+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0196 started at 18:00:12 on 21-Mar-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0196 in P2(1)/n CELL 0.71073 9.2979 18.4632 18.9798 90.000 99.325 90.000 ZERR 4.00 0.0005 0.0008 0.0009 0.000 0.003 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H O P GA MO I UNIT 108 164 8 4 4 4 12 V = 3215.19 F(000) = 1864.0 Mu = 4.18 mm-1 Cell Wt = 3899.71 Rho = 2.014 MERG 2 OMIT -3.00 55.00 OMIT 0 0 4 SHEL 7 0.84 DELU DFIX 1.31 0.14 P1 H1 FMAP 2 PLAN 10 SIZE 0.02 0.05 0.18 ACTA BOND $H WGHT 0.08060 91.19110 L.S. 10 TEMP -153.00 FVAR 0.20440 MOLE 1 C1 1 0.375113 0.152168 0.912186 11.00000 0.02520 0.03971 = 0.03897 0.00429 0.00469 -0.00090 C2 1 0.178873 0.046458 0.906688 11.00000 0.05087 0.02805 = 0.03727 -0.00560 -0.00129 -0.00075 C3 1 0.217849 0.031444 1.074444 11.00000 0.06203 0.03153 = 0.04109 0.01225 0.00758 -0.00087 AFIX 43 H3 2 0.165851 -0.012489 1.077173 11.00000 -1.20000 AFIX 0 C4 1 0.135517 0.092800 1.077780 11.00000 0.04495 0.04029 = 0.03563 0.01221 0.01114 -0.00314 AFIX 43 H4 2 0.035070 0.085537 1.079686 11.00000 -1.20000 AFIX 0 C5 1 0.183635 0.165713 1.078695 11.00000 0.04111 0.03253 = 0.02350 -0.00263 0.00249 0.00365 AFIX 43 H5 2 0.109377 0.201334 1.076800 11.00000 -1.20000 AFIX 0 C6 1 0.327155 0.192788 1.082045 11.00000 0.04913 0.03964 = 0.02946 -0.00161 -0.00682 -0.00804 AFIX 43 H6 2 0.340010 0.243472 1.089049 11.00000 -1.20000 AFIX 0 C7 1 0.449175 0.153200 1.076196 11.00000 0.03641 0.06186 = 0.03313 0.00806 -0.00835 -0.00926 AFIX 43 H7 2 0.535467 0.181182 1.078120 11.00000 -1.20000 AFIX 0 C8 1 0.469361 0.077638 1.067757 11.00000 0.03859 0.06910 = 0.04034 0.01682 -0.00542 0.01790 AFIX 43 H8 2 0.564234 0.062802 1.061371 11.00000 -1.20000 AFIX 0 C9 1 0.365224 0.021862 1.067720 11.00000 0.06762 0.04200 = 0.02890 0.01246 0.01022 0.01800 AFIX 43 H9 2 0.397563 -0.026393 1.062711 11.00000 -1.20000 AFIX 0 O1 3 0.427806 0.174909 0.866741 11.00000 0.03968 0.07918 = 0.04677 0.01788 0.01419 0.00114 O2 3 0.135050 0.012347 0.861413 11.00000 0.09703 0.04820 = 0.04412 -0.01560 0.00004 -0.00342 GA1 5 0.075317 0.196340 0.917155 11.00000 0.02505 0.02763 = 0.02743 0.00013 0.00111 0.00317 MO1 6 0.270416 0.111209 0.987725 11.00000 0.02838 0.02762 = 0.02558 0.00230 0.00233 0.00407 I1 7 0.132490 0.336068 0.948604 11.00000 0.03394 0.02526 = 0.04527 -0.00212 -0.00115 0.00049 I2 7 -0.188748 0.177538 0.953192 11.00000 0.02903 0.03288 = 0.05153 0.00354 0.01229 0.00214 I3 7 0.013100 0.201678 0.777400 11.00000 0.03863 0.05125 = 0.02605 0.00016 -0.00268 -0.00260 MOLE 2 C10 1 0.804999 0.452395 0.837922 11.00000 0.04320 0.01889 = 0.01924 -0.00124 0.00464 0.00886 AFIX 13 H10 2 0.896408 0.457509 0.873439 11.00000 -1.20000 AFIX 0 C11 1 0.731379 0.527498 0.835483 11.00000 0.03462 0.02571 = 0.05089 -0.00179 0.01280 -0.00451 AFIX 23 H11A 2 0.643271 0.527532 0.798379 11.00000 -1.20000 H11B 2 0.700687 0.537640 0.882070 11.00000 -1.20000 AFIX 0 C12 1 0.833614 0.585344 0.819271 11.00000 0.02666 0.02693 = 0.04707 0.00101 0.00657 -0.01164 AFIX 23 H12A 2 0.915843 0.589340 0.859348 11.00000 -1.20000 H12B 2 0.782043 0.632435 0.814297 11.00000 -1.20000 AFIX 0 C13 1 0.893176 0.568262 0.749674 