+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005src0328 started at 11:00:13 on 20-May-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005src0328 in Pbca CELL 0.71073 7.7470 15.5194 25.7449 90.000 90.000 90.000 ZERR 8.00 0.0089 0.0179 0.0081 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N RU UNIT 128 192 16 8 V = 3095.28 F(000) = 1424.0 Mu = 1.00 mm-1 Cell Wt = 2763.54 Rho = 1.483 MERG 2 OMIT -3.00 55.00 OMIT 0 0 4 OMIT 0 0 6 OMIT 1 2 3 SHEL 7 0.77 SIMU 0.005 FLAT C1 C2 C3 C4 C5 C1 FLAT C6 C7 C8 C9 C10 C6 FMAP 2 PLAN 5 SIZE 0.02 0.03 0.18 ACTA BOND $H WGHT 0.00000 72.17880 L.S. 20 TEMP -153.00 FVAR 0.22369 0.85215 MOLE 1 PART 1 C1 1 0.088585 0.746931 0.410220 21.00000 0.02107 0.02332 = 0.01316 0.00108 0.00099 -0.00075 C2 1 -0.034895 0.747695 0.369371 21.00000 0.02093 0.02279 = 0.01661 -0.00165 0.00150 -0.00117 C3 1 -0.113769 0.832318 0.367882 21.00000 0.01939 0.02444 = 0.01584 0.00117 0.00675 0.00505 AFIX 43 H3 2 -0.201917 0.850714 0.344750 21.00000 -1.20000 AFIX 0 C4 1 -0.036674 0.881640 0.406548 21.00000 0.02214 0.02471 = 0.01272 0.00290 0.00404 0.00347 AFIX 43 H4 2 -0.064158 0.940145 0.413580 21.00000 -1.20000 AFIX 0 C5 1 0.088369 0.833050 0.434083 21.00000 0.02277 0.02430 = 0.00917 0.00116 0.00356 0.00165 AFIX 43 H5 2 0.157856 0.852200 0.462210 21.00000 -1.20000 AFIX 0 SAME C1 > C5 C6 1 0.410226 0.813760 0.316352 21.00000 0.02024 0.02588 = 0.02513 0.00910 0.00717 -0.00284 AFIX 43 H6 2 0.475799 0.764457 0.325785 21.00000 -1.20000 AFIX 0 C7 1 0.281851 0.817287 0.277224 21.00000 0.02188 0.02619 = 0.02319 0.00468 0.00642 -0.00343 AFIX 43 H7 2 0.248606 0.771154 0.255129 21.00000 -1.20000 AFIX 0 C8 1 0.210281 0.903249 0.276767 21.00000 0.01945 0.02448 = 0.02046 0.00684 0.00660 -0.00472 AFIX 43 H8 2 0.121439 0.923865 0.254574 21.00000 -1.20000 AFIX 0 C9 1 0.295598 0.949996 0.314794 21.00000 0.01858 0.02327 = 0.02146 0.00738 0.00622 -0.00667 AFIX 43 H9 2 0.271521 1.008374 0.323205 21.00000 -1.20000 AFIX 0 C10 1 0.423909 0.898968 0.339533 21.00000 0.01597 0.02380 = 0.02702 0.00774 0.00592 -0.00575 AFIX 43 H10 2 0.502357 0.916819 0.365775 21.00000 -1.20000 AFIX 0 C11 1 0.198536 0.673712 0.426210 21.00000 0.01735 0.02136 = 0.01425 0.00322 0.00264 -0.00089 AFIX 23 H11A 2 0.304585 0.696623 0.442630 21.00000 -1.20000 H11B 2 0.233662 0.641343 0.394804 21.00000 -1.20000 AFIX 0 C12 1 0.223941 0.539089 0.473339 21.00000 0.02751 0.02389 = 0.01674 -0.00193 0.00537 0.00264 AFIX 137 H12A 2 0.256711 0.512118 0.440363 21.00000 -1.50000 H12B 2 0.161616 0.497248 0.494813 21.00000 -1.50000 H12C 2 0.327997 0.558146 0.491686 21.00000 -1.50000 AFIX 0 C13 1 0.074435 0.656196 0.511974 21.00000 0.02677 0.03077 = 0.01598 -0.00229 0.00716 0.00800 AFIX 137 H13A 2 0.021445 0.615137 0.536101 21.00000 -1.50000 H13B 2 -0.005696 0.703862 0.505496 21.00000 -1.50000 H13C 2 0.181289 0.678747 0.527150 21.00000 -1.50000 AFIX 0 C14 1 -0.087026 0.669087 0.334230 21.00000 0.02666 0.02483 = 0.02356 -0.00561 -0.00179 -0.00018 AFIX 23 H14A 2 -0.067929 0.683215 0.297174 21.00000 -1.20000 H14B 2 -0.016058 0.618126 0.343115 21.00000 -1.20000 AFIX 0 C15 1 -0.301153 0.623791 0.394916 21.00000 0.03975 0.02308 = 0.04017 -0.01065 0.00504 -0.01517 AFIX 137 H15A 2 -0.214672 0.580666 0.404714 21.00000 -1.50000 H15B 2 -0.416746 0.598529 0.397600 21.00000 -1.50000 H15C 2 -0.292602 0.673483 0.418262 21.00000 -1.50000 AFIX 0 C16 1 -0.317369 0.582057 0.307803 21.00000 0.04019 0.03710 = 0.04166 -0.00450 -0.00240 -0.01046 AFIX 137 H16A 2 -0.289788 0.599863 0.272238 21.00000 -1.50000 H16B 2 -0.441236 0.570044 0.310500 21.00000 -1.50000 H16C 2 -0.251943 0.529974 0.316503 21.00000 -1.50000 AFIX 0 N1 3 0.113469 0.612864 0.463190 21.00000 0.01635 0.02294 = 0.01138 0.00042 0.00657 0.00484 N2 3 -0.271693 0.650575 0.343579 21.00000 0.03154 0.02641 = 0.03115 -0.00920 -0.00096 -0.00390 RU1 4 0.163113 0.842415 0.352111 21.00000 0.01963 0.02259 = 0.01224 0.00227 0.00140 0.00005 PART 2 SAME C1 > RU1 C21 1 0.413517 0.743693 0.409126 -21.00000 0.02206 0.01903 = 0.01919 0.00384 0.00054 -0.00323 C22 1 0.538015 0.745093 0.368755 -21.00000 0.02317 0.01778 = 0.02067 0.00492 -0.00094 -0.00536 C23 1 0.618030 0.829478 0.368579 -21.00000 0.02364 0.01808 = 0.02050 0.00540 -0.00159 -0.00555 AFIX 43 H23 2 0.707567 0.848171 0.346023 -21.00000 -1.20000 AFIX 0 C24 1 0.540309 0.878030 0.407283 -21.00000 0.02348 0.01815 = 0.01995 0.00463 -0.00051 -0.00503 AFIX 43 H24 2 0.567474 0.936411 0.414786 -21.00000 -1.20000 AFIX 0 C25 1 0.414808 0.828677 0.434123 -21.00000 0.02290 0.01871 = 0.01952 0.00415 -0.00026 -0.00380 AFIX 43 H25 2 0.345582 0.846914 0.462529 -21.00000 -1.20000 AFIX 0 C26 1 0.093948 0.813939 0.316029 -21.00000 0.01964 0.02412 = 0.01668 0.00346 0.00384 -0.00231 AFIX 43 H26 2 0.027120 0.765002 0.325357 -21.00000 -1.20000 AFIX 0 C27 1 0.222672 0.817589 0.276979 -21.00000 0.02002 0.02504 = 0.02040 0.00486 0.00567 -0.00384 AFIX 43 H27 2 0.254307 0.771627 0.254544 -21.00000 -1.20000 AFIX 0 C28 1 0.297921 0.902902 0.276942 -21.00000 0.01995 0.02457 = 0.02102 0.00591 0.00603 -0.00465 AFIX 43 H28 2 0.388080 0.922742 0.254975 -21.00000 -1.20000 AFIX 0 C29 1 0.213858 0.950333 0.314970 -21.00000 0.01919 0.02372 = 0.01995 0.00603 0.00567 -0.00439 AFIX 43 H29 2 0.239865 1.008431 0.323562 -21.00000 -1.20000 AFIX 0 C30 1 0.083445 0.900097 0.339329 -21.00000 0.01920 0.02315 = 0.01674 0.00419 0.00391 -0.00202 AFIX 43 H30 2 0.005178 0.918597 0.365455 -21.00000 -1.20000 AFIX 0 C31 1 0.304152 0.670363 0.424885 -21.00000 0.02032 0.02062 = 0.01753 0.00278 0.00180 -0.00033 AFIX 23 H31A 2 0.267117 0.638467 0.393503 -21.00000 -1.20000 H31B 2 0.199319 0.692547 0.442342 -21.00000 -1.20000 AFIX 0 C32 1 0.430618 0.652493 0.510061 -21.00000 0.02121 0.02070 = 0.02016 0.00194 0.00143 0.00345 AFIX 137 H32A 2 0.321145 0.667615 0.526816 -21.00000 -1.50000 H32B 2 0.497860 0.704965 0.503807 -21.00000 -1.50000 H32C 2 0.496113 0.613677 0.532712 -21.00000 -1.50000 AFIX 0 C33 1 0.290646 0.533952 0.469893 -21.00000 0.02405 0.02247 = 0.01837 0.00108 0.00328 0.00350 AFIX 137 H33A 2 0.353658 0.493470 0.492118 -21.00000 -1.50000 H33B 2 0.264100 0.506242 0.436634 -21.00000 -1.50000 H33C 2 0.182981 0.550949 0.487050 -21.00000 -1.50000 AFIX 0 C34 1 0.585100 0.672176 0.328674 -21.00000 0.02346 0.01674 = 0.02226 0.00544 -0.00129 -0.00687 AFIX 23 H34A 2 0.509057 0.621710 0.334117 -21.00000 -1.20000 H34B 2 0.567137 0.693498 0.292836 -21.00000 -1.20000 AFIX 0 C35 1 0.888933 0.712374 0.335120 -21.00000 0.02399 0.01401 = 0.02909 0.00193 -0.00371 -0.01147 AFIX 137 H35A 2 0.935042 0.718933 0.299894 -21.00000 -1.50000 H35B 2 0.983030 0.697811 0.358999 -21.00000 -1.50000 H35C 2 0.835072 0.766524 0.346112 -21.00000 -1.50000 AFIX 0 C36 1 0.800074 0.584170 0.295036 -21.00000 0.02276 0.01832 = 0.02575 0.00452 0.00005 -0.01061 AFIX 137 H36A 2 0.712036 0.589293 0.267876 -21.00000 -1.50000 H36B 2 0.796884 0.525965 0.309767 -21.00000 -1.50000 H36C 2 0.914297 0.594999 0.280035 -21.00000 -1.50000 AFIX 0 N21 3 0.396070 0.609757 0.460825 -21.00000 0.02091 0.02084 = 0.01852 0.00237 0.00151 0.00094 N22 3 0.766046 0.646699 0.335626 -21.00000 0.02335 0.01574 = 0.02421 0.00471 -0.00077 -0.00836 RU21 4 0.341519 0.841125 0.352220 -21.00000 0.01502 0.01886 = 0.03031 0.00213 0.00320 -0.00085 HKLF 4 Covalent radii and connectivity table for 2005src0328 in Pbca C 0.770 H 0.320 N 0.700 RU 1.330 C1_a - C2_a C5_a C11_a Ru1_a C2_a - C1_a C3_a C14_a Ru1_a C3_a - C4_a C2_a Ru1_a C4_a - C3_a C5_a Ru1_a C5_a - C4_a C1_a Ru1_a C6_a - C7_a C10_a Ru1_a C7_a - C6_a C8_a Ru1_a C8_a - C9_a C7_a Ru1_a C9_a - C8_a C10_a Ru1_a C10_a - C9_a C6_a Ru1_a C11_a - C1_a N1_a C12_a - N1_a C13_a - N1_a C14_a - N2_a C2_a C15_a - N2_a C16_a - N2_a N1_a - C12_a C13_a C11_a N2_a - C15_a C16_a C14_a Ru1_a - C6_a C2_a C7_a C4_a C9_a C1_a C8_a C3_a C5_a C10_a C21_b - C22_b C25_b C31_b Ru21_b C22_b - C21_b C23_b C34_b Ru21_b C23_b - C24_b C22_b Ru21_b C24_b - C23_b C25_b Ru21_b C25_b - C24_b C21_b Ru21_b C26_b - C27_b C30_b Ru21_b C27_b - C26_b C28_b Ru21_b C28_b - C29_b C27_b Ru21_b C29_b - C28_b C30_b Ru21_b C30_b - C29_b C26_b Ru21_b C31_b - C21_b N21_b C32_b - N21_b C33_b - N21_b C34_b - N22_b C22_b C35_b - N22_b C36_b - N22_b N21_b - C33_b C32_b C31_b N22_b - C35_b C36_b C34_b Ru21_b - C24_b C22_b C26_b C27_b C21_b C29_b C28_b C23_b C25_b C30_b 14544 Reflections read, of which 1211 rejected -7 =< h =< 9, -19 =< k =< 19, -33 =< l =< 21, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 4 5 15 104.29 26.57 2 306.14 1 Inconsistent equivalents 3397 Unique reflections, of which 0 suppressed R(int) = 0.1721 R(sigma) = 0.2068 Friedel opposites merged Maximum memory for data reduction = 5161 / 33798 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 = 6248 / 445571 wR2 = 0.2333 before cycle 1 for 3397 data and 352 / 352 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint -0.0181 0.0050 SIMU U33 Ru1_a Ru21_b Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 117. 0. 0. 6. 0. 300. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.100 0.000 0.006 0.000 0.000 rms deviation 0.000 0.000 0.000 0.011 0.000 0.000 0.045 0.000 0.003 0.000 0.000 GooF = S = 1.114; Restrained GooF = 1.057 for 423 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 72.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22365 0.00094 -0.039 OSF 2 0.85219 0.00236 0.018 FVAR 2 Mean shift/esd = 0.003 Maximum = -0.039 for OSF Max. shift = 0.003 A for H35A_b Max. dU = 0.000 for C35_b Least-squares cycle 2 Maximum vector length = 511 Memory required = 6248 / 445571 wR2 = 0.2333 before cycle 2 for 3397 data and 352 / 352 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint -0.0180 0.0050 SIMU U33 Ru1_a Ru21_b Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 117. 0. 0. 6. 0. 300. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.100 0.000 0.006 0.000 0.000 rms deviation 0.000 0.000 0.000 0.011 0.000 0.000 0.045 0.000 0.003 0.000 0.000 GooF = S = 1.115; Restrained GooF = 1.057 for 423 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 72.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22364 0.00094 -0.010 OSF 2 0.85221 0.00236 0.007 FVAR 2 Mean shift/esd = 0.001 Maximum = -0.010 for OSF Max. shift = 0.003 A for H35C_b Max. dU = 0.000 for C35_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 6248 / 445571 wR2 = 0.2333 before cycle 3 for 3397 data and 352 / 352 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint -0.0180 0.0050 SIMU U33 Ru1_a Ru21_b Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 117. 0. 0. 6. 0. 300. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.100 0.000 0.006 0.000 0.000 rms deviation 0.000 0.000 0.000 0.011 0.000 0.000 0.045 0.000 0.003 0.000 0.000 GooF = S = 1.114; Restrained GooF = 1.057 for 423 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 72.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22364 0.00094 0.000 OSF 2 0.85221 0.00236 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.005 for tors H35A_b Max. shift = 0.002 A for H35A_b Max. dU = 0.000 for C35_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 6248 / 445571 wR2 = 0.2333 before cycle 4 for 3397 data and 352 / 352 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint -0.0180 0.0050 SIMU U33 Ru1_a Ru21_b Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 117. 0. 0. 6. 0. 300. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.100 0.000 0.006 0.000 0.000 rms deviation 0.000 0.000 0.000 0.011 0.000 0.000 0.045 0.000 0.003 0.000 0.000 GooF = S = 1.114; Restrained GooF = 1.057 for 423 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 72.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22364 0.00094 0.000 OSF 2 0.85221 0.00236 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.003 for tors H35A_b Max. shift = 0.002 A for H35C_b Max. dU = 0.000 for C36_b Least-squares cycle 5 Maximum vector length = 511 Memory required = 6248 / 445571 wR2 = 0.2333 before cycle 5 for 3397 data and 352 / 352 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint -0.0180 0.0050 SIMU U33 Ru1_a Ru21_b Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 117. 0. 0. 6. 0. 300. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.100 0.000 0.006 0.000 0.000 rms deviation 0.000 0.000 0.000 0.011 0.000 0.000 0.045 0.000 0.003 0.000 0.000 GooF = S = 1.114; Restrained GooF = 1.057 for 423 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 72.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22364 0.00094 0.000 OSF 2 0.85221 0.00236 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.002 for tors H35A_b Max. shift = 0.001 A for H35A_b Max. dU = 0.000 for N22_b Least-squares cycle 6 Maximum vector length = 511 Memory required = 6248 / 445571 wR2 = 0.2333 before cycle 6 for 3397 data and 352 / 352 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint -0.0180 0.0050 SIMU U33 Ru1_a Ru21_b Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 117. 0. 0. 6. 0. 300. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.100 0.000 0.006 0.000 0.000 rms deviation 0.000 0.000 0.000 0.011 0.000 0.000 0.045 0.000 0.003 0.000 0.000 GooF = S = 1.115; Restrained GooF = 1.057 for 423 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 72.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22364 0.00094 0.000 OSF 2 0.85221 0.00236 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.001 for tors H35A_b Max. shift = 0.001 A for H35C_b Max. dU = 0.000 for C36_b Least-squares cycle 7 Maximum vector length = 511 Memory required = 6248 / 445571 wR2 = 0.2333 before cycle 7 for 3397 data and 352 / 352 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint -0.0180 0.0050 SIMU U33 Ru1_a Ru21_b Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 117. 0. 0. 6. 0. 300. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.100 0.000 0.006 0.000 0.000 rms deviation 0.000 0.000 0.000 0.011 0.000 0.000 0.045 0.000 0.003 0.000 0.000 GooF = S = 1.114; Restrained GooF = 1.057 for 423 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 72.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22364 0.00094 0.000 OSF 2 0.85221 0.00236 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.001 for z C35_b Max. shift = 0.000 A for H35A_b Max. dU = 0.000 for C36_b Least-squares cycle 8 Maximum vector length = 511 Memory required = 6248 / 445571 wR2 = 0.2333 before cycle 8 for 3397 data and 352 / 352 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint -0.0180 0.0050 SIMU U33 Ru1_a Ru21_b Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 117. 0. 0. 6. 0. 300. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.100 0.000 0.006 0.000 0.000 rms deviation 0.000 0.000 0.000 0.011 0.000 0.000 0.045 0.000 0.003 0.000 0.000 GooF = S = 1.114; Restrained GooF = 1.057 for 423 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 72.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22364 0.00094 0.000 OSF 2 0.85221 0.00236 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.001 for tors H35A_b Max. shift = 0.000 A for H35C_b Max. dU = 0.000 for C36_b Least-squares cycle 9 Maximum vector length = 511 Memory required = 6248 / 445571 wR2 = 0.2333 before cycle 9 for 3397 data and 352 / 352 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint -0.0180 0.0050 SIMU U33 Ru1_a Ru21_b Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 117. 0. 0. 6. 0. 300. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.100 0.000 0.006 0.000 0.000 rms deviation 0.000 0.000 0.000 0.011 0.000 0.000 0.045 0.000 0.003 0.000 0.000 GooF = S = 1.114; Restrained GooF = 1.057 for 423 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 72.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22364 0.00094 0.000 OSF 2 0.85221 0.00236 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z C35_b Max. shift = 0.000 A for H35A_b Max. dU = 0.000 for N22_b Least-squares cycle 10 Maximum vector length = 511 Memory required = 6248 / 445571 wR2 = 0.2333 before cycle 10 for 3397 data and 352 / 352 parameters Disagreeable restraints before cycle 10 Observed Target Error Sigma Restraint -0.0180 0.0050 SIMU U33 Ru1_a Ru21_b Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 117. 0. 0. 6. 0. 300. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.100 0.000 0.006 0.000 0.000 rms deviation 0.000 0.000 0.000 0.011 0.000 0.000 0.045 0.000 0.003 0.000 0.000 GooF = S = 1.114; Restrained GooF = 1.057 for 423 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 72.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22364 0.00094 0.000 OSF 2 0.85221 0.00236 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for y Ru1_a Max. shift = 0.000 A for H35C_b Max. dU = 0.000 for C36_b Least-squares cycle 11 Maximum vector length = 511 Memory required = 6248 / 445571 wR2 = 0.2333 before cycle 11 for 3397 data and 352 / 352 parameters Disagreeable restraints before cycle 11 Observed Target Error Sigma Restraint -0.0180 0.0050 SIMU U33 Ru1_a Ru21_b Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 117. 0. 0. 6. 0. 300. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.100 0.000 0.006 0.000 0.000 rms deviation 0.000 0.000 0.000 0.011 0.000 0.000 0.045 0.000 0.003 0.000 0.000 GooF = S = 1.114; Restrained GooF = 1.057 for 423 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 72.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22364 0.00094 0.000 OSF 2 0.85221 0.00236 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for y Ru1_a Max. shift = 0.000 A for H35A_b Max. dU = 0.000 for C36_b Least-squares cycle 12 Maximum vector length = 511 Memory required = 6248 / 445571 wR2 = 0.2333 before cycle 12 for 3397 data and 352 / 352 parameters Disagreeable restraints before cycle 12 Observed Target Error Sigma Restraint -0.0180 0.0050 SIMU U33 Ru1_a Ru21_b Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 117. 0. 0. 6. 0. 300. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.100 0.000 0.006 0.000 0.000 rms deviation 0.000 0.000 0.000 0.011 0.000 0.000 0.045 0.000 0.003 0.000 0.000 GooF = S = 1.114; Restrained GooF = 1.057 for 423 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 72.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22364 0.00094 0.000 OSF 2 0.85221 0.00236 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for y Ru1_a Max. shift = 0.000 A for H35C_b Max. dU = 0.000 for C16_a Least-squares cycle 13 Maximum vector length = 511 Memory required = 6248 / 445571 wR2 = 0.2333 before cycle 13 for 3397 data and 352 / 352 parameters Disagreeable restraints before cycle 13 Observed Target Error Sigma Restraint -0.0180 0.0050 SIMU U33 Ru1_a Ru21_b Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 117. 0. 0. 6. 0. 300. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.100 0.000 0.006 0.000 0.000 rms deviation 0.000 0.000 0.000 0.011 0.000 0.000 0.045 0.000 0.003 0.000 0.000 GooF = S = 1.114; Restrained GooF = 1.057 for 423 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 72.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22364 0.00094 0.000 OSF 2 0.85221 0.00236 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for y Ru1_a Max. shift = 0.000 A for H35A_b Max. dU = 0.000 for Ru21_b Least-squares cycle 14 Maximum vector length = 511 Memory required = 6248 / 445571 wR2 = 0.2333 before cycle 14 for 3397 data and 352 / 352 parameters Disagreeable restraints before cycle 14 Observed Target Error Sigma Restraint -0.0180 0.0050 SIMU U33 Ru1_a Ru21_b Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 117. 0. 0. 6. 0. 300. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.100 0.000 0.006 0.000 0.000 rms deviation 0.000 0.000 0.000 0.011 0.000 0.000 0.045 0.000 0.003 0.000 0.000 GooF = S = 1.114; Restrained GooF = 1.057 for 423 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 72.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22364 0.00094 0.000 OSF 2 0.85221 0.00236 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for y Ru1_a Max. shift = 0.000 A for H35C_b Max. dU = 0.000 for C36_b Least-squares cycle 15 Maximum vector length = 511 Memory required = 6248 / 445571 wR2 = 0.2333 before cycle 15 for 3397 data and 352 / 352 parameters Disagreeable restraints before cycle 15 Observed Target Error Sigma Restraint -0.0180 0.0050 SIMU U33 Ru1_a Ru21_b Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 117. 0. 0. 6. 0. 300. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.100 0.000 0.006 0.000 0.000 rms deviation 0.000 0.000 0.000 0.011 0.000 0.000 0.045 0.000 0.003 0.000 0.000 GooF = S = 1.114; Restrained GooF = 1.057 for 423 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 72.