0.09) F3 - P1 - F4 - Na -107.74 ( 0.09) F2 - P1 - F4 - Na 71.78 ( 0.09) F5 - P1 - F4 - Na -17.93 ( 0.09) F6 - P1 - F4 - Na -44.67 ( 0.12) O2 - Na - F4 - P1 -109.88 ( 0.09) O1 - Na - F4 - P1 49.44 ( 0.14) O3 - Na - F4 - P1 -179.99 ( 0.09) N1 - Na - F4 - P1 110.18 ( 0.09) N2 - Na - F4 - P1 14.02 ( 0.07) F6 - Na - F4 - P1 -163.81 ( 0.09) F1 - P1 - F6 - Na 9.63 ( 3.67) F3 - P1 - F6 - Na 105.62 ( 0.09) F2 - P1 - F6 - Na -73.18 ( 0.09) F5 - P1 - F6 - Na 16.33 ( 0.08) F4 - P1 - F6 - Na -13.59 ( 0.07) F4 - Na - F6 - P1 118.87 ( 0.09) O2 - Na - F6 - P1 52.50 ( 0.11) O1 - Na - F6 - P1 -172.20 ( 0.09) O3 - Na - F6 - P1 -50.80 ( 0.22) N1 - Na - F6 - P1 -102.50 ( 0.09) N2 - Na - F6 - P1 -60.41 ( 0.17) F4 - Na - N1 - C6 162.07 ( 0.16) O2 - Na - N1 - C6 -141.34 ( 0.18) O1 - Na - N1 - C6 90.59 ( 0.17) O3 - Na - N1 - C6 26.70 ( 0.16) N2 - Na - N1 - C6 -29.44 ( 0.29) F6 - Na - N1 - C6 -60.41 ( 0.19) P1 - Na - N1 - C6 62.73 ( 0.18) F4 - Na - N1 - C8 -74.79 ( 0.18) O2 - Na - N1 - C8 -18.20 ( 0.16) O1 - Na - N1 - C8 -146.27 ( 0.17) O3 - Na - N1 - C8 149.84 ( 0.19) N2 - Na - N1 - C8 93.70 ( 0.24) F6 - Na - N1 - C8 62.73 ( 0.19) P1 - Na - N1 - C8 -179.39 ( 0.16) F4 - Na - N1 - C7 43.08 ( 0.19) O2 - Na - N1 - C7 99.67 ( 0.18) O1 - Na - N1 - C7 -28.40 ( 0.18) O3 - Na - N1 - C7 -92.29 ( 0.18) N2 - Na - N1 - C7 -148.43 ( 0.20) F6 - Na - N1 - C7 -179.40 ( 0.14) P1 - Na - N1 - C7 83.02 ( 0.16) F4 - Na - N2 - C1 -130.70 ( 0.17) O2 - Na - N2 - C1 -5.65 ( 0.22) O1 - Na - N2 - C1 -132.80 ( 0.17) O3 - Na - N2 - C1 -23.50 ( 0.15) N1 - Na - N2 - C1 137.78 ( 0.15) F6 - Na - N2 - C1 109.37 ( 0.15) P1 - Na - N2 - C1 -151.05 ( 0.16) F4 - Na - N2 - C15 -4.77 ( 0.23) O2 - Na - N2 - C15 120.28 ( 0.18) O1 - Na - N2 - C15 -6.87 ( 0.16) O3 - Na - N2 - C15 102.42 ( 0.18) N1 - Na - N2 - C15 -96.30 ( 0.17) F6 - Na - N2 - C15 -124.71 ( 0.16) P1 - Na - N2 - C15 -34.75 ( 0.17) F4 - Na - N2 - C16 111.53 ( 0.19) O2 - Na - N2 - C16 -123.42 ( 0.18) O1 - Na - N2 - C16 109.43 ( 0.18) O3 - Na - N2 - C16 -141.27 ( 0.18) N1 - Na - N2 - C16 20.01 ( 0.17) F6 - Na - N2 - C16 -8.40 ( 0.17) P1 - Na - N2 - C16 78.18 ( 0.30) C15 - N2 - C1 - C2 -45.35 ( 0.32) C16 - N2 - C1 - C2 -158.06 ( 0.20) Na - N2 - C1 - C2 -105.20 ( 0.29) C15 - N2 - C1 - C6 131.27 ( 0.26) C16 - N2 - C1 - C6 18.56 ( 0.28) Na - N2 - C1 - C6 -2.80 ( 0.41) C6 - C1 - C2 - C3 173.84 ( 0.25) N2 - C1 - C2 - C3 -0.25 ( 0.44) C1 - C2 - C3 - C4 2.48 ( 0.47) C2 - C3 - C4 - C5 -1.67 ( 0.50) C3 - C4 - C5 - C6 3.51 ( 0.40) C2 - C1 - C6 - C5 -173.12 ( 0.25) N2 - C1 - C6 - C5 -176.02 ( 0.23) C2 - C1 - C6 - N1 7.35 ( 0.38) N2 - C1 - C6 - N1 -1.35 ( 0.46) C4 - C5 - C6 - C1 178.18 ( 0.27) C4 - C5 - C6 - N1 -147.19 ( 0.26) C8 - N1 - C6 - C1 88.48 ( 0.29) C7 - N1 - C6 - C1 -29.11 ( 0.29) Na - N1 - C6 - C1 33.29 ( 0.37) C8 - N1 - C6 - C5 -91.04 ( 0.32) C7 - N1 - C6 - C5 151.37 ( 0.24) Na - N1 - C6 - C5 167.01 ( 0.23) C6 - N1 - C8 - C9 -69.02 ( 0.31) C7 - N1 - C8 - C9 46.91 ( 0.27) Na - N1 - C8 - C9 169.79 ( 0.24) C10 - O1 - C9 - C8 39.99 ( 0.28) Na - O1 - C9 - C8 -60.41 ( 0.33) N1 - C8 - C9 - O1 -86.93 ( 0.32) C9 - O1 - C10 - C11 44.54 ( 0.31) Na - O1 - C10 - C11 174.07 ( 0.25) C12 - O2 - C11 - C10 39.87 ( 0.30) Na - O2 - C11 - C10 -56.26 ( 0.35) O1 - C10 - C11 - O2 -166.56 ( 0.25) C11 - O2 - C12 - C13 -32.01 ( 0.29) Na - O2 - C12 - C13 175.72 ( 0.24) C14 - O3 - C13 - C12 -59.71 ( 0.24) Na - O3 - C13 - C12 61.85 ( 0.30) O2 - C12 - C13 - O3 174.58 ( 0.22) C13 - O3 - C14 - C15 52.95 ( 0.26) Na - O3 - C14 - C15 160.30 ( 0.24) C1 - N2 - C15 - C14 -75.43 ( 0.30) C16 - N2 - C15 - C14 36.66 ( 0.28) Na - N2 - C15 - C14 -60.38 ( 0.31) O3 - C14 - C15 - N2 FMAP and GRID set by program FMAP 2 3 21 GRID -1.389 -2 -2 1.389 2 2 R1 = 0.0628 for 2718 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.24 at 0.4944 0.5787 0.0299 [ 0.84 A from N2 ] Deepest hole -0.26 at 0.8154 0.5229 0.1916 [ 0.62 A from P1 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 4711 / 22998 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9944 0.9213 0.9701 1.00000 0.05 0.24 0.84 N2 1.61 C15 1.80 NA 1.94 C16 Q2 1 0.7149 0.9181 0.8847 1.00000 0.05 0.22 0.57 H7C 1.02 C7 1.34 H7B 1.88 H7A Q3 1 1.0008 0.7971 0.7433 1.00000 0.05 0.21 1.05 O2 1.65 C11 1.78 H10A 1.90 C10 Q4 1 0.7272 0.9692 0.9842 1.00000 0.05 0.21 0.49 H7B 1.15 C7 1.56 H7A 1.96 H7C Q5 1 0.9135 0.9045 1.1347 1.00000 0.05 0.21 0.87 H15B 1.33 H15A 1.33 C15 2.07 H9B Q6 1 0.9232 1.0916 0.9844 1.00000 0.05 0.21 