11.00000 0.06203 0.03200 = 0.03166 0.00191 0.00692 -0.01077 AFIX 23 H13A 2 0.812624 0.571637 0.708731 11.00000 -1.20000 H13B 2 0.967280 0.604937 0.742727 11.00000 -1.20000 AFIX 0 C14 1 0.962108 0.492222 0.750768 11.00000 0.03303 0.04611 = 0.04802 -0.00418 0.01806 -0.00503 AFIX 23 H14A 2 0.989533 0.481623 0.703562 11.00000 -1.20000 H14B 2 1.051670 0.490760 0.786934 11.00000 -1.20000 AFIX 0 C15 1 0.855456 0.435392 0.768310 11.00000 0.03493 0.03198 = 0.02235 -0.00088 0.00318 0.00181 AFIX 23 H15A 2 0.770276 0.433566 0.729579 11.00000 -1.20000 H15B 2 0.902952 0.387250 0.771483 11.00000 -1.20000 AFIX 0 C16 1 0.542380 0.344460 0.814378 11.00000 0.03504 0.01913 = 0.03164 -0.00813 -0.00591 0.00238 AFIX 13 H16 2 0.490668 0.312675 0.844842 11.00000 -1.20000 AFIX 0 C17 1 0.583339 0.295191 0.753929 11.00000 0.03087 0.04328 = 0.02511 0.00124 -0.00083 0.01295 AFIX 23 H17A 2 0.634427 0.324210 0.721737 11.00000 -1.20000 H17B 2 0.649851 0.256230 0.775036 11.00000 -1.20000 AFIX 0 C18 1 0.446389 0.262172 0.711748 11.00000 0.04200 0.03443 = 0.03001 -0.00807 -0.00694 -0.00544 AFIX 23 H18A 2 0.403884 0.227640 0.742581 11.00000 -1.20000 H18B 2 0.472488 0.234757 0.670804 11.00000 -1.20000 AFIX 0 C19 1 0.332398 0.319462 0.684031 11.00000 0.03320 0.04325 = 0.01933 0.00521 -0.00661 -0.01628 AFIX 23 H19A 2 0.241688 0.295049 0.661536 11.00000 -1.20000 H19B 2 0.368539 0.348886 0.646947 11.00000 -1.20000 AFIX 0 C20 1 0.297947 0.369752 0.743785 11.00000 0.02336 0.04457 = 0.03927 0.00775 0.00075 -0.00060 AFIX 23 H20A 2 0.230227 0.408208 0.722610 11.00000 -1.20000 H20B 2 0.248497 0.341515 0.777206 11.00000 -1.20000 AFIX 0 C21 1 0.432900 0.404211 0.784577 11.00000 0.04148 0.03228 = 0.02708 -0.00269 -0.00777 0.01237 AFIX 23 H21A 2 0.407071 0.433577 0.824345 11.00000 -1.20000 H21B 2 0.477621 0.436642 0.752657 11.00000 -1.20000 AFIX 0 C22 1 0.655187 0.409350 0.957644 11.00000 0.03498 0.02415 = 0.02106 0.00162 0.00120 0.00752 AFIX 13 H22 2 0.580500 0.448584 0.947739 11.00000 -1.20000 AFIX 0 C23 1 0.588532 0.346929 0.996326 11.00000 0.04840 0.03315 = 0.02853 -0.01344 0.01269 -0.01566 AFIX 23 H23A 2 0.500171 0.328428 0.965390 11.00000 -1.20000 H23B 2 0.659552 0.306709 1.005322 11.00000 -1.20000 AFIX 0 C24 1 0.548717 0.372701 1.066938 11.00000 0.05503 0.06227 = 0.02499 -0.00601 0.01711 -0.01021 AFIX 23 H24A 2 0.469691 0.409035 1.057191 11.00000 -1.20000 H24B 2 0.511201 0.331137 1.091473 11.00000 -1.20000 AFIX 0 C25 1 0.676626 0.405845 1.115894 11.00000 0.05072 0.03953 = 0.01928 -0.00019 0.00656 0.01215 AFIX 23 H25A 2 0.643991 0.425175 1.159328 11.00000 -1.20000 H25B 2 0.751868 0.368480 1.130617 11.00000 -1.20000 AFIX 0 C26 1 0.739666 0.466199 1.076663 11.00000 0.04025 0.05903 = 0.01702 0.00491 0.00056 0.00183 AFIX 23 H26A 2 0.824900 0.487176 1.108059 11.00000 -1.20000 H26B 2 0.665853 0.504907 1.065361 11.00000 -1.20000 AFIX 0 C27 1 0.786503 0.439973 1.007864 11.00000 0.05512 0.03803 = 0.02114 -0.00707 0.00666 -0.01616 AFIX 23 H27A 2 0.862002 0.402010 1.018846 11.00000 -1.20000 H27B 2 0.829046 0.480740 0.984312 11.00000 -1.20000 AFIX 0 P1 4 0.702687 0.380233 0.872960 11.00000 0.02933 0.03069 = 0.02382 -0.00162 -0.00046 -0.00095 H1 2 0.800866 0.320473 