++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XL - CRYSTAL STRUCTURE REFINEMENT - SHELXTL Ver. 6.12 W95/98/NT/2000/ME + + Copyright(c) 2001 Bruker Analytical X-ray Solutions All Rights Reserved + + jain001 started at 12:59:26 on 16-Jan-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL jain001 in P2(1)2(1)2(1) CELL 0.71073 7.8876 13.4571 16.1920 90.000 90.000 90.000 ZERR 4.00 0.0030 0.0046 0.0072 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 O UNIT 84 112 8 V = 1718.69 F(000) = 680.0 Mu = 0.08 mm-1 Cell Wt = 1249.74 Rho = 1.207 L.S. 20 MERG 4 BOND $H HTAB FMAP 2 PLAN 20 OMIT 9 6 7 OMIT 9 5 7 TEMP -153 ACTA 50 CONF WPDB SIZE 0.192 0.155 0.052 WGHT 0.028300 1.052300 FVAR 0.84661 C1 1 0.90705 -0.13742 -0.03155 11.00000 0.02253 0.02871 = 0.02914 -0.00250 0.00248 -0.00119 AFIX 23 H1A 2 0.81175 -0.16168 -0.00067 11.00000 -1.20000 H1B 2 0.86500 -0.09128 -0.07186 11.00000 -1.20000 AFIX 0 C2 1 0.99032 -0.22487 -0.07651 11.00000 0.02852 0.02904 = 0.03350 -0.00754 -0.00061 -0.00453 AFIX 23 H2A 2 0.91224 -0.25143 -0.11627 11.00000 -1.20000 H2B 2 1.01565 -0.27634 -0.03736 11.00000 -1.20000 AFIX 0 C3 1 1.15070 -0.19429 -0.11971 11.00000 0.02889 0.03343 = 0.02579 -0.00242 -0.00164 0.00801 C4 1 1.24630 -0.11352 -0.08281 11.00000 0.02265 0.03311 = 0.02864 0.00244 0.00200 0.00025 AFIX 43 H4A 2 1.35135 -0.09462 -0.10830 11.00000 -1.20000 AFIX 0 C5 1 1.19669 -0.06360 -0.01513 11.00000 0.02509 0.02687 = 0.02193 0.00499 0.00073 0.00303 C6 1 1.31221 0.01163 0.02390 11.00000 0.02082 0.03653 = 0.02880 -0.00246 0.00170 -0.00183 AFIX 23 H6A 2 1.40599 0.02406 -0.01245 11.00000 -1.20000 H6B 2 1.35667 -0.01516 0.07440 11.00000 -1.20000 AFIX 0 C7 1 1.22295 0.10911 0.04227 11.00000 0.02669 0.03130 = 0.02866 -0.00052 -0.00051 -0.00714 AFIX 23 H7A 2 1.19132 0.14046 -0.00870 11.00000 -1.20000 H7B 2 1.29931 0.15272 0.07087 11.00000 -1.20000 AFIX 0 C8 1 1.06481 0.09263 0.09496 11.00000 0.02423 0.02785 = 0.02047 -0.00110 -0.00261 -0.00052 AFIX 13 H8A 2 1.09769 0.06477 0.14714 11.00000 -1.20000 AFIX 0 C9 1 0.94358 0.01991 0.05078 11.00000 0.02237 0.02747 = 0.02037 0.00113 -0.00222 0.00013 AFIX 13 H9A 2 0.91470 0.05098 -0.00071 11.00000 -1.20000 AFIX 0 C10 1 1.02703 -0.08194 0.02765 11.00000 0.02250 0.02400 = 0.02408 -0.00072 -0.00001 -0.00012 C11 1 0.77515 0.00702 0.09777 11.00000 0.02309 0.02815 = 0.03605 -0.00717 0.00237 -0.00313 AFIX 23 H11A 2 0.79662 -0.02886 0.14793 11.00000 -1.20000 H11B 2 0.69957 -0.03232 0.06473 11.00000 -1.20000 AFIX 0 C12 1 0.68723 0.10575 0.11927 11.00000 0.02316 0.03108 = 0.03207 -0.00504 0.00194 0.00189 AFIX 23 H12A 2 0.59007 0.09298 0.15337 11.00000 -1.20000 H12B 2 0.64896 0.13743 0.06953 11.00000 -1.20000 AFIX 0 C13 1 0.80962 0.17443 0.16483 11.00000 0.02957 0.02661 = 0.02396 -0.00163 -0.00005 0.00208 C14 1 0.96725 0.18865 0.10993 11.00000 0.02983 0.02643 = 0.02192 0.00167 -0.00485 -0.00004 AFIX 13 H14A 2 0.92569 0.20935 0.05693 11.00000 -1.20000 AFIX 0 C15 1 1.05663 0.27927 0.14695 11.00000 0.03728 0.02751 = 0.02995 0.00057 -0.00260 -0.00611 AFIX 23 H15A 2 1.12471 0.31267 0.10640 11.00000 -1.20000 H15B 2 1.12685 0.26079 0.19288 11.00000 -1.20000 AFIX 0 C16 1 0.90807 0.34405 0.17467 11.00000 0.04655 0.02856 = 0.01965 0.00259 -0.00659 0.00206 C17 1 0.75298 0.28139 0.17842 11.00000 0.04017 0.02929 = 0.02018 0.00223 -0.00396 0.00344 C18 1 0.85283 0.13163 0.25072 11.00000 0.04194 0.03244 = 0.02647 0.00216 0.00230 0.00738 AFIX 137 H18A 2 0.75062 0.12426 0.28232 11.00000 -1.50000 H18B 2 0.90623 0.06798 0.24438 11.00000 -1.50000 H18C 2 0.92853 0.17603 0.27890 11.00000 -1.50000 AFIX 0 C19 1 1.06146 -0.14601 0.10459 11.00000 0.02897 0.03063 = 0.02701 0.00239 0.00194 0.00175 AFIX 137 H19A 2 1.11247 -0.20767 0.08812 11.00000 -1.50000 H19B 2 1.13683 -0.11117 0.14104 11.00000 -1.50000 H19C 2 0.95654 -0.15914 0.13259 11.00000 -1.50000 AFIX 0 C20 1 0.59444 0.31140 0.19355 11.00000 0.04325 0.02979 = 0.03074 0.00141 0.00796 0.00397 AFIX 43 H20A 2 0.50902 0.26059 0.19294 11.00000 -1.20000 AFIX 0 C21 1 0.53424 0.41427 0.21125 11.00000 0.05106 0.03658 = 0.04231 0.00342 