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22364 0.00094 0.000 OSF 2 0.85221 0.00236 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for y Ru1_a Max. shift = 0.000 A for H35B_b Max. dU = 0.000 for C36_b Least-squares cycle 16 Maximum vector length = 511 Memory required = 6248 / 445571 wR2 = 0.2333 before cycle 16 for 3397 data and 352 / 352 parameters Disagreeable restraints before cycle 16 Observed Target Error Sigma Restraint -0.0180 0.0050 SIMU U33 Ru1_a Ru21_b Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 117. 0. 0. 6. 0. 300. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.100 0.000 0.006 0.000 0.000 rms deviation 0.000 0.000 0.000 0.011 0.000 0.000 0.045 0.000 0.003 0.000 0.000 GooF = S = 1.114; Restrained GooF = 1.057 for 423 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 72.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22364 0.00094 0.000 OSF 2 0.85221 0.00236 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for y Ru1_a Max. shift = 0.000 A for H35C_b Max. dU = 0.000 for C35_b Least-squares cycle 17 Maximum vector length = 511 Memory required = 6248 / 445571 wR2 = 0.2333 before cycle 17 for 3397 data and 352 / 352 parameters Disagreeable restraints before cycle 17 Observed Target Error Sigma Restraint -0.0180 0.0050 SIMU U33 Ru1_a Ru21_b Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 117. 0. 0. 6. 0. 300. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.100 0.000 0.006 0.000 0.000 rms deviation 0.000 0.000 0.000 0.011 0.000 0.000 0.045 0.000 0.003 0.000 0.000 GooF = S = 1.114; Restrained GooF = 1.057 for 423 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 72.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22364 0.00094 0.000 OSF 2 0.85221 0.00236 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for y Ru1_a Max. shift = 0.000 A for H35B_b Max. dU = 0.000 for Ru21_b Least-squares cycle 18 Maximum vector length = 511 Memory required = 6248 / 445571 wR2 = 0.2333 before cycle 18 for 3397 data and 352 / 352 parameters Disagreeable restraints before cycle 18 Observed Target Error Sigma Restraint -0.0180 0.0050 SIMU U33 Ru1_a Ru21_b Summary of restraints applied in cycle 18 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 117. 0. 0. 6. 0. 300. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.100 0.000 0.006 0.000 0.000 rms deviation 0.000 0.000 0.000 0.011 0.000 0.000 0.045 0.000 0.003 0.000 0.000 GooF = S = 1.114; Restrained GooF = 1.057 for 423 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 72.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22364 0.00094 0.000 OSF 2 0.85221 0.00236 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for y Ru1_a Max. shift = 0.000 A for H35C_b Max. dU = 0.000 for C36_b Least-squares cycle 19 Maximum vector length = 511 Memory required = 6248 / 445571 wR2 = 0.2333 before cycle 19 for 3397 data and 352 / 352 parameters Disagreeable restraints before cycle 19 Observed Target Error Sigma Restraint -0.0180 0.0050 SIMU U33 Ru1_a Ru21_b Summary of restraints applied in cycle 19 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 117. 0. 0. 6. 0. 300. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.100 0.000 0.006 0.000 0.000 rms deviation 0.000 0.000 0.000 0.011 0.000 0.000 0.045 0.000 0.003 0.000 0.000 GooF = S = 1.114; Restrained GooF = 1.057 for 423 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 72.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22364 0.00094 0.000 OSF 2 0.85221 0.00236 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for y Ru1_a Max. shift = 0.000 A for H35C_b Max. dU = 0.000 for C35_b Least-squares cycle 20 Maximum vector length = 511 Memory required = 6248 / 445571 wR2 = 0.2333 before cycle 20 for 3397 data and 352 / 352 parameters Disagreeable restraints before cycle 20 Observed Target Error Sigma Restraint -0.0180 0.0050 SIMU U33 Ru1_a Ru21_b Summary of restraints applied in cycle 20 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 117. 0. 0. 6. 0. 300. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.100 0.000 0.006 0.000 0.000 rms deviation 0.000 0.000 0.000 0.011 0.000 0.000 0.045 0.000 0.003 0.000 0.000 GooF = S = 1.114; Restrained GooF = 1.057 for 423 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 72.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22364 0.00094 0.000 OSF 2 0.85221 0.00236 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for y Ru1_a Max. shift = 0.000 A for H35B_b Max. dU = 0.000 for C35_b Largest correlation matrix elements 0.869 U11 N22_b / U11 C34_b 0.850 U11 C23_b / U11 C22_b 0.840 U12 C25_b / U12 C24_b 0.862 U22 N22_b / U22 C34_b 0.849 U33 C24_b / U33 C23_b 0.840 U33 C23_b / U33 C22_b 0.861 U33 N22_b / U33 C34_b 0.849 U22 C25_b / U22 C24_b 0.839 U13 C25_b / U13 C24_b 0.858 U11 C24_b / U11 C23_b 0.845 U12 C24_b / U12 C23_b 0.835 U11 C34_b / U11 C22_b 0.855 U22 C24_b / U22 C23_b 0.845 U22 C23_b / U22 C22_b 0.835 U12 C23_b / U12 C22_b 0.854 U13 N22_b / U13 C34_b 0.845 U23 N22_b / U23 C34_b 0.834 U13 C23_b / U13 C22_b 0.853 U12 N22_b / U12 C34_b 0.844 U13 C24_b / U13 C23_b 0.833 U23 C24_b / U23 C23_b 0.852 U11 C25_b / U11 C24_b 0.844 U33 C25_b / U33 C24_b 0.829 U11 C25_b / U11 C21_b Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by ** Bond(s) to Ru1_a ignored in idealizing H-atoms attached to C3_a ** H3 -0.2019 0.8507 0.3448 43 0.950 0.000 C3_a C4_a C2_a ** Bond(s) to Ru1_a ignored in idealizing H-atoms attached to C4_a ** H4 -0.0641 0.9401 0.4136 43 0.950 0.000 C4_a C3_a C5_a ** Bond(s) to Ru1_a ignored in idealizing H-atoms attached to C5_a ** H5 0.1579 0.8522 0.4622 43 0.950 0.000 C5_a C4_a C1_a ** Bond(s) to Ru1_a ignored in idealizing H-atoms attached to C6_a ** H6 0.4758 0.7645 0.3258 43 0.950 0.000 C6_a C7_a C10_a ** Bond(s) to Ru1_a ignored in idealizing H-atoms attached to C7_a ** H7 0.2486 0.7711 0.2551 43 0.950 0.000 C7_a C6_a C8_a ** Bond(s) to Ru1_a ignored in idealizing H-atoms attached to C8_a ** H8 0.1214 0.9239 0.2546 43 0.950 0.000 C8_a C9_a C7_a ** Bond(s) to Ru1_a ignored in idealizing H-atoms attached to C9_a ** H9 0.2715 1.0084 0.3232 43 0.950 0.000 C9_a C8_a C10_a ** Bond(s) to Ru1_a ignored in idealizing H-atoms attached to C10_a ** H10 0.5024 0.9168 0.3658 43 0.950 0.000 C10_a C9_a C6_a H11A 0.3046 0.6966 0.4426 23 0.990 0.000 C11_a C1_a N1_a H11B 0.2337 0.6413 0.3948 23 0.990 0.000 C11_a C1_a N1_a H12A 0.2568 0.5121 0.4404 137 0.980 0.000 C12_a N1_a H12A_a H12B 0.1616 0.4972 0.4948 137 0.980 0.000 C12_a N1_a H12A_a H12C 0.3280 0.5581 0.4917 137 0.980 0.000 C12_a N1_a H12A_a H13A 0.0214 0.6151 0.5361 137 0.980 0.000 C13_a N1_a H13A_a H13B -0.0057 0.7039 0.5055 137 0.980 0.000 C13_a N1_a H13A_a H13C 0.1813 0.6787 0.5272 137 0.980 0.000 C13_a N1_a H13A_a H14A -0.0680 0.6832 0.2972 23 0.990 0.000 C14_a N2_a C2_a H14B -0.0161 0.6181 0.3431 23 0.990 0.000 