0.876214 11.00000 0.02774 HKLF 4 Covalent radii and connectivity table for 2007src0196 in P2(1)/n C 0.770 H 0.320 O 0.660 P 1.100 GA 1.260 MO 1.360 I 1.330 C1 - O1 Mo1 C2 - O2 Mo1 C3 - C4 C9 Mo1 C4 - C3 C5 Mo1 C5 - C6 C4 Mo1 C6 - C7 C5 Mo1 C7 - C6 C8 Mo1 C8 - C9 C7 Mo1 C9 - C3 C8 Mo1 O1 - C1 O2 - C2 Ga1 - Mo1 I3 I2 I1 Mo1 - C1 C2 C5 C8 C7 C4 C9 C3 C6 Ga1 I1 - Ga1 I2 - Ga1 I3 - Ga1 C10 - C15 C11 P1 C11 - C12 C10 C12 - C11 C13 C13 - C14 C12 C14 - C15 C13 C15 - C10 C14 C16 - C21 C17 P1 C17 - C18 C16 C18 - C17 C19 C19 - C18 C20 C20 - C21 C19 C21 - C20 C16 C22 - C27 C23 P1 C23 - C24 C22 C24 - C25 C23 C25 - C26 C24 C26 - C25 C27 C27 - C26 C22 P1 - C22 C10 C16 h k l Fo^2 Sigma Why rejected 4 0 5 47.05 8.02 observed but should be systematically absent 24005 Reflections read, of which 3650 rejected -11 =< h =< 11, -21 =< k =< 21, -22 =< l =< 21, Max. 2-theta = 50.05 1 Systematic absence violations 0 Inconsistent equivalents 5554 Unique reflections, of which 0 suppressed R(int) = 0.0731 R(sigma) = 0.0661 Friedel opposites merged Maximum memory for data reduction = 4414 / 55179 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 = 5397 / 405101 wR2 = 0.2047 before cycle 1 for 5554 data and 320 / 320 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 144. 0. 0. 0. rms sigma 0.000 0.140 0.000 0.000 0.000 0.000 0.000 0.010 0.000 0.000 0.000 rms deviation 0.000 0.117 0.000 0.000 0.000 0.000 0.000 0.004 0.000 0.000 0.000 GooF = S = 1.077; Restrained GooF = 1.064 for 145 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0806 * P )^2 + 91.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20440 0.00061 0.000 OSF Mean shift/esd = 0.001 Maximum = -0.009 for z I1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5397 / 405101 wR2 = 0.2047 before cycle 2 for 5554 data and 320 / 320 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 144. 0. 0. 0. rms sigma 0.000 0.140 0.000 0.000 0.000 0.000 0.000 0.010 0.000 0.000 0.000 rms deviation 0.000 0.117 0.000 0.000 0.000 0.000 0.000 0.004 0.000 0.000 0.000 GooF = S = 1.077; Restrained GooF = 1.064 for 145 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0806 * P )^2 + 91.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20440 0.00061 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.003 for U13 I2 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5397 / 405101 wR2 = 0.2047 before cycle 3 for 5554 data and 320 / 320 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 144. 0. 0. 0. rms sigma 0.000 0.140 0.000 0.000 0.000 0.000 0.000 0.010 0.000 0.000 0.000 rms deviation 0.000 0.117 0.000 0.000 0.000 0.000 0.000 0.004 0.000 0.000 0.000 GooF = S = 1.077; Restrained GooF = 1.064 for 145 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0806 * P )^2 + 91.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20440 0.00061 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z I3 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5397 / 405101 wR2 = 0.2047 before cycle 4 for 5554 data and 320 / 320 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 144. 0. 0. 