0.01397 0.00953 AFIX 137 H21A 2 0.41377 0.41357 0.21966 11.00000 -1.50000 H21B 2 0.58919 0.43878 0.26007 11.00000 -1.50000 H21D 2 0.56100 0.45669 0.16539 11.00000 -1.50000 AFIX 0 O1 3 1.20061 -0.23784 -0.18177 11.00000 0.03619 0.05367 = 0.03367 -0.01508 0.00467 0.00434 O2 3 0.92006 0.43234 0.19032 11.00000 0.05775 0.02437 = 0.04758 -0.00364 -0.00874 -0.00075 HKLF 4 Covalent radii and connectivity table for jain001 in P2(1)2(1)2(1) C 0.770 H 0.320 O 0.660 C1 - C2 C10 C2 - C3 C1 C3 - O1 C4 C2 C4 - C5 C3 C5 - C4 C6 C10 C6 - C5 C7 C7 - C6 C8 C8 - C14 C7 C9 C9 - C11 C8 C10 C10 - C5 C19 C1 C9 C11 - C12 C9 C12 - C13 C11 C13 - C17 C12 C14 C18 C14 - C8 C15 C13 C15 - C16 C14 C16 - O2 C17 C15 C17 - C20 C16 C13 C18 - C13 C19 - C10 C20 - C17 C21 C21 - C20 O1 - C3 O2 - C16 19138 Reflections read, of which 75 rejected -10 =< h =< 10, -16 =< k =< 17, -20 =< l =< 21, Max. 2-theta = 56.40 0 Systematic absence violations 0 Inconsistent equivalents 2324 Unique reflections, of which 0 suppressed R(int) = 0.0701 R(sigma) = 0.0432 Friedel opposites merged Maximum memory for data reduction = 3007 / 22774 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 = 3656 / 260403 wR2 = 0.1278 before cycle 1 for 2324 data and 211 / 211 parameters GooF = S = 1.213; Restrained GooF = 1.213 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84429 0.00197 -1.175 OSF Mean shift/esd = 0.291 Maximum = -2.208 for tors H18A Max. shift = 0.058 A for H18A Max. dU = 0.000 for C9 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3656 / 260403 wR2 = 0.1259 before cycle 2 for 2324 data and 211 / 211 parameters GooF = S = 1.194; Restrained GooF = 1.194 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84423 0.00194 -0.034 OSF Mean shift/esd = 0.106 Maximum = -0.714 for x C21 Max. shift = 0.023 A for H21B Max. dU = 0.000 for C21 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3656 / 260403 wR2 = 0.1258 before cycle 3 for 2324 data and 211 / 211 parameters GooF = S = 1.193; Restrained GooF = 1.193 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84431 0.00194 0.043 OSF Mean shift/esd = 0.024 Maximum = 1.228 for tors H21A Max. shift = 0.034 A for H21B Max. dU = 0.000 for C19 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3656 / 260403 wR2 = 0.1257 before cycle 4 for 2324 data and 211 / 211 parameters GooF = S = 1.191; Restrained GooF = 1.191 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84448 0.00194 0.087 OSF Mean shift/esd = 0.041 Maximum = 2.138 for tors H21A Max. shift = 0.060 A for H21D Max. dU = 0.000 for C16 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3656 / 260403 wR2 = 0.1253 before cycle 5 for 2324 data and 211 / 211 parameters GooF = S = 1.188; Restrained GooF = 1.188 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84468 0.00193 0.104 OSF 193 0.09914 0.02737 3.622 tors H21A Mean shift/esd = 0.070 Maximum = 3.622 for tors H21A Max. shift = 0.100 A for H21D Max. dU = 0.000 for C1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3656 / 260403 wR2 = 0.1243 before cycle 6 for 2324 data and 211 / 211 parameters GooF = S = 1.178; Restrained GooF = 1.178 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84500 0.00192 0.169 OSF 193 0.15272 0.02668 5.723 tors H21A Mean shift/esd = 0.108 Maximum = 5.723 for tors H21A Max. shift = 0.154 A for H21D Max. dU = 0.000 for C1 Least-squares cycle 7 Maximum vector length = 511 Memory required = 3656 / 260403 wR2 = 0.1220 before cycle 7 for 2324 data and 211 / 211 parameters GooF = S = 1.156; Restrained GooF = 1.156 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84537 0.00188 0.192 OSF 193 0.19864 0.02574 7.716 tors H21A Mean shift/esd = 0.136 Maximum = 7.716 for tors H21A Max. shift = 0.200 A for H21A Max. dU = 0.000 for C1 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3656 / 260403 wR2 = 0.1185 before cycle 8 for 2324 data and 211 / 211 parameters GooF = S = 1.122; Restrained GooF = 1.122 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84542 0.00183 0.031 OSF 193 0.20337 0.02549 7.977 tors H21A Mean