C14_a N2_a C2_a H15A -0.2148 0.5806 0.4047 137 0.980 0.000 C15_a N2_a H15A_a H15B -0.4168 0.5986 0.3976 137 0.980 0.000 C15_a N2_a H15A_a H15C -0.2925 0.6735 0.4183 137 0.980 0.000 C15_a N2_a H15A_a H16A -0.2897 0.5998 0.2722 137 0.980 0.000 C16_a N2_a H16A_a H16B -0.4412 0.5700 0.3105 137 0.980 0.000 C16_a N2_a H16A_a H16C -0.2520 0.5300 0.3165 137 0.980 0.000 C16_a N2_a H16A_a ** Bond(s) to Ru21_b ignored in idealizing H-atoms attached to C23_b ** H23 0.7076 0.8482 0.3460 43 0.950 0.000 C23_b C24_b C22_b ** Bond(s) to Ru21_b ignored in idealizing H-atoms attached to C24_b ** H24 0.5674 0.9364 0.4148 43 0.950 0.000 C24_b C23_b C25_b ** Bond(s) to Ru21_b ignored in idealizing H-atoms attached to C25_b ** H25 0.3455 0.8469 0.4625 43 0.950 0.000 C25_b C24_b C21_b ** Bond(s) to Ru21_b ignored in idealizing H-atoms attached to C26_b ** H26 0.0271 0.7650 0.3253 43 0.950 0.000 C26_b C27_b C30_b ** Bond(s) to Ru21_b ignored in idealizing H-atoms attached to C27_b ** H27 0.2544 0.7716 0.2545 43 0.950 0.000 C27_b C26_b C28_b ** Bond(s) to Ru21_b ignored in idealizing H-atoms attached to C28_b ** H28 0.3882 0.9228 0.2550 43 0.950 0.000 C28_b C29_b C27_b ** Bond(s) to Ru21_b ignored in idealizing H-atoms attached to C29_b ** H29 0.2399 1.0084 0.3236 43 0.950 0.000 C29_b C28_b C30_b ** Bond(s) to Ru21_b ignored in idealizing H-atoms attached to C30_b ** H30 0.0051 0.9186 0.3654 43 0.950 0.000 C30_b C29_b C26_b H31A 0.2671 0.6384 0.3935 23 0.990 0.000 C31_b C21_b N21_b H31B 0.1993 0.6925 0.4423 23 0.990 0.000 C31_b C21_b N21_b H32A 0.3212 0.6676 0.5268 137 0.980 0.000 C32_b N21_b H32A_b H32B 0.4979 0.7050 0.5038 137 0.980 0.000 C32_b N21_b H32A_b H32C 0.4962 0.6137 0.5327 137 0.980 0.000 C32_b N21_b H32A_b H33A 0.3536 0.4935 0.4922 137 0.980 0.000 C33_b N21_b H33A_b H33B 0.2640 0.5062 0.4367 137 0.980 0.000 C33_b N21_b H33A_b H33C 0.1829 0.5510 0.4871 137 0.980 0.000 C33_b N21_b H33A_b H34A 0.5091 0.6217 0.3341 23 0.990 0.000 C34_b N22_b C22_b H34B 0.5671 0.6935 0.2928 23 0.990 0.000 C34_b N22_b C22_b H35A 0.9350 0.7190 0.2999 137 0.980 0.000 C35_b N22_b H35A_b H35B 0.9830 0.6979 0.3590 137 0.980 0.000 C35_b N22_b H35A_b H35C 0.8350 0.7666 0.3461 137 0.980 0.000 C35_b N22_b H35A_b H36A 0.7118 0.5891 0.2680 137 0.980 0.000 C36_b N22_b H36A_b H36B 0.7974 0.5260 0.3098 137 0.980 0.000 C36_b N22_b H36A_b H36C 0.9141 0.5952 0.2799 137 0.980 0.000 C36_b N22_b H36A_b 2005src0328 in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1_a 0.08858 0.74693 0.41022 0.85221 0.02107 0.02332 0.01316 0.00109 0.00100 -0.00076 0.01918 0.02013 0.00151 0.00076 0.00043 0.00236 0.00341 0.00355 0.00333 0.00317 0.00311 0.00332 0.00174 C2_a -0.03490 0.74769 0.36937 0.85221 0.02091 0.02278 0.01660 -0.00163 0.00150 -0.00117 0.02010 0.02001 0.00152 0.00076 0.00044 0.00236 0.00359 0.00361 0.00349 0.00324 0.00318 0.00335 0.00179 C3_a -0.11376 0.83232 0.36788 0.85221 0.01938 0.02443 0.01583 0.00118 0.00674 0.00505 0.01988 0.02016 0.00146 0.00076 0.00042 0.00236 0.00404 0.00418 0.00382 0.00360 0.00341 0.00376 0.00199 H3_a -0.20191 0.85072 0.34475 0.85221 0.02385 0.00236 0.00000 C4_a -0.03667 0.88164 0.40655 0.85221 0.02213 0.02471 0.01270 0.00291 0.00407 0.00348 0.01985 0.02075 0.00154 0.00078 0.00045 0.00236 0.00417 0.00426 0.00391 0.00364 0.00360 0.00383 0.00201 H4_a -0.06414 0.94014 0.41358 0.85221 0.02382 0.00236 0.00000 C5_a 0.08837 0.83305 0.43408 0.85221 0.02276 0.02431 0.00917 0.00117 0.00358 0.00164 0.01874 0.02037 0.00152 0.00076 0.00042 0.00236 0.00387 0.00413 0.00370 0.00361 0.00347 0.00380 0.00192 H5_a 0.15786 0.85220 0.46221 0.85221 0.02249 0.00236 0.00000 C6_a 0.41023 0.81376 0.31635 0.85221 0.02022 0.02586 0.02512 0.00909 0.00716 -0.00284 0.02373 0.02158 0.00156 0.00078 0.00048 0.00236 0.00326 0.00330 0.00327 0.00314 0.00314 0.00311 0.00172 H6_a 0.47580 0.76445 0.32578 0.85221 0.02848 0.00236 0.00000 C7_a 0.28185 0.81728 0.27722 0.85221 0.02188 0.02616 0.02319 0.00469 0.00642 -0.00342 0.02375 0.02089 0.00154 0.00076 0.00044 0.00236 0.00351 0.00328 0.00315 0.00299 0.00312 0.00316 0.00175 H7_a 0.24861 0.77115 0.25513 0.85221 0.02849 0.00236 0.00000 C8_a 0.21028 0.90325 0.27677 0.85221 0.01946 0.02445 0.02047 0.00685 0.00659 -0.00471 0.02146 0.01987 0.00145 0.00075 0.00042 0.00236 0.00352 0.00322 0.00309 0.00296 0.00306 0.00313 0.00171 H8_a 0.12143 0.92387 0.25458 0.85221 0.02575 0.00236 0.00000 C9_a 0.29560 0.94999 0.31479 0.85221 0.01859 0.02325 0.02147 0.00738 0.00621 -0.00666 0.02110 0.02030 0.00145 0.00077 0.00045 0.00236 0.00347 0.00331 0.00321 0.00298 0.00311 0.00310 0.00173 H9_a 0.27153 1.00837 0.32321 0.85221 0.02532 0.00236 0.00000 C10_a 0.42391 0.89897 0.33953 0.85221 0.01597 0.02379 0.02702 0.00772 0.00592 -0.00575 0.02226 0.02114 0.00152 0.00077 0.00048 0.00236 0.00322 0.00331 0.00334 0.00310 0.00311 0.00306 0.00172 H10_a 0.50237 0.91682 0.36577 0.85221 0.02671 0.00236 0.00000 C11_a 0.19855 0.67371 0.42621 0.85221 0.01736 0.02135 0.01425 0.00323 0.00265 -0.00090 0.01765 0.02173 0.00150 0.00076 0.00046 0.00236 0.00380 0.00385 0.00336 0.00315 0.00336 0.00344 0.00186 H11A_a 0.30460 0.69662 0.44263 0.85221 0.02118 0.00236 0.00000 H11B_a 0.23367 0.64134 0.39480 0.85221 0.02118 0.00236 0.00000 C12_a 0.22395 0.53909 0.47334 0.85221 0.02750 0.02386 0.01669 -0.00190 0.00536 0.00262 0.02268 0.02630 0.00187 0.00090 0.00056 0.00236 0.00660 0.00579 0.00548 0.00469 0.00556 0.00537 0.00297 H12A_a 0.25680 0.51215 0.44036 0.85221 0.03402 0.00236 0.00000 H12B_a 0.16159 0.49722 0.49479 0.85221 0.03402 0.00236 0.00000 H12C_a 0.32796 0.55814 0.49172 0.85221 0.03402 0.00236 0.00000 C13_a 0.07442 0.65619 0.51197 0.85221 0.02673 0.03074 0.01599 -0.00232 0.00717 0.00799 0.02449 0.02462 0.00177 0.00099 0.00046 0.00236 0.00601 0.00629 0.00573 0.00600 0.00513 0.00619 0.00275 H13A_a 0.02137 0.61514 0.53609 0.85221 0.03673 0.00236 0.00000 H13B_a -0.00566 0.70388 0.50548 0.85221 0.03673 0.00236 0.00000 H13C_a 0.18127 0.67872 0.52716 0.85221 0.03673 0.00236 0.00000 C14_a -0.08706 0.66909 0.33423 0.85221 0.02661 0.02480 0.02352 -0.00558 -0.00180 -0.00020 0.02498 0.02379 0.00174 0.00096 0.00055 0.00236 0.00416 0.00415 0.00410 0.00389 0.00377 0.00402 0.00210 H14A_a -0.06799 0.68323 0.29717 0.85221 0.02998 0.00236 0.00000 H14B_a -0.01608 0.61813 0.34311 0.85221 0.02998 0.00236 0.00000 C15_a -0.30119 0.62379 0.39491 0.85221 0.03968 0.02305 0.04015 -0.01065 0.00501 -0.01515 0.03430 0.02396 0.00197 0.00092 0.00055 0.00236 0.00758 0.00637 0.00703 0.00583 0.00637 0.00586 0.00339 H15A_a -0.21480 0.58062 0.40470 0.85221 0.05144 0.00236 0.00000 H15B_a -0.41684 0.59860 0.39760 0.85221 0.05144 0.00236 0.00000 H15C_a -0.29250 0.67348 0.41826 0.85221 0.05144 0.00236 0.00000 C16_a -0.31736 0.58205 0.30781 0.85221 0.04013 0.03710 0.04164 -0.00448 -0.00241 -0.01049 0.03962 0.02475 0.00220 0.00099 0.00059 0.00236 0.00740 0.00723 0.00743 0.00630 0.00698 0.00681 