0. rms sigma 0.000 0.140 0.000 0.000 0.000 0.000 0.000 0.010 0.000 0.000 0.000 rms deviation 0.000 0.117 0.000 0.000 0.000 0.000 0.000 0.004 0.000 0.000 0.000 GooF = S = 1.077; Restrained GooF = 1.064 for 145 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0806 * P )^2 + 91.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20440 0.00061 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z I3 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 5397 / 405101 wR2 = 0.2047 before cycle 5 for 5554 data and 320 / 320 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 144. 0. 0. 0. rms sigma 0.000 0.140 0.000 0.000 0.000 0.000 0.000 0.010 0.000 0.000 0.000 rms deviation 0.000 0.117 0.000 0.000 0.000 0.000 0.000 0.004 0.000 0.000 0.000 GooF = S = 1.077; Restrained GooF = 1.064 for 145 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0806 * P )^2 + 91.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20440 0.00061 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z I3 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 5397 / 405101 wR2 = 0.2047 before cycle 6 for 5554 data and 320 / 320 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 144. 0. 0. 0. rms sigma 0.000 0.140 0.000 0.000 0.000 0.000 0.000 0.010 0.000 0.000 0.000 rms deviation 0.000 0.117 0.000 0.000 0.000 0.000 0.000 0.004 0.000 0.000 0.000 GooF = S = 1.077; Restrained GooF = 1.064 for 145 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0806 * P )^2 + 91.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20440 0.00061 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z I3 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 7 Maximum vector length = 511 Memory required = 5397 / 405101 wR2 = 0.2047 before cycle 7 for 5554 data and 320 / 320 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 144. 0. 0. 0. rms sigma 0.000 0.140 0.000 0.000 0.000 0.000 0.000 0.010 0.000 0.000 0.000 rms deviation 0.000 0.117 0.000 0.000 0.000 0.000 0.000 0.004 0.000 0.000 0.000 GooF = S = 1.077; Restrained GooF = 1.064 for 145 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0806 * P )^2 + 91.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20440 0.00061 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z I3 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 8 Maximum vector length = 511 Memory required = 5397 / 405101 wR2 = 0.2047 before cycle 8 for 5554 data and 320 / 320 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 144. 0. 0. 0. rms sigma 0.000 0.140 0.000 0.000 0.000 0.000 0.000 0.010 0.000 0.000 0.000 rms deviation 0.000 0.117 0.000 0.000 0.000 0.000 0.000 0.004 0.000 0.000 0.000 GooF = S = 1.077; Restrained GooF = 1.064 for 145 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0806 * P )^2 + 91.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20440 0.00061 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z I3 Max. shift = 0.000 A for C8 Max. dU = 0.000 for H1 Least-squares cycle 9 Maximum vector length = 511 Memory required = 5397 / 405101 wR2 = 0.2047 before cycle 9 for 5554 data and 320 / 320 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 144. 0. 0. 