shift/esd = 0.166 Maximum = 7.977 for tors H21A Max. shift = 0.208 A for H21A Max. dU = 0.000 for C3 Least-squares cycle 9 Maximum vector length = 511 Memory required = 3656 / 260403 wR2 = 0.1156 before cycle 9 for 2324 data and 211 / 211 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84534 0.00178 -0.048 OSF 193 0.13259 0.02562 5.174 tors H21A Mean shift/esd = 0.140 Maximum = 5.174 for tors H21A Max. shift = 0.136 A for H21A Max. dU = 0.000 for C21 Least-squares cycle 10 Maximum vector length = 511 Memory required = 3656 / 260403 wR2 = 0.1145 before cycle 10 for 2324 data and 211 / 211 parameters GooF = S = 1.084; Restrained GooF = 1.084 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84523 0.00177 -0.061 OSF Mean shift/esd = 0.056 Maximum = 1.899 for tors H21A Max. shift = 0.049 A for H21A Max. dU = 0.000 for C21 Least-squares cycle 11 Maximum vector length = 511 Memory required = 3656 / 260403 wR2 = 0.1144 before cycle 11 for 2324 data and 211 / 211 parameters GooF = S = 1.083; Restrained GooF = 1.083 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84521 0.00176 -0.008 OSF Mean shift/esd = 0.015 Maximum = 0.498 for tors H21A Max. shift = 0.013 A for H21A Max. dU = 0.000 for C21 Least-squares cycle 12 Maximum vector length = 511 Memory required = 3656 / 260403 wR2 = 0.1144 before cycle 12 for 2324 data and 211 / 211 parameters GooF = S = 1.083; Restrained GooF = 1.083 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84521 0.00176 -0.001 OSF Mean shift/esd = 0.003 Maximum = 0.122 for tors H21A Max. shift = 0.003 A for H21A Max. dU = 0.000 for C21 Least-squares cycle 13 Maximum vector length = 511 Memory required = 3656 / 260403 wR2 = 0.1144 before cycle 13 for 2324 data and 211 / 211 parameters GooF = S = 1.083; Restrained GooF = 1.083 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84521 0.00176 0.000 OSF Mean shift/esd = 0.001 Maximum = 0.030 for tors H21A Max. shift = 0.001 A for H21A Max. dU = 0.000 for C21 Least-squares cycle 14 Maximum vector length = 511 Memory required = 3656 / 260403 wR2 = 0.1144 before cycle 14 for 2324 data and 211 / 211 parameters GooF = S = 1.083; Restrained GooF = 1.083 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84521 0.00176 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.007 for tors H21A Max. shift = 0.000 A for H21A Max. dU = 0.000 for C21 Least-squares cycle 15 Maximum vector length = 511 Memory required = 3656 / 260403 wR2 = 0.1144 before cycle 15 for 2324 data and 211 / 211 parameters GooF = S = 1.083; Restrained GooF = 1.083 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84521 0.00176 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.002 for tors H21A Max. shift = 0.000 A for H21A Max. dU = 0.000 for C16 Least-squares cycle 16 Maximum vector length = 511 Memory required = 3656 / 260403 wR2 = 0.1144 before cycle 16 for 2324 data and 211 / 211 parameters GooF = S = 1.083; Restrained GooF = 1.083 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84521 0.00176 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H21A Max. dU = 0.000 for O1 Least-squares cycle 17 Maximum vector length = 511 Memory required = 3656 / 260403 wR2 = 0.1144 before cycle 17 for 2324 data and 211 / 211 parameters GooF = S = 1.083; Restrained GooF = 1.083 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84521 0.00176 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C10 Max. shift = 0.000 A for H21A Max. dU = 0.000 for C20 Least-squares cycle 18 Maximum vector length = 511 Memory required = 3656 / 260403 wR2 = 0.1144 before cycle 18 for 2324 data and 211 / 211 parameters GooF = S = 1.083; Restrained GooF = 1.083 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84521 0.00176 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C4 Max. dU = 0.000 for O1 Least-squares cycle 19 Maximum vector length = 511 Memory required = 3656 / 260403 wR2 = 0.1144 before cycle 19 for 2324 data and 211 / 211 parameters GooF = S = 1.083; Restrained GooF = 1.083 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84521 