0.00349 H16A_a -0.28973 0.59985 0.27224 0.85221 0.05943 0.00236 0.00000 H16B_a -0.44123 0.57004 0.31049 0.85221 0.05943 0.00236 0.00000 H16C_a -0.25196 0.52996 0.31652 0.85221 0.05943 0.00236 0.00000 N1_a 0.11348 0.61286 0.46319 0.85221 0.01637 0.02292 0.01139 0.00042 0.00655 0.00484 0.01690 0.01843 0.00130 0.00068 0.00039 0.00236 0.00399 0.00404 0.00368 0.00341 0.00342 0.00353 0.00189 N2_a -0.27171 0.65057 0.34358 0.85221 0.03149 0.02640 0.03111 -0.00919 -0.00098 -0.00391 0.02966 0.02093 0.00165 0.00092 0.00053 0.00236 0.00450 0.00430 0.00459 0.00408 0.00412 0.00419 0.00224 Ru1_a 0.16311 0.84241 0.35211 0.85221 0.01962 0.02257 0.01224 0.00227 0.00140 0.00005 0.01814 0.00186 0.00014 0.00007 0.00004 0.00236 0.00051 0.00054 0.00046 0.00056 0.00056 0.00058 0.00030 C21_b 0.41349 0.74369 0.40913 0.14779 0.02203 0.01900 0.01915 0.00386 0.00055 -0.00330 0.02006 0.05506 0.00395 0.00167 0.00104 0.00236 0.00683 0.00673 0.00655 0.00619 0.00650 0.00654 0.00360 C22_b 0.53801 0.74508 0.36876 0.14779 0.02313 0.01775 0.02062 0.00494 -0.00093 -0.00545 0.02050 0.05442 0.00340 0.00166 0.00118 0.00236 0.00777 0.00762 0.00750 0.00704 0.00734 0.00736 0.00409 C23_b 0.61801 0.82948 0.36859 0.14779 0.02361 0.01805 0.02045 0.00541 -0.00157 -0.00564 0.02070 0.04980 0.00249 0.00206 0.00136 0.00236 0.00835 0.00823 0.00809 0.00765 0.00792 0.00796 0.00444 H23_b 0.70756 0.84818 0.34604 0.14779 0.02484 0.00236 0.00000 C24_b 0.54027 0.87802 0.40729 0.14779 0.02344 0.01812 0.01991 0.00463 -0.00049 -0.00512 0.02049 0.03488 0.00386 0.00202 0.00120 0.00236 0.00839 0.00829 0.00815 0.00774 0.00800 0.00804 0.00448 H24_b 0.56743 0.93640 0.41480 0.14779 0.02459 0.00236 0.00000 C25_b 0.41476 0.82867 0.43413 0.14779 0.02287 0.01868 0.01948 0.00417 -0.00024 -0.00388 0.02035 0.04995 0.00454 0.00214 0.00076 0.00236 0.00792 0.00784 0.00768 0.00730 0.00758 0.00762 0.00423 H25_b 0.34552 0.84690 0.46253 0.14779 0.02442 0.00236 0.00000 C26_b 0.09398 0.81394 0.31600 0.14779 0.01964 0.02410 0.01669 0.00346 0.00384 -0.00231 0.02014 0.04584 0.00326 0.00237 0.00147 0.00236 0.00350 0.00345 0.00341 0.00340 0.00344 0.00345 0.00197 H26_b 0.02715 0.76500 0.32532 0.14779 0.02417 0.00236 0.00000 C27_b 0.22274 0.81760 0.27697 0.14779 0.02002 0.02502 0.02041 0.00487 0.00567 -0.00384 0.02182 0.04579 0.00482 0.00240 0.00094 0.00236 0.00375 0.00353 0.00344 0.00335 0.00350 0.00352 0.00196 H27_b 0.25440 0.77164 0.25453 0.14779 0.02618 0.00236 0.00000 C28_b 0.29798 0.90292 0.27695 0.14779 0.01995 0.02455 0.02102 0.00591 0.00603 -0.00464 0.02184 0.06600 0.00455 0.00247 0.00096 0.00236 0.00366 0.00343 0.00332 0.00321 0.00338 0.00339 0.00188 H28_b 0.38816 0.92277 0.25499 0.14779 0.02621 0.00236 0.00000 C29_b 0.21387 0.95033 0.31497 0.14779 0.01919 0.02371 0.01996 0.00603 0.00566 -0.00439 0.02095 0.06231 0.00443 0.00176 0.00140 0.00236 0.00375 0.00355 0.00347 0.00336 0.00352 0.00353 0.00197 H29_b 0.23986 1.00843 0.32357 0.14779 0.02514 0.00236 0.00000 C30_b 0.08344 0.90009 0.33931 0.14779 0.01920 0.02314 0.01674 0.00419 0.00391 -0.00202 0.01970 0.06563 0.00309 0.00250 0.00142 0.00236 0.00349 0.00345 0.00342 0.00340 0.00345 0.00345 0.00197 H30_b 0.00515 0.91858 0.36543 0.14779 0.02363 0.00236 0.00000 C31_b 0.30414 0.67035 0.42488 0.14779 0.02032 0.02061 0.01751 0.00279 0.00182 -0.00037 0.01948 0.07136 0.00523 0.00236 0.00170 0.00236 0.00551 0.00541 0.00511 0.00487 0.00527 0.00530 0.00287 H31A_b 0.26715 0.63844 0.39350 0.14779 0.02338 0.00236 0.00000 H31B_b 0.19927 0.69252 0.44232 0.14779 0.02338 0.00236 0.00000 C32_b 0.43064 0.65251 0.51006 0.14779 0.02122 0.02069 0.02014 0.00194 0.00146 0.00342 0.02068 0.08750 0.00875 0.00416 0.00180 0.00236 0.01157 0.01152 0.01142 0.01132 0.01131 0.01151 0.00637 H32A_b 0.32119 0.66764 0.52682 0.14779 0.03103 0.00236 0.00000 H32B_b 0.49787 0.70498 0.50379 0.14779 0.03103 0.00236 0.00000 H32C_b 0.49616 0.61371 0.53271 0.14779 0.03103 0.00236 0.00000 C33_b 0.29059 0.53396 0.46992 0.14779 0.02403 0.02245 0.01832 0.00109 0.00328 0.00346 0.02160 0.10764 0.00921 0.00308 0.00286 0.00236 0.00902 0.00825 0.00809 0.00778 0.00855 0.00842 0.00469 H33A_b 0.35359 0.49349 0.49215 0.14779 0.03241 0.00236 0.00000 H33B_b 0.26403 0.50624 0.43667 0.14779 0.03241 0.00236 0.00000 H33C_b 0.18293 0.55098 0.48708 0.14779 0.03241 0.00236 0.00000 C34_b 0.58513 0.67218 0.32868 0.14779 0.02342 0.01670 0.02221 0.00546 -0.00128 -0.00698 0.02077 0.06858 0.00496 0.00259 0.00190 0.00236 0.00891 0.00871 0.00864 0.00813 0.00842 0.00841 0.00472 H34A_b 0.50914 0.62169 0.33413 0.14779 0.02493 0.00236 0.00000 H34B_b 0.56712 0.69349 0.29285 0.14779 0.02493 0.00236 0.00000 C35_b 0.88891 0.71243 0.33508 0.14779 0.02393 0.01395 0.02903 0.00196 -0.00372 -0.01161 0.02230 0.09352 0.00668 0.00401 0.00303 0.00236 0.01365 0.01333 0.01346 0.01287 0.01301 0.01299 0.00742 H35A_b 0.93500 0.71896 0.29985 0.14779 0.03345 0.00236 0.00000 H35B_b 0.98302 0.69792 0.35897 0.14779 0.03345 0.00236 0.00000 H35C_b 0.83500 0.76658 0.34605 0.14779 0.03345 0.00236 0.00000 C36_b 0.80011 0.58420 0.29503 0.14779 0.02272 0.01825 0.02568 0.00455 0.00003 -0.01073 0.02222 0.10104 0.00726 0.00374 0.00267 0.00236 0.01369 0.01338 0.01341 0.01276 0.01301 0.01300 0.00740 H36A_b 0.71175 0.58914 0.26795 0.14779 0.03332 0.00236 0.00000 H36B_b 0.79744 0.52601 0.30979 0.14779 0.03332 0.00236 0.00000 H36C_b 0.91410 0.59519 0.27991 0.14779 0.03332 0.00236 0.00000 N21_b 0.39602 0.60975 0.46084 0.14779 0.02091 0.02083 0.01850 0.00238 0.00152 0.00090 0.02008 0.07723 0.00585 0.00229 0.00160 0.00236 0.00679 0.00665 0.00643 0.00621 0.00656 0.00657 0.00362 N22_b 0.76610 0.64673 0.33562 0.14779 0.02330 0.01569 0.02414 0.00474 -0.00076 -0.00848 0.02105 0.08190 0.00538 0.00319 0.00225 0.00236 0.00997 0.00968 0.00968 0.00908 0.00937 0.00936 0.00530 Ru21_b 0.34151 0.84112 0.35222 0.14779 0.01499 0.01885 0.03028 0.00213 0.00319 -0.00086 0.02137 0.01105 0.00079 0.00040 0.00025 0.00236 0.00230 0.00237 0.00243 0.00251 0.00249 0.00237 0.00136 Final Structure Factor Calculation for 2005src0328 in Pbca Total number of l.s. parameters = 352 Maximum vector length = 511 Memory required = 5896 / 22995 wR2 = 0.2333 before cycle 21 for 3397 data and 0 / 352 parameters Disagreeable restraints before cycle 21 Observed Target Error Sigma Restraint -0.0180 0.0050 SIMU U33 Ru1_a Ru21_b Summary of restraints applied in cycle 21 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 117. 0. 0. 6. 0. 300. 0. 0. rms sigma 0.000 0.000 0.000 0.033 0.000 0.000 0.100 0.000 0.006 0.000 0.000 rms deviation 0.000 0.000 0.000 0.011 0.000 0.000 0.045 0.000 0.003 0.000 0.000 GooF = S = 1.114; Restrained GooF = 1.057 for 423 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 72.