0. rms sigma 0.000 0.140 0.000 0.000 0.000 0.000 0.000 0.010 0.000 0.000 0.000 rms deviation 0.000 0.117 0.000 0.000 0.000 0.000 0.000 0.004 0.000 0.000 0.000 GooF = S = 1.077; Restrained GooF = 1.064 for 145 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0806 * P )^2 + 91.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20440 0.00061 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z I3 Max. shift = 0.000 A for C5 Max. dU = 0.000 for H1 Least-squares cycle 10 Maximum vector length = 511 Memory required = 5397 / 405101 wR2 = 0.2047 before cycle 10 for 5554 data and 320 / 320 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 144. 0. 0. 0. rms sigma 0.000 0.140 0.000 0.000 0.000 0.000 0.000 0.010 0.000 0.000 0.000 rms deviation 0.000 0.117 0.000 0.000 0.000 0.000 0.000 0.004 0.000 0.000 0.000 GooF = S = 1.077; Restrained GooF = 1.064 for 145 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0806 * P )^2 + 91.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20440 0.00061 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z I3 Max. shift = 0.000 A for C8 Max. dU = 0.000 for H1 Largest correlation matrix elements 0.559 U22 C8 / U22 C7 0.538 U13 C4 / U33 C4 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by ** Bond(s) to Mo1 ignored in idealizing H-atoms attached to C3 ** H3 0.1659 -0.0125 1.0772 43 0.950 0.000 C3 C4 C9 ** Bond(s) to Mo1 ignored in idealizing H-atoms attached to C4 ** H4 0.0351 0.0855 1.0797 43 0.950 0.000 C4 C3 C5 ** Bond(s) to Mo1 ignored in idealizing H-atoms attached to C5 ** H5 0.1094 0.2013 1.0768 43 0.950 0.000 C5 C6 C4 ** Bond(s) to Mo1 ignored in idealizing H-atoms attached to C6 ** H6 0.3400 0.2435 1.0890 43 0.950 0.000 C6 C7 C5 ** Bond(s) to Mo1 ignored in idealizing H-atoms attached to C7 ** H7 0.5355 0.1812 1.0781 43 0.950 0.000 C7 C6 C8 ** Bond(s) to Mo1 ignored in idealizing H-atoms attached to C8 ** H8 0.5642 0.0628 1.0614 43 0.950 0.000 C8 C9 C7 ** Bond(s) to Mo1 ignored in idealizing H-atoms attached to C9 ** H9 0.3976 -0.0264 1.0627 43 0.950 0.000 C9 C3 C8 H10 0.8964 0.4575 0.8734 13 1.000 0.000 C10 C15 C11 P1 H11A 0.6433 0.5275 0.7984 23 0.990 0.000 C11 C12 C10 H11B 0.7007 0.5376 0.8821 23 0.990 0.000 C11 C12 C10 H12A 0.9158 0.5893 0.8593 23 0.990 0.000 C12 C11 C13 H12B 0.7820 0.6324 0.8143 23 0.990 0.000 C12 C11 C13 H13A 0.8126 0.5716 0.7087 23 0.990 0.000 C13 C14 C12 H13B 0.9673 0.6049 0.7427 23 0.990 0.000 C13 C14 C12 H14A 0.9895 0.4816 0.7036 23 0.990 0.000 C14 C15 C13 H14B 1.0517 0.4908 0.7869 23 0.990 0.000 C14 C15 C13 H15A 0.7703 0.4336 0.7296 23 0.990 0.000 C15 C10 C14 H15B 0.9030 0.3873 0.7715 23 0.990 0.000 C15 C10 C14 H16 0.4907 0.3127 0.8448 13 1.000 0.000 C16 C21 C17 P1 H17A 0.6344 0.3242 0.7217 23 0.990 0.000 C17 C18 C16 H17B 0.6499 0.2562 0.7750 23 0.990 0.000 C17 C18 C16 H18A 0.4039 0.2276 0.7426 23 0.990 0.000 C18 C17 C19 H18B 0.4725 0.2348 0.6708 23 0.990 0.000 C18 C17 C19 H19A 0.2417 0.2950 0.6615 23 0.990 0.000 C19 C18 C20 H19B 0.3685 0.3489 0.6469 23 0.990 0.000 C19 C18 C20 H20A 0.2302 0.4082 0.7226 23 0.990 0.000 C20 C21 C19 H20B 0.2485 0.3415 0.7772 23 0.990 0.000 C20 C21 C19 H21A 0.4071 0.4336 0.8243 23 0.990 0.000 C21 C20 C16 H21B 0.4776 0.4366 0.7527 23 0.990 0.000 C21 C20 C16 H22 0.5805 0.4486 0.9477 13 1.000 0.000 C22 C27 C23 P1 H23A 0.5002 