0.00176 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C10 Max. shift = 0.000 A for H21B Max. dU = 0.000 for C20 Least-squares cycle 20 Maximum vector length = 511 Memory required = 3656 / 260403 wR2 = 0.1144 before cycle 20 for 2324 data and 211 / 211 parameters GooF = S = 1.083; Restrained GooF = 1.083 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.84521 0.00176 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C4 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C19 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 H1A 0.8089 -0.1623 0.0002 23 0.990 0.000 C1 C2 C10 H1B 0.8641 -0.0898 -0.0732 23 0.990 0.000 C1 C2 C10 H2A 1.0168 -0.2780 -0.0360 23 0.990 0.000 C2 C3 C1 H2B 0.9100 -0.2525 -0.1174 23 0.990 0.000 C2 C3 C1 H4A 1.3501 -0.0947 -0.1083 43 0.950 0.000 C4 C5 C3 H6A 1.4089 0.0243 -0.0135 23 0.990 0.000 C6 C5 C7 H6B 1.3579 -0.0161 0.0760 23 0.990 0.000 C6 C5 C7 H7A 1.1904 0.1415 -0.0102 23 0.990 0.000 C7 C6 C8 H7B 1.3017 0.1541 0.0719 23 0.990 0.000 C7 C6 C8 H8A 1.0990 0.0637 0.1493 13 1.000 0.000 C8 C14 C7 C9 H9A 0.9135 0.0522 -0.0029 13 1.000 0.000 C9 C11 C8 C10 H11A 0.6970 -0.0335 0.0637 23 0.990 0.000 C11 C12 C9 H11B 0.7971 -0.0300 0.1495 23 0.990 0.000 C11 C12 C9 H12A 0.6482 0.1385 0.0679 23 0.990 0.000 C12 C13 C11 H12B 0.5870 0.0928 0.1543 23 0.990 0.000 C12 C13 C11 H14A 0.9240 0.2103 0.0548 13 1.000 0.000 C14 C8 C15 C13 H15A 1.1290 0.2603 0.1945 23 0.990 0.000 C15 C16 C14 H15B 1.1271 0.3138 0.1053 23 0.990 0.000 C15 C16 C14 H18A 0.7495 0.1284 0.2845 137 0.980 0.000 C18 C13 H18A H18B 0.9359 0.1748 0.2782 137 0.980 0.000 C18 C13 H18A H18C 0.9004 0.0649 0.2447 137 0.980 0.000 C18 C13 H18A H19A 1.1160 -0.2084 0.0881 137 0.980 0.000 C19 C10 H19A H19B 0.9543 -0.1606 0.1327 137 0.980 0.000 C19 C10 H19A H19C 1.1367 -0.1098 0.1425 137 0.980 0.000 C19 C10 H19A H20A 0.5100 0.2612 0.1928 43 0.950 0.000 C20 C17 C21 H21A 0.4808 0.4159 0.2661 137 0.980 0.000 C21 C20 H21A H21B 0.4510 0.4342 0.1696 137 0.980 0.000 C21 C20 H21A H21D 0.6304 0.4602 0.2104 137 0.980 0.000 C21 C20 H21A jain001 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.90728 -0.13737 -0.03154 1.00000 0.02270 0.02845 0.02917 -0.00233 0.00246 -0.00133 0.02677 0.00494 0.00036 0.00021 0.00019 0.00000 0.00141 0.00142 0.00148 0.00124 0.00128 0.00125 0.00062 H1A 0.80887 -0.16231 0.00025 1.00000 0.03213 0.00000 0.00000 H1B 0.86407 -0.08981 -0.07317 1.00000 0.03213 0.00000 0.00000 C2 0.99054 -0.22498 -0.07645 1.00000 0.02834 0.02909 0.03312 -0.00715 -0.00065 -0.00429 0.03018 0.00513 0.00039 0.00022 0.00019 0.00000 0.00160 0.00155 0.00156 0.00132 0.00136 0.00129 0.00068 H2A 1.01681 -0.27798 -0.03603 1.00000 0.03622 0.00000 0.00000 H2B 0.91001 -0.25245 -0.11741 1.00000 0.03622 0.00000 0.00000 C3 1.15067 -0.19426 -0.11966 1.00000 0.02847 0.03307 0.02626 -0.00227 -0.00155 0.00828 0.02927 0.00544 0.00039 0.00023 0.00018 0.00000 0.00159 0.00156 0.00149 0.00127 0.00130 0.00134 0.00067 C4 1.24630 -0.11349 -0.08295 1.00000 0.02279 0.03313 0.02825 0.00237 0.00160 0.00012 0.02806 0.00525 0.00038 0.00022 0.00019 0.00000 0.00146 0.00156 0.00152 0.00123 0.00127 0.00126 0.00065 H4A 1.35011 -0.09473 -0.10829 1.00000 0.03367 0.00000 0.00000 C5 1.19670 -0.06356 -0.01512 1.00000 0.02495 0.02698 0.02189 0.00495 0.00073 0.00292 0.02461 0.00508 0.00037 0.00021 0.00017 0.00000 0.00144 0.00140 0.00136 0.00114 0.00124 0.00123 0.00061 C6 1.31216 0.01154 0.02395 1.00000 0.02073 0.03627 0.02881 -0.00195 0.00165 -0.00192 0.02860 0.00497 0.00037 0.00022 0.00019 0.00000 0.00138 0.00161 0.00148 0.00131 0.00129 0.00131 0.00065 H6A 1.40892 0.02435 -0.01352 1.00000 0.03432 0.00000 0.00000 H6B 1.35793 -0.01614 0.07602 1.00000 0.03432 0.00000 0.00000 C7 1.22292 0.10914 0.04237 1.00000 0.02664 0.03133 0.02834 -0.00027 -0.00052 -0.00702 0.02877 0.00514 0.00038 0.00022 0.00019 0.00000 0.00157 0.00153 0.00153 0.00123 0.00131 0.00133 0.00067 H7A 1.19038 0.14153 -0.01019 1.00000 0.03453 0.00000 0.00000 H7B 1.30170 0.15407 0.07189 1.00000 0.03453 0.00000 0.00000 C8 1.06481 0.09270 0.09498 1.00000 0.02430 0.02768 0.02065 -0.00101 -0.00258 -0.00051 0.02421 0.00486 0.00037 0.00021 0.00017 0.00000 0.00142 0.00143 0.00134 0.00111 0.00121 0.00123 0.00060 H8A 1.09903 0.06367 0.14934 1.00000 0.02905 0.00000 0.00000 C9 0.94358 0.01987 0.05074 1.00000 0.02185 0.02710 0.02038 0.00111 -0.00272 0.00005 0.02311 0.00475 0.00037 0.00021 0.00017 0.00000 0.00140 0.00141 0.00128 0.00110 0.00114 0.00121 0.00059 H9A 0.91353 0.05222 -0.00289 1.00000 0.02773 0.00000 0.00000 C10 1.02703 -0.08193 0.02764 1.00000 0.02223 0.02434 0.02403 -0.00088 0.00034 -0.00032 0.02354 0.00483 0.00035 0.00021 0.00018 0.00000 0.00138 0.00137 0.00134 0.00113 0.00123 0.00118 0.00059 C11 0.77502 0.00701 0.09775 1.00000 0.02327 0.02833 0.03543 -0.00677 0.00186 -0.00301 0.02901 0.00512 0.00038 0.00022 0.00019 0.00000 0.00152 0.00148 0.00164 0.00129 0.00133 0.00126 0.00067 H11A 0.69702 -0.03350 0.06368 1.00000 0.03481 0.00000 0.00000 H11B 0.79709 -0.02999 0.14949 1.00000 0.03481 0.00000 0.00000 C12 0.68741 0.10583 0.11920 1.00000 0.02260 0.03106 0.03207 -0.00498 0.00205 0.00170 0.02858 0.00514 0.00038 0.00022 0.00020 0.00000 0.00145 0.00152 0.00160 0.00126 0.00131 0.00130 0.00066 H12A 0.64824 0.13855 0.06787 1.00000 0.03429 0.00000 0.00000 H12B 0.58703 0.09275 0.15426 1.00000 0.03429 0.00000 0.00000 C13 0.80962 0.17439 0.16485 1.00000 0.02934 0.02624 0.02372 -0.00176 0.00012 0.00193 0.02643 0.00509 0.00039 0.00021 0.00018 0.00000 0.00155 0.00143 0.00139 0.00115 0.00128 0.00126 0.00063 C14 0.96727 0.18869 0.10997 1.00000 0.02965 0.02621 0.02196 0.00142 -0.00468 0.00011 0.02594 0.00492 0.00039 0.00021 0.00018 0.00000 0.00154 0.00140 0.00132 0.00116 0.00126 0.00126 0.00062 H14A 0.92399 0.21028 0.05477 1.00000 0.03113 0.00000 0.00000 C15 1.05673 0.27933 0.14707 1.00000 0.03737 0.02790 0.02914 0.00036 -0.00287 -0.00619 0.03147 0.00527 0.00043 0.00022 0.00019 0.00000 0.00178 0.00153 0.00152 0.00125 0.00140 0.00142 0.00070 H15A 1.12898 0.26026 0.19449 1.00000 0.03776 0.00000 0.00000 H15B 1.12708 0.31376 0.10530 1.00000 0.03776 0.00000 0.00000 C16 0.90813 0.34406 0.17464 1.00000 0.04647 0.02822 0.01965 0.00294 -0.00679 0.00205 0.03145 0.00534 0.00044 0.00022 0.00018 0.00000 0.00195 0.00149 0.00139 0.00122 0.00143 0.00145 0.00071 C17 0.75302 0.28145 0.17838 1.00000 0.04005 0.02911 0.01980 0.00208 -0.00395 0.00312 0.02965 0.00526 0.00041 0.00022 0.00018 0.00000 0.00179 0.00150 0.00137 0.00120 0.00135 0.00136 0.00068 C18 0.85279 0.13172 0.25092 1.00000 0.04223 0.03250 0.02649 0.00222 0.00277 0.00761 0.03374 0.00585 0.00044 0.00023 0.00019 0.00000 0.00184 0.00163 0.00151 0.00130 0.00146 0.00147 0.00073 H18A 0.74952 0.12843 0.28445 1.00000 0.05061 0.00000 0.00000 H18B 0.93589 0.17482 0.27815 1.00000 0.05061 0.00000 0.00000 H18C 0.90035 0.06486 0.24473 1.00000 0.05061 0.00000 0.00000 C19 1.06164 -0.14603 0.10476 1.00000 0.02946 0.03019 0.02774 0.00202 0.00191 0.00157 0.02913 0.00541 0.00041 0.00022 0.00018 0.00000 0.00161 0.00151 0.00147 0.00126 0.00133 0.00133 0.00066 H19A 1.11595 -0.20838 0.08809 1.00000 0.04369 0.00000 0.00000 H19B 0.95431 -0.16062 0.13273 1.00000 0.04369 0.00000 0.00000 H19C 1.13667 -0.10983 0.14247 1.00000 0.04369 0.00000 0.00000 C20 0.59449 0.31147 0.19353 1.00000 0.04310 0.02949 0.03062 0.00140 0.00821 0.00414 0.03440 0.00603 0.00044 0.00024 0.00020 0.00000 0.00190 0.00154 0.00162 0.00132 0.00151 0.00149 0.00074 H20A 0.50999 0.26117 0.19280 1.00000 0.04128 0.00000 0.00000 C21 0.53397 0.41427 0.21145 1.00000 0.05168 0.03689 0.04323 0.00396 0.01485 0.00958 0.04393 0.00699 0.00051 0.00025 0.00023 0.00000 0.00223 0.00188 0.00198 0.00158 0.00181 0.00174 0.00091 H21A 0.48081 0.41590 0.26614 1.00000 0.06590 0.00000 0.00000 H21B 0.45100 0.43424 0.16957 1.00000 0.06590 0.00000 0.00000 H21D 0.63036 0.46020 0.21042 1.00000 0.06590 0.00000 0.00000 O1 1.20055 -0.23779 -0.18182 1.00000 0.03597 0.05379 0.03347 -0.01524 0.00483 0.00454 0.04107 0.00398 0.00029 0.00018 0.00014 0.00000 0.00126 0.00143 0.00120 0.00111 0.00111 0.00119 0.00058 O2 0.92011 0.43228 0.19031 1.00000 0.05814 0.02438 0.04677 -0.00337 -0.00875 -0.00042 0.04310 0.00401 0.00034 0.00016 0.00015 0.00000 0.00158 0.00113 0.00143 0.00103 0.00134 0.00115 0.00062 Final Structure Factor Calculation for jain001 in P2(1)2(1)2(1) Total number of l.s. parameters = 211 Maximum vector length = 511 Memory required = 3447 / 24024 wR2 = 0.1144 before cycle 21 for 2324 data and 2 / 211 parameters GooF = S = 1.083; Restrained GooF = 1.083 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0489 for 1887 Fo > 4sig(Fo) and 0.0744 for all 2324 data wR2 = 0.1144, GooF = S = 1.083, Restrained GooF = 1.083 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 23.