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 RMS deviation from FLAT planes = 0.0085 for 12 atoms R1 = 0.1089 for 1750 Fo > 4sig(Fo) and 0.2192 for all 3397 data wR2 = 0.2333, GooF = S = 1.114, Restrained GooF = 1.057 for all data Occupancy sum of asymmetric unit = 19.00 for non-hydrogen and 24.00 for hydrogen atoms Principal mean square atomic displacements U 0.0236 0.0210 0.0129 C1_a 0.0240 0.0204 0.0159 C2_a 0.0293 0.0200 0.0103 C3_a 0.0286 0.0200 0.0110 C4_a 0.0259 0.0221 0.0082 C5_a 0.0353 0.0251 0.0108 C6_a 0.0300 0.0278 0.0135 C7_a 0.0296 0.0257 0.0090 C8_a 0.0299 0.0259 0.0075 C9_a 0.0334 0.0249 0.0085 C10_a 0.0226 0.0187 0.0116 C11_a 0.0302 0.0241 0.0137 C12_a 0.0373 0.0255 0.0107 C13_a 0.0301 0.0265 0.0183 C14_a 0.0553 0.0352 0.0123 C15_a 0.0494 0.0431 0.0264 C16_a 0.0264 0.0178 0.0065 N1_a 0.0386 0.0321 0.0182 N2_a 0.0231 0.0198 0.0115 Ru1_a 0.0248 0.0212 0.0142 C21_b 0.0282 0.0208 0.0125 C22_b 0.0293 0.0203 0.0125 C23_b 0.0277 0.0209 0.0129 C24_b 0.0262 0.0209 0.0140 C25_b 0.0256 0.0223 0.0126 C26_b 0.0281 0.0256 0.0117 C27_b 0.0290 0.0261 0.0105 C28_b 0.0282 0.0247 0.0100 C29_b 0.0252 0.0219 0.0120 C30_b 0.0225 0.0207 0.0153 C31_b 0.0255 0.0192 0.0174 C32_b 0.0279 0.0201 0.0168 C33_b 0.0301 0.0214 0.0108 C34_b 0.0347 0.0259 0.0063 C35_b 0.0327 0.0252 0.0088 C36_b 0.0234 0.0200 0.0168 N21_b 0.0306 0.0233 0.0093 N22_b 0.0312 0.0189 0.0140 Ru21_b Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.020 0.031 0.044 0.059 0.080 0.103 0.138 0.199 1.000 Number in group 381. 321. 320. 345. 347. 338. 331. 333. 341. 340. GooF 1.193 1.157 1.257 1.204 1.032 1.088 1.045 1.102 0.919 1.108 K 42.152 7.147 2.959 2.690 1.359 1.159 1.119 1.037 1.017 0.979 Resolution(A) 0.77 0.80 0.84 0.88 0.93 0.98 1.06 1.17 1.33 1.67 inf Number in group 342. 337. 345. 343. 331. 346. 340. 337. 335. 341. GooF 0.997 1.136 1.007 1.011 1.068 1.050 1.031 1.134 1.205 1.437 K 1.142 1.148 1.183 1.274 1.100 1.122 1.075 1.042 1.031 0.992 R1 0.428 0.419 0.359 0.314 0.231 0.211 0.161 0.134 0.094 0.071 Recommended weighting scheme: WGHT 0.0001 72.2574 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 5 263.71 7904.91 7.85 0.214 0.83 3 2 7 2501.33 112.51 7.57 0.026 2.04 3 6 2 2083.04 154.41 6.37 0.030 1.81 3 0 12 3108.88 273.17 6.05 0.040 1.65 1 1 2 20011.29 32314.75 5.61 0.433 6.10 6 16 0 -286.50 3793.66 5.30 0.148 0.78 3 6 8 1241.29 46.02 4.92 0.016 1.59 3 0 2 2041.72 533.92 4.58 0.056 2.53 3 2 3 2857.21 1091.18 4.47 0.080 2.36 0 16 8 -171.34 2050.67 4.06 0.109 0.93 2 15 6 288.30 3011.49 4.04 0.132 0.97 3 8 13 1219.38 7.86 3.71 0.007 1.22 3 0 8 4779.70 2635.21 3.70 0.124 2.01 3 8 3 1839.83 561.92 3.65 0.057 1.53 3 2 11 1967.46 697.01 3.52 0.064 1.69 3 5 3 743.81 73.04 3.44 0.021 1.93 6 14 0 365.08 2411.49 3.34 0.118 0.84 3 8 7 4115.59 2276.63 3.27 0.115 1.43 3 4 7 5821.89 3757.14 3.23 0.148 1.86 3 6 6 913.91 133.00 3.22 0.028 1.68 3 4 12 1927.36 731.51 3.20 0.065 1.52 3 2 17 1236.95 202.56 3.19 0.034 1.29 3 0 6 1067.07 259.16 3.14 0.039 2.21 2 10 17 395.92 1832.83 3.10 0.103 1.04 3 6 9 821.67 3.49 3.09 0.005 1.54 3 2 13 1576.11 581.76 2.99 0.058 1.54 3 6 16 890.77 2.04 2.94 0.003 1.21 2 4 7 567.87 41.98 2.92 0.016 2.20 1 6 15 797.02 1.85 2.84 0.003 1.41 0 12 4 11028.52 15520.75 2.83 0.300 1.27 1 13 14 1287.67 0.81 2.80 0.002 0.99 3 10 2 711.14 6.24 2.78 0.006 1.32 3 6 28 2123.28 27.87 2.78 0.013 0.82 4 12 10 3929.48 1815.28 2.77 0.103 0.99 4 2 2 344.46 5.92 2.74 0.006 1.86 5 9 14 1009.54 6.49 2.73 0.006 0.98 0 6 17 1321.23 39.13 2.72 0.015 1.31 4 0 2 456.62 5.85 2.70 0.006 1.92 2 2 15 5144.33 3457.65 2.67 0.142 1.54 2 13 21 3106.16 1116.29 2.66 0.081 0.84 3 4 16 1173.69 224.65 2.66 0.036 1.29 8 8 1 1686.84 251.84 2.62 0.038 0.87 2 8 25 3163.32 1226.26 2.61 0.084 0.89 8 8 2 1076.84 0.01 2.60 0.000 0.86 1 2 2 8874.11 6787.42 2.59 0.199 5.04 3 0 16 1267.24 310.12 2.57 0.042 1.37 3 2 1 1333.69 629.75 2.57 0.060 2.44 2 3 4 757.11 208.14 2.57 0.035 2.79 3 4 13 837.97 176.74 2.54 0.032 1.46 1 6 29 2710.21 0.38 2.54 0.001 0.83 Bond lengths and angles C1_a - Distance Angles C2_a 1.4217 (0.0141) C5_a 1.4710 (0.0146) 107.50 (0.96) C11_a 1.4787 (0.0154) 126.86 (1.06) 125.63 (1.02) Ru1_a 2.1834 (0.0114) 70.46 (0.61) 70.72 (0.61) 124.05 (0.80) C1_a - C2_a C5_a C11_a C2_a - Distance Angles C1_a 1.4217 (0.0141) C3_a 1.4491 (0.0146) 108.10 (0.97) C14_a 1.5715 (0.0174) 126.33 (1.09) 125.44 (1.06) Ru1_a 2.1707 (0.0117) 71.43 (0.62) 71.26 (0.62) 126.12 (0.81) C2_a - C1_a C3_a C14_a C3_a - Distance Angles C4_a 1.3904 (0.0140) C2_a 1.4491 (0.0146) 107.39 (0.97) Ru1_a 2.1887 (0.0114) 70.88 (0.66) 69.91 (0.59) H3_a 0.9500 126.30 126.30 124.52 C3_a - C4_a C2_a Ru1_a C4_a - Distance Angles C3_a 1.3904 (0.0140) C5_a 1.4176 (0.0141) 111.02 (1.03) Ru1_a 2.1749 (0.0119) 71.96 (0.65) 71.77 (0.66) H4_a 0.9500 124.49 124.49 123.35 C4_a - C3_a C5_a Ru1_a C5_a - Distance Angles C4_a 1.4176 (0.0141) C1_a 1.4710 (0.0146) 105.97 (0.97) Ru1_a 2.1932 (0.0109) 70.36 (0.64) 70.00 (0.59) H5_a 0.9500 127.01 127.01 124.28 C5_a - C4_a C1_a Ru1_a C6_a - Distance Angles C7_a 1.4165 (0.0146) C10_a 1.4547 (0.0152) 107.93 (1.02) Ru1_a 2.1703 (0.0123) 71.00 (0.64) 72.78 (0.67) H6_a 0.9500 126.04 126.04 121.89 C6_a - C7_a C10_a Ru1_a C7_a - Distance Angles C6_a 1.4165 (0.0146) C8_a 1.4449 (0.0146) 108.11 (1.00) Ru1_a 2.1715 (0.0111) 70.92 (0.62) 71.26 (0.59) H7_a 0.9500 125.94 125.94 123.51 C7_a - C6_a C8_a Ru1_a C8_a - Distance Angles C9_a 1.3862 (0.0138) C7_a 1.4449 (0.0146) 107.12 (0.98) Ru1_a 2.1880 (0.0106) 71.30 (0.63) 70.03 (0.59) H8_a 0.9500 126.44 126.44 123.88 C8_a - C9_a C7_a Ru1_a C9_a - Distance Angles C8_a 1.3862 (0.0137) C10_a 1.4215 (0.0142) 111.00 (1.05) Ru1_a 2.1826 (0.0112) 71.72 (0.63) 72.87 (0.66) H9_a 0.9500 124.50 124.50 122.47 C9_a - C8_a C10_a Ru1_a C10_a - Distance Angles C9_a 1.4215 (0.0142) C6_a 1.4547 (0.0152) 105.76 (1.01) Ru1_a 2.2265 (0.0119) 69.53 (0.64) 68.60 (0.65) H10_a 0.9500 127.12 127.12 126.30 C10_a - C9_a C6_a Ru1_a C11_a - Distance Angles C1_a 1.4787 (0.0154) N1_a 1.4942 (0.0141) 114.14 (0.94) H11A_a 0.9900 108.72 108.72 H11B_a 0.9900 108.72 108.72 107.63 C11_a - C1_a N1_a H11A_a C12_a - Distance Angles N1_a 1.4531 (0.0164) H12A_a 0.9800 109.47 H12B_a 0.9800 109.47 109.47 H12C_a 0.9800 109.47 109.47 109.47 C12_a - N1_a H12A_a H12B_a C13_a - Distance Angles N1_a 1.4562 (0.0150) H13A_a 0.9800 109.47 H13B_a 0.9800 109.47 109.47 H13C_a 0.9800 109.47 109.47 109.47 C13_a - N1_a H13A_a H13B_a C14_a - Distance Angles N2_a 1.4788 (0.0185) C2_a 1.5715 (0.0174) 107.81 (1.12) H14A_a 0.9900 110.14 110.14 H14B_a 0.9900 110.14 110.14 108.45 C14_a - N2_a C2_a H14A_a C15_a - Distance Angles N2_a 1.4040 (0.0195) H15A_a 0.9800 109.47 H15B_a 0.9800 109.47 109.47 H15C_a 0.9800 109.47 109.47 109.47 C15_a - N2_a H15A_a H15B_a C16_a - Distance Angles N2_a 1.4506 (0.0164) H16A_a 0.9800 109.47 H16B_a 0.9800 109.47 109.47 H16C_a 0.9800 109.47 109.47 109.47 C16_a - N2_a H16A_a H16B_a N1_a - Distance Angles C12_a 1.4531 (0.0165) C13_a 1.4562 (0.0150) 109.34 (0.99) C11_a 1.4942 (0.0141) 110.66 (0.95) 110.44 (1.03) N1_a - C12_a C13_a N2_a - Distance Angles C15_a 1.4040 (0.0194) C16_a 1.4506 (0.0164) 109.94 (1.30) C14_a 1.4788 (0.0185) 111.60 (1.26) 105.96 (1.18) N2_a - C15_a C16_a Ru1_a - Distance Angles C6_a 2.1703 (0.0124) C2_a 2.1707 (0.0118) 124.85 (0.45) C7_a 2.1715 (0.0111) 38.08 (0.40) 111.07 (0.47) C4_a 2.1749 (0.0119) 163.42 (0.46) 63.56 (0.43) 157.50 (0.45) C9_a 2.1826 (0.0112) 63.59 (0.43) 160.13 (0.44) 63.09 (0.42) 113.84 (0.49) C1_a 2.1834 (0.0114) 112.64 (0.48) 38.11 (0.38) 126.76 (0.43) 63.91 (0.43) 160.92 (0.43) C8_a 2.1880 (0.0106) 64.22 (0.42) 126.28 (0.42) 38.71 (0.39) 124.70 (0.43) 36.98 (0.36) 160.81 (0.43) C3_a 2.1887 (0.0115) 158.20 (0.45) 38.83 (0.40) 124.54 (0.43) 37.16 (0.37) 126.68 (0.44) 64.22 (0.41) 111.04 (0.45) C5_a 2.1932 (0.0109) 128.87 (0.45) 64.63 (0.42) 162.60 (0.44) 37.87 (0.37) 126.75 (0.44) 39.28 (0.39) 157.78 (0.44) C10_a 2.2265 (0.0121) 38.61 (0.40) 159.72 (0.44) 63.72 (0.43) 128.99 (0.45) 37.60 (0.37) 127.39 (0.43) 63.22 (0.41) Ru1_a - C6_a C2_a C7_a C4_a C9_a C1_a C8_a C21_b - Distance Angles C22_b 1.4180 (0.0189) C25_b 1.4676 (0.0196) 107.64 (1.51) C31_b 1.4757 (0.0217) 127.14 (2.36) 125.20 (2.33) Ru21_b 2.1780 (0.0175) 70.77 (0.93) 70.90 (0.93) 124.99 (1.93) C21_b - C22_b C25_b C31_b C22_b - Distance Angles C21_b 1.4180 (0.0189) C23_b 1.4490 (0.0193) 107.88 (1.51) C34_b 1.5743 (0.0233) 128.84 (2.30) 123.26 (2.25) Ru21_b 2.1726 (0.0179) 71.19 (0.94) 71.28 (0.94) 121.81 (2.00) C22_b - C21_b C23_b C34_b C23_b - Distance Angles C24_b 1.3867 (0.0190) C22_b 1.4490 (0.0193) 107.64 (1.58) Ru21_b 2.1906 (0.0177) 70.66 (0.99) 69.93 (0.92) H23_b 0.9500 126.18 126.18 124.84 C23_b - C24_b C22_b Ru21_b C24_b - Distance Angles C23_b 1.3867 (0.0191) C25_b 1.4175 (0.0194) 110.76 (1.69) Ru21_b 2.1701 (0.0180) 72.26 (0.99) 71.89 (0.98) H24_b 0.9500 124.62 124.62 122.80 C24_b - C23_b C25_b Ru21_b C25_b - Distance Angles C24_b 1.4175 (0.0194) C21_b 1.4676 (0.0196) 106.05 (1.57) Ru21_b 2.1923 (0.0175) 70.19 (0.96) 69.86 (0.91) H25_b 0.9500 126.98 126.98 124.61 C25_b - C24_b C21_b Ru21_b C26_b - Distance Angles C27_b 1.4171 (0.0196) C30_b 1.4678 (0.0201) 107.01 (1.60) Ru21_b 2.1736 (0.0183) 71.06 (0.95) 72.36 (0.97) H26_b 0.9500 126.49 126.49 121.85 C26_b - C27_b C30_b Ru21_b C27_b - Distance Angles C26_b 1.4171 (0.0195) C28_b 1.4468 (0.0195) 108.69 (1.59) Ru21_b 2.1756 (0.0171) 70.91 (0.94) 71.12 (0.91) H27_b 0.9500 125.65 125.65 123.93 C27_b - C26_b C28_b Ru21_b C28_b - Distance Angles C29_b 1.3872 (0.0189) C27_b 1.4468 (0.0195) 107.22 (1.60) Ru21_b 2.1884 (0.0168) 71.33 (0.94) 70.16 (0.91) H28_b 0.9500 126.39 126.39 123.76 C28_b - C29_b C27_b Ru21_b C29_b - Distance Angles C28_b 1.3872 (0.0189) C30_b 1.4218 (0.0194) 110.73 (1.68) Ru21_b 2.1841 (0.0172) 71.67 (0.95) 72.70 (0.97) H29_b 0.9500 124.64 124.64 122.56 C29_b - C28_b C30_b Ru21_b C30_b - Distance Angles C29_b 1.4218 (0.0194) C26_b 1.4678 (0.0201) 106.25 (1.57) Ru21_b 2.2238 (0.0179) 69.67 (0.94) 68.67 (0.95) H30_b 0.9500 126.88 126.88 126.34 C30_b - C29_b C26_b Ru21_b C31_b - Distance Angles C21_b 1.4757 (0.0216) N21_b 1.4993 (0.0226) 112.39 (2.37) H31A_b 0.9900 109.12 109.12 H31B_b 0.9900 109.12 109.12 107.85 C31_b - C21_b N21_b H31A_b C32_b - Distance Angles N21_b 1.4554 (0.0247) H32A_b 0.9800 109.47 H32B_b 0.9800 109.47 109.47 H32C_b 0.9800 109.47 109.47 109.47 C32_b - N21_b H32A_b H32B_b C33_b - Distance Angles N21_b 1.4510 (0.0241) H33A_b 0.9800 109.47 H33B_b 0.9800 109.47 109.47 H33C_b 0.9800 109.47 109.47 109.47 C33_b - N21_b H33A_b H33B_b C34_b - Distance Angles N22_b 1.4674 (0.0271) C22_b 1.5743 (0.0234) 109.58 (2.36) H34A_b 0.9900 109.75 109.75 H34B_b 0.9900 109.75 109.75 108.22 C34_b - N22_b C22_b H34A_b C35_b - Distance Angles N22_b 1.3946 (0.0288) H35A_b 0.9800 109.47 H35B_b 0.9800 109.47 109.47 H35C_b 0.9800 109.47 109.47 109.47 C35_b - N22_b H35A_b H35B_b C36_b - Distance Angles N22_b 1.4502 (0.0239) H36A_b 0.9800 109.47 H36B_b 0.9800 109.47 109.47 H36C_b 0.9800 109.47 109.47 109.47 C36_b - N22_b H36A_b H36B_b N21_b - Distance Angles C33_b 1.4510 (0.0241) C32_b 1.4554 (0.0248) 109.45 (2.78) C31_b 1.4993 (0.0226) 109.92 (2.79) 109.82 (2.71) N21_b - C33_b C32_b N22_b - Distance Angles C35_b 1.3946 (0.0287) C36_b 1.4502 (0.0238) 110.99 (3.32) C34_b 1.4674 (0.0270) 116.99 (3.44) 105.42 (2.71) N22_b - C35_b C36_b Ru21_b - Distance Angles C24_b 2.1701 (0.0181) C22_b 2.1726 (0.0179) 63.63 (0.76) C26_b 2.1736 (0.0184) 163.23 (1.22) 124.69 (1.07) C27_b 2.1756 (0.0171) 157.85 (1.22) 110.84 (1.05) 38.03 (0.57) C21_b 2.1780 (0.0175) 64.03 (0.77) 38.04 (0.55) 112.31 (1.07) 126.21 (1.06) C29_b 2.1841 (0.0173) 113.79 (1.10) 159.34 (1.16) 64.08 (0.77) 63.11 (0.76) 161.81 (1.16) C28_b 2.1884 (0.0168) 124.91 (1.10) 125.61 (1.07) 64.48 (0.76) 38.72 (0.55) 159.95 (1.17) 36.99 (0.54) C23_b 2.1906 (0.0179) 37.08 (0.55) 38.79 (0.56) 158.31 (1.19) 124.83 (1.11) 64.08 (0.75) 126.25 (1.07) 110.93 (1.07) C25_b 2.1923 (0.0175) 37.92 (0.56) 64.51 (0.75) 128.60 (1.12) 162.03 (1.18) 39.24 (0.56) 127.44 (1.08) 158.49 (1.17) C30_b 2.2238 (0.0181) 128.83 (1.11) 160.31 (1.17) 38.98 (0.57) 63.62 (0.78) 128.05 (1.08) 37.62 (0.55) 63.18 (0.75) Ru21_b - C24_b C22_b C26_b C27_b C21_b C29_b C28_b FMAP and GRID set by program FMAP 2 1 12 GRID -2.778 -2 -1 2.778 2 1 R1 = 0.2173 for 3397 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.12 at 0.0678 0.3458 0.3305 [ 0.64 A from C6 ] Deepest hole -1.58 at 0.0142 0.8416 0.3538 [ 1.07 A from C3 ] Mean = 0.00, Rms deviation from mean = 0.20 e/A^3, Highest memory used = 6493 / 33141 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4322 0.8458 0.3305 1.00000 0.05 1.12 0.64 C6 0.86 C10 0.90 RU21 1.31 H6 Q2 1 0.4339 0.8425 0.3791 1.00000 0.05 0.88 1.00 RU21 1.23 C24 1.32 H10 1.35 C10 Q3 1 0.3390 0.8041 0.3070 1.00000 0.05 0.80 0.62 C6 0.91 C7 1.21 C27 1.30 RU21 Q4 1 0.3373 0.8775 0.3941 1.00000 0.05 0.79 1.22 RU21 1.41 C25 1.59 C10 1.59 H10 Q5 1 0.3476 0.7612 0.3982 1.00000 0.05 0.73 0.64 C21 1.49 C25 1.56 H11A 1.60 C31 Shortest distances between peaks (including symmetry equivalents) 2 4 1.00 1 3 1.14 1 2 1.25 2 5 1.51 4 5 1.81 1 4 1.86 2 3 2.08 1 5 2.28 3 5 2.44 3 4 2.51 Time profile in seconds ----------------------- 0.07: Read and process instructions 0.00: Fit rigid groups 0.01: 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. 0.53: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.04: Set up l.s. refinement 0.01: Generate idealized H-atoms 10.24: Structure factors and derivatives 13.05: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.13: Apply other restraints 1.83: Solve l.s. equations 0.00: Generate HTAB table 0.07: Other dependent quantities, CIF, tables 0.12: Analysis of variance 0.04: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.08: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005src0328 finished at 11:00:41 Total CPU time: 26.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++