0.71 C1 0.73 C6 1.86 N2 1.87 C2 Q7 1 0.8228 1.0631 0.8526 1.00000 0.05 0.20 0.71 N1 0.82 C8 1.45 H8A 1.60 H8B Q8 1 1.4854 0.8979 0.7817 1.00000 0.05 0.20 0.87 F1 1.81 P1 1.87 F3 2.12 F2 Q9 1 1.1101 0.8490 0.7198 1.00000 0.05 0.19 1.41 F5 1.69 H10A 2.32 C10 2.35 O2 Q10 1 0.9156 0.7484 1.0003 1.00000 0.05 0.19 0.84 C14 0.90 O3 1.13 H14B 1.70 H14A Q11 1 0.8806 0.8951 0.9384 1.00000 0.05 0.19 1.70 O3 1.74 NA 1.77 H7B 1.95 N2 Q12 1 0.9462 0.9190 0.8037 1.00000 0.05 0.19 1.07 NA 1.39 O1 2.01 O2 2.19 C10 Q13 1 1.0558 0.8830 0.7586 1.00000 0.05 0.19 1.81 NA 1.87 H10A 1.93 F5 1.95 O1 Q14 1 0.8749 1.2364 1.0692 1.00000 0.05 0.18 0.75 C4 0.81 C3 1.55 H4A 1.60 H3A Q15 1 1.2599 0.9267 0.7458 1.00000 0.05 0.18 0.60 F5 1.06 P1 1.77 F3 1.80 F4 Q16 1 0.8753 0.7967 0.8930 1.00000 0.05 0.18 1.10 O3 1.81 C13 1.91 C12 1.95 NA Q17 1 1.2151 0.9621 0.7902 1.00000 0.05 0.18 0.86 F4 1.08 P1 1.42 F5 1.86 F6 Q18 1 0.6379 1.2598 1.0041 1.00000 0.05 0.18 1.73 H5A 1.99 C5 2.32 C4 2.34 H4A Q19 1 0.9751 0.8151 0.9241 1.00000 0.05 0.18 0.89 O3 1.61 NA 1.77 C14 1.88 C13 Q20 1 1.3885 0.9048 0.7616 1.00000 0.05 0.18 0.90 F1 1.06 P1 1.47 F3 1.67 F5 Shortest distances between peaks (including symmetry equivalents) 9 13 0.94 15 17 0.96 8 20 1.03 16 19 1.14 3 13 1.23 1 11 1.29 3 9 1.33 15 20 1.34 11 19 1.39 12 13 1.40 11 16 1.44 1 19 1.54 10 19 1.61 2 4 1.76 9 15 1.83 3 12 1.89 2 11 1.90 10 16 1.90 17 20 1.93 4 11 1.94 13 17 1.94 9 17 2.10 10 11 2.12 13 15 2.12 2 7 2.17 2 16 2.21 12 16 2.23 1 6 2.25 9 12 2.31 7 12 2.32 11 12 2.33 1 16 2.33 6 14 2.33 1 10 2.35 8 15 2.36 12 19 2.38 6 7 2.41 4 6 2.49 7 11 2.59 6 11 2.60 14 18 2.62 4 7 2.64 2 12 2.67 1 4 2.75 12 17 2.75 3 16 2.76 1 12 2.77 8 17 2.82 1 5 2.83 6 18 2.84 2 8 2.86 14 18 2.89 5 10 2.94 9 20 2.95 13 19 2.96 2 19 2.98 3 19 2.99 Time profile in seconds ----------------------- 0.00: 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. 0.09: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 3.38: Structure factors and derivatives 3.14: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.23: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + jsib001 finished at 14:06:30 Total CPU time: 7.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++