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.0320 0.0265 0.0218 C1 0.0390 0.0301 0.0215 C2 0.0399 0.0257 0.0222 C3 0.0341 0.0277 0.0223 C4 0.0313 0.0238 0.0187 C5 0.0371 0.0285 0.0203 C6 0.0364 0.0284 0.0215 C7 0.0278 0.0256 0.0192 C8 0.0273 0.0238 0.0182 C9 0.0252 0.0233 0.0222 C10 0.0401 0.0252 0.0217 C11 0.0366 0.0279 0.0213 C12 0.0303 0.0263 0.0227 C13 0.0319 0.0264 0.0195 C14 0.0411 0.0287 0.0246 C15 0.0482 0.0291 0.0170 C16 0.0414 0.0292 0.0184 C17 0.0470 0.0285 0.0258 C18 0.0329 0.0282 0.0262 C19 0.0482 0.0286 0.0264 C20 0.0663 0.0353 0.0301 C21 0.0621 0.0389 0.0223 O1 0.0629 0.0426 0.0238 O2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.019 0.030 0.040 0.050 0.060 0.074 0.091 0.119 0.177 1.000 Number in group 247. 228. 235. 229. 231. 239. 222. 232. 227. 234. GooF 1.066 1.086 1.086 1.315 1.116 1.238 1.023 0.960 0.901 0.964 K 1.434 0.976 0.937 0.975 1.009 1.008 0.986 0.995 0.991 1.012 Resolution(A) 0.75 0.79 0.82 0.86 0.91 0.97 1.05 1.16 1.34 1.72 inf Number in group 237. 231. 232. 230. 234. 235. 227. 232. 235. 231. GooF 1.649 1.254 1.156 1.058 0.946 0.879 0.793 0.795 0.839 1.145 K 0.607 1.130 1.136 1.105 1.050 0.998 0.997 0.975 0.980 1.017 R1 0.344 0.151 0.132 0.116 0.085 0.060 0.044 0.032 0.035 0.023 Recommended weighting scheme: WGHT 0.0173 1.0771 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) 6 14 4 4.07 57.04 5.00 0.065 0.76 1 17 5 1.18 61.17 3.87 0.067 0.77 8 2 10 25.75 3.26 3.84 0.015 0.84 1 16 8 -0.23 24.89 3.82 0.043 0.77 1 2 21 7.70 77.94 3.56 0.076 0.76 6 11 11 -3.76 24.26 3.50 0.042 0.77 0 16 9 13.65 62.12 3.28 0.068 0.76 2 5 1 3582.45 3203.44 3.18 0.486 2.20 9 4 9 23.39 78.07 3.13 0.076 0.77 0 6 19 295.87 215.30 3.05 0.126 0.80 2 15 10 -4.54 23.43 3.01 0.042 0.77 10 0 4 19.50 68.93 2.99 0.071 0.77 1 2 20 105.18 148.65 2.98 0.105 0.80 3 13 12 4.09 29.24 2.93 0.046 0.78 3 0 2 1936.95 1722.06 2.91 0.356 2.50 3 9 17 -11.06 33.54 2.86 0.050 0.77 0 0 2 1170.53 1336.78 2.86 0.314 8.10 5 4 18 3.37 54.34 2.85 0.063 0.76 6 9 13 28.80 54.54 2.83 0.063 0.77 3 14 11 -4.26 23.64 2.81 0.042 0.77 8 7 8 96.09 55.00 2.75 0.064 0.80 4 16 1 28.72 62.67 2.72 0.068 0.77 5 8 7 94.30 132.93 2.70 0.099 1.03 4 10 4 81.48 52.01 2.69 0.062 1.07 0 1 21 -16.36 30.82 2.68 0.048 0.77 6 14 2 16.00 42.75 2.66 0.056 0.77 1 5 20 43.35 86.89 2.64 0.080 0.77 3 5 19 -10.69 20.09 2.63 0.038 0.78 4 0 0 720.48 620.08 2.60 0.214 1.97 3 15 9 19.42 59.40 2.58 0.066 0.77 4 13 12 6.76 42.55 2.57 0.056 0.76 7 4 11 107.87 73.70 2.55 0.074 0.86 5 0 18 -0.17 21.35 2.54 0.040 0.78 0 6 6 71.29 101.71 2.54 0.087 1.72 0 6 15 17.81 1.47 2.52 0.010 0.97 3 15 10 -13.40 22.91 2.51 0.041 0.75 5 14 3 39.59 21.76 2.49 0.040 0.81 2 14 12 -7.85 13.76 2.48 0.032 0.77 2 7 15 20.42 7.07 2.47 0.023 0.92 5 12 6 38.67 15.76 2.47 0.034 0.87 3 10 12 35.10 17.27 2.47 0.036 0.90 1 14 12 6.68 33.56 2.47 0.050 0.78 3 4 5 474.54 406.81 2.46 0.173 1.75 6 2 6 225.84 280.13 2.46 0.144 1.16 8 9 6 -9.06 16.33 2.46 0.035 0.79 0 1 7 98.15 71.28 2.45 0.072 2.28 0 1 2 1806.07 1991.54 2.44 0.383 6.94 2 17 4 -10.60 25.32 2.44 0.043 0.76 0 1 19 179.26 128.69 2.43 0.097 0.85 6 13 7 3.90 26.19 2.42 0.044 0.77 Bond lengths and angles C1 - Distance Angles C2 1.5329 (0.0039) C10 1.5386 (0.0039) 113.92 (0.24) H1A 0.9900 108.77 108.77 H1B 0.9900 108.77 108.77 107.66 C1 - C2 C10 H1A C2 - Distance Angles C3 1.5019 (0.0042) C1 1.5329 (0.0039) 111.69 (0.25) H2A 0.9900 109.28 109.28 H2B 0.9900 109.28 109.28 107.95 C2 - C3 C1 H2A C3 - Distance Angles O1 1.2292 (0.0036) C4 1.4505 (0.0042) 121.75 (0.29) C2 1.5019 (0.0042) 121.30 (0.29) 116.92 (0.26) C3 - O1 C4 C4 - Distance Angles C5 1.3457 (0.0040) C3 1.4505 (0.0042) 123.88 (0.28) H4A 0.9500 118.06 118.06 C4 - C5 C3 C5 - Distance Angles C4 1.3457 (0.0040) C6 1.5003 (0.0040) 120.26 (0.27) C10 1.5269 (0.0039) 122.96 (0.27) 116.74 (0.24) C5 - C4 C6 C6 - Distance Angles C5 1.5003 (0.0040) C7 1.5197 (0.0040) 112.57 (0.24) H6A 0.9900 109.08 109.08 H6B 0.9900 109.08 109.08 107.83 C6 - C5 C7 H6A C7 - Distance Angles C6 1.5197 (0.0040) C8 1.5265 (0.0040) 111.26 (0.23) H7A 0.9900 109.38 109.38 H7B 0.9900 109.38 109.38 108.00 C7 - C6 C8 H7A C8 - Distance Angles C14 1.5230 (0.0039) C7 1.5265 (0.0040) 112.25 (0.24) C9 1.5453 (0.0037) 107.41 (0.23) 109.80 (0.23) H8A 1.0000 109.11 109.11 109.11 C8 - C14 C7 C9 C9 - Distance Angles C11 1.5417 (0.0040) C8 1.5453 (0.0037) 112.08 (0.22) C10 1.5652 (0.0038) 112.48 (0.23) 113.93 (0.23) H9A 1.0000 105.85 105.85 105.85 C9 - C11 C8 C10 C10 - Distance Angles C5 1.5269 (0.0039) C19 1.5420 (0.0040) 107.61 (0.23) C1 1.5386 (0.0039) 109.52 (0.23) 109.99 (0.23) C9 1.5652 (0.0038) 109.59 (0.23) 111.75 (0.23) 108.37 (0.23) C10 - C5 C19 C1 C11 - Distance Angles C12 1.5384 (0.0040) C9 1.5417 (0.0040) 113.69 (0.24) H11A 0.9900 108.82 108.82 H11B 0.9900 108.82 108.82 107.69 C11 - C12 C9 H11A C12 - Distance Angles C13 1.5253 (0.0041) C11 1.5384 (0.0040) 110.39 (0.25) H12A 0.9900 109.58 109.58 H12B 0.9900 109.58 109.58 108.12 C12 - C13 C11 H12A C13 - Distance Angles C17 1.5242 (0.0039) C12 1.5253 (0.0041) 117.15 (0.26) C14 1.5404 (0.0042) 101.61 (0.23) 107.83 (0.23) C18 1.5452 (0.0041) 106.63 (0.24) 110.58 (0.25) 112.88 (0.25) C13 - C17 C12 C14 C14 - Distance Angles C8 1.5230 (0.0039) C15 1.5318 (0.0040) 120.34 (0.25) C13 1.5404 (0.0042) 113.18 (0.23) 104.19 (0.24) H14A 1.0000 106.05 106.05 106.05 C14 - C8 C15 C13 C15 - Distance Angles C16 1.5270 (0.0045) C14 1.5318 (0.0040) 102.43 (0.25) H15A 0.9900 111.28 111.28 H15B 0.9900 111.28 111.28 109.18 C15 - C16 C14 H15A C16 - Distance Angles O2 1.2178 (0.0035) C17 1.4867 (0.0044) 127.44 (0.32) C15 1.5270 (0.0045) 123.88 (0.31) 108.68 (0.24) C16 - O2 C17 C17 - Distance Angles C20 1.3367 (0.0045) C16 1.4867 (0.0044) 127.30 (0.29) C13 1.5242 (0.0039) 125.87 (0.29) 106.78 (0.25) C17 - C20 C16 C18 - Distance Angles C13 1.5452 (0.0041) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - C13 H18A H18B C19 - Distance Angles C10 1.5420 (0.0040) H19A 0.9800 109.47 H19B 0.9800 109.47 109.47 H19C 0.9800 109.47 109.47 109.47 C19 - C10 H19A H19B C20 - Distance Angles C17 1.3367 (0.0045) C21 1.4920 (0.0044) 127.96 (0.32) H20A 0.9500 116.02 116.02 C20 - C17 C21 C21 - Distance Angles C20 1.4920 (0.0044) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21D 0.9800 109.47 109.47 109.47 C21 - C20 H21A H21B O1 - Distance Angles C3 1.2292 (0.0036) O1 - O2 - Distance Angles C16 1.2178 (0.0035) O2 - Selected torsion angles -53.15 ( 0.34) C10 - C1 - C2 - C3 -151.84 ( 0.29) C1 - C2 - C3 - O1 30.31 ( 0.37) C1 - C2 - C3 - C4 179.86 ( 0.30) O1 - C3 - C4 - C5 -2.31 ( 0.44) C2 - C3 - C4 - C5 173.42 ( 0.27) C3 - C4 - C5 - C6 -4.29 ( 0.45) C3 - C4 - C5 - C10 131.94 ( 0.29) C4 - C5 - C6 - C7 -50.21 ( 0.34) C10 - C5 - C6 - C7 54.68 ( 0.33) C5 - C6 - C7 - C8 -176.57 ( 0.24) C6 - C7 - C8 - C14 -57.17 ( 0.31) C6 - C7 - C8 - C9 -53.04 ( 0.30) C14 - C8 - C9 - C11 -175.37 ( 0.24) C7 - C8 - C9 - C11 177.79 ( 0.22) C14 - C8 - C9 - C10 55.47 ( 0.30) C7 - C8 - C9 - C10 101.94 ( 0.31) C4 - C5 - C10 - C19 -75.85 ( 0.30) C6 - C5 - C10 - C19 -17.60 ( 0.37) C4 - C5 - C10 - C1 164.62 ( 0.24) C6 - C5 - C10 - C1 -136.35 ( 0.28) C4 - C5 - C10 - C9 45.86 ( 0.32) C6 - C5 - C10 - C9 45.72 ( 0.33) C2 - C1 - C10 - C5 -72.34 ( 0.31) C2 - C1 - C10 - C19 165.23 ( 0.24) C2 - C1 - C10 - C9 -177.44 ( 0.23) C11 - C9 - C10 - C5 -48.48 ( 0.30) C8 - C9 - C10 - C5 -58.25 ( 0.30) C11 - C9 - C10 - C19 70.71 ( 0.30) C8 - C9 - C10 - C19 63.10 ( 0.30) C11 - C9 - C10 - C1 -167.94 ( 0.23) C8 - C9 - C10 - C1 51.69 ( 0.33) C8 - C9 - C11 - C12 -178.39 ( 0.25) C10 - C9 - C11 - C12 -53.25 ( 0.33) C9 - C11 - C12 - C13 170.31 ( 0.25) C11 - C12 - C13 - C17 56.58 ( 0.31) C11 - C12 - C13 - C14 -67.27 ( 0.31) C11 - C12 - C13 - C18 -54.46 ( 0.34) C7 - C8 - C14 - C15 -175.26 ( 0.25) C9 - C8 - C14 - C15 -178.50 ( 0.23) C7 - C8 - C14 - C13 60.71 ( 0.29) C9 - C8 - C14 - C13 172.84 ( 0.24) C17 - C13 - C14 - C8 -63.42 ( 0.30) C12 - C13 - C14 - C8 59.03 ( 0.31) C18 - C13 - C14 - C8 40.38 ( 0.27) C17 - C13 - C14 - C15 164.11 ( 0.24) C12 - C13 - C14 - C15 -73.44 ( 0.29) C18 - C13 - C14 - C15 -163.82 ( 0.25) C8 - C14 - C15 - C16 -35.61 ( 0.28) C13 - C14 - C15 - C16 -162.64 ( 0.30) C14 - C15 - C16 - O2 17.30 ( 0.30) C14 - C15 - C16 - C17 5.57 ( 0.54) O2 - C16 - C17 - C20 -174.37 ( 0.31) C15 - C16 - C17 - C20 -172.27 ( 0.30) O2 - C16 - C17 - C13 7.80 ( 0.32) C15 - C16 - C17 - C13 35.52 ( 0.44) C12 - C13 - C17 - C20 152.69 ( 0.31) C14 - C13 - C17 - C20 -88.91 ( 0.38) C18 - C13 - C17 - C20 -146.61 ( 0.26) C12 - C13 - C17 - C16 -29.44 ( 0.29) C14 - C13 - C17 - C16 88.96 ( 0.28) C18 - C13 - C17 - C16 -0.88 ( 0.57) C16 - C17 - C20 - C21 176.56 ( 0.31) C13 - C17 - C20 - C21 FMAP and GRID set by program FMAP 2 3 21 GRID -1.389 -2 -2 1.389 2 2 R1 = 0.0744 for 2324 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.24 at 0.2587 0.8164 0.1910 [ 1.59 A from H19C ] Deepest hole -0.22 at 0.8804 0.0790 0.1246 [ 1.35 A from C11 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 3403 / 20844 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.2587 -0.1836 0.1910 1.00000 0.05 0.24 1.59 H19C 1.89 H2B 2.04 H19A 2.15 C19 Q2 1 1.2715 -0.1253 -0.0312 1.00000 0.05 0.23 0.88 C4 1.05 C5 1.45 H4A 1.96 C3 Q3 1 1.0555 0.4416 0.2470 1.00000 0.05 0.23 1.41 O2 1.70 H18C 2.07 H11B 2.11 C16 Q4 1 0.6841 0.3002 0.1445 1.00000 0.05 0.22 0.81 C17 1.07 C20 1.66 H20A 1.93 C16 Q5 1 1.1733 -0.1618 -0.1965 1.00000 0.05 0.21 1.07 O1 1.33 C3 2.03 C4 2.19 H4A Q6 1 1.0749 0.4590 0.1632 1.00000 0.05 0.20 1.35 O2 2.04 C16 2.07 H18C 2.21 H15B Q7 1 0.8049 -0.1193 0.1654 1.00000 0.05 0.20 1.23 H11B 1.41 H19B 2.04 C11 2.11 O1 Q8 1 1.2038 -0.0770 -0.0581 1.00000 0.05 0.19 0.72 C4 0.72 C5 1.43 H4A 1.91 C3 Q9 1 1.0445 0.0054 0.0600 1.00000 0.05 0.19 0.83 C9 1.29 C10 1.31 C8 1.58 H9A Q10 1 0.7725 0.3601 0.1646 1.00000 0.05 0.19 1.09 C17 1.10 C16 1.57 O2 1.62 C20 Q11 1 0.4116 0.3222 0.1137 1.00000 0.05 0.19 1.71 H20A 1.79 H21B 1.94 C20 2.23 C21 Q12 1 0.4979 0.2775 0.1476 1.00000 0.05 0.19 0.77 H20A 1.16 C20 2.07 C17 2.13 C21 Q13 1 0.7772 0.1446 0.1427 1.00000 0.05 0.18 0.60 C13 0.96 C12 1.58 H12A 1.66 H12B Q14 1 0.9491 -0.1574 -0.0643 1.00000 0.05 0.18 0.68 C1 0.99 C2 1.14 H1B 1.52 H1A Q15 1 0.9008 0.1989 0.2229 1.00000 0.05 0.18 0.99 H18B 1.08 C18 1.23 C13 1.76 C17 Q16 1 1.0254 -0.0769 -0.1233 1.00000 0.05 0.18 1.52 H1B 1.86 C3 1.92 C4 1.93 C1 Q17 1 1.0901 -0.1784 -0.1956 1.00000 0.05 0.18 1.20 O1 1.34 C3 2.15 H2B 2.17 C2 Q18 1 0.7743 0.2368 0.1613 1.00000 0.05 0.18 0.68 C17 0.89 C13 1.80 C16 1.81 C20 Q19 1 1.0477 0.2587 0.2661 1.00000 0.05 0.17 1.33 H15A 1.45 H18B 1.95 C15 1.97 H19B Q20 1 0.9340 -0.2774 -0.0119 1.00000 0.05 0.17 0.76 H2A 1.34 C2 1.75 H2B 1.85 H1A Shortest distances between peaks (including symmetry equivalents) 5 17 0.69 2 8 0.95 11 12 1.06 4 10 1.11 4 18 1.14 13 18 1.28 3 6 1.39 4 12 1.50 15 18 1.50 14 16 1.56 15 19 1.57 10 18 1.66 8 16 1.76 13 15 1.78 14 20 1.83 16 17 1.87 2 20 1.96 3 7 1.97 5 16 2.02 4 13 2.22 4 11 2.23 12 18 2.26 8 14 2.28 7 19 2.30 14 17 2.41 1 10 2.42 10 12 2.45 1 15 2.45 3 19 2.48 5 8 2.53 4 15 2.53 2 16 2.53 8 9 2.54 10 15 2.57 5 19 2.63 1 19 2.63 1 18 2.63 2 14 2.63 1 4 2.71 6 10 2.73 18 19 2.76 8 17 2.76 5 14 2.78 3 10 2.82 2 5 2.83 12 13 2.84 8 20 2.90 2 9 2.91 10 13 2.92 12 17 2.95 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. 0.11: 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 0.77: Structure factors and derivatives 0.94: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.17: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + jain001 finished at 12:59:28 Total CPU time: 2.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++