0.3284 0.9654 23 0.990 0.000 C23 C24 C22 H23B 0.6596 0.3067 1.0053 23 0.990 0.000 C23 C24 C22 H24A 0.4697 0.4090 1.0572 23 0.990 0.000 C24 C25 C23 H24B 0.5112 0.3311 1.0915 23 0.990 0.000 C24 C25 C23 H25A 0.6440 0.4252 1.1593 23 0.990 0.000 C25 C26 C24 H25B 0.7519 0.3685 1.1306 23 0.990 0.000 C25 C26 C24 H26A 0.8249 0.4872 1.1081 23 0.990 0.000 C26 C25 C27 H26B 0.6659 0.5049 1.0654 23 0.990 0.000 C26 C25 C27 H27A 0.8620 0.4020 1.0188 23 0.990 0.000 C27 C26 C22 H27B 0.8290 0.4807 0.9843 23 0.990 0.000 C27 C26 C22 2007src0196 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.37511 0.15217 0.91219 1.00000 0.02520 0.03972 0.03897 0.00428 0.00469 -0.00090 0.03469 0.02639 0.00149 0.00077 0.00078 0.00000 0.00591 0.00727 0.00529 0.00489 0.00463 0.00500 0.00259 C2 0.17887 0.04646 0.90669 1.00000 0.05087 0.02805 0.03727 -0.00560 -0.00129 -0.00074 0.03966 0.02670 0.00174 0.00076 0.00078 0.00000 0.00856 0.00585 0.00535 0.00463 0.00513 0.00519 0.00293 C3 0.21785 0.03144 1.07444 1.00000 0.06203 0.03153 0.04109 0.01224 0.00758 -0.00086 0.04497 0.03069 0.00190 0.00081 0.00081 0.00000 0.00680 0.00492 0.00664 0.00497 0.00650 0.00476 0.00282 H3 0.16585 -0.01249 1.07717 1.00000 0.05396 0.00000 0.00000 C4 0.13552 0.09280 1.07778 1.00000 0.04495 0.04028 0.03563 0.01222 0.01114 -0.00314 0.03978 0.02888 0.00173 0.00080 0.00076 0.00000 0.00613 0.00575 0.00612 0.00544 0.00522 0.00428 0.00255 H4 0.03507 0.08554 1.07969 1.00000 0.04773 0.00000 0.00000 C5 0.18363 0.16571 1.07869 1.00000 0.04111 0.03253 0.02350 -0.00263 0.00249 0.00366 0.03268 0.02476 0.00159 0.00073 0.00068 0.00000 0.00545 0.00486 0.00490 0.00461 0.00474 0.00460 0.00225 H5 0.10938 0.20133 1.07680 1.00000 0.03922 0.00000 0.00000 C6 0.32715 0.19279 1.08205 1.00000 0.04912 0.03964 0.02946 -0.00161 -0.00682 -0.00804 0.04087 0.02602 0.00174 0.00083 0.00075 0.00000 0.00630 0.00547 0.00565 0.00457 0.00531 0.00427 0.00256 H6 0.34001 0.24347 1.08905 1.00000 0.04904 0.00000 0.00000 C7 0.44918 0.15320 1.07620 1.00000 0.03641 0.06186 0.03313 0.00806 -0.00835 -0.00926 0.04535 0.02818 0.00172 0.00094 0.00078 0.00000 0.00514 0.00630 0.00615 0.00601 0.00466 0.00474 0.00275 H7 0.53547 0.18118 1.07812 1.00000 0.05442 0.00000 0.00000 C8 0.46936 0.07764 1.06776 1.00000 0.03859 0.06910 0.04034 0.01682 -0.00542 0.01790 0.05065 0.03274 0.00180 0.00099 0.00083 0.00000 0.00525 0.00701 0.00747 0.00662 0.00478 0.00479 0.00305 H8 0.56423 0.06280 1.06137 1.00000 0.06079 0.00000 0.00000 C9 0.36522 0.02186 1.06772 1.00000 0.06761 0.04201 0.02890 0.01246 0.01021 0.01800 0.04591 0.03226 0.00192 0.00087 0.00075 0.00000 0.00743 0.00530 0.00651 0.00488 0.00608 0.00470 0.00285 H9 0.39756 -0.02639 1.06271 1.00000 0.05509 0.00000 0.00000 O1 0.42780 0.17491 0.86674 1.00000 0.03967 0.07918 0.04676 0.01787 0.01419 0.00114 0.05441 0.02321 0.00122 0.00071 0.00060 0.00000 0.00638 0.00849 0.00652 0.00569 0.00489 0.00573 0.00301 O2 0.13505 0.01235 0.86141 1.00000 0.09704 0.04820 0.04412 -0.01560 0.00004 -0.00342 0.06439 0.02239 0.00162 0.00065 0.00062 0.00000 0.01039 0.00678 0.00651 0.00498 0.00617 0.00666 0.00349 Ga1 0.07532 0.19634 0.91716 1.00000 0.02505 0.02763 0.02743 0.00013 0.00111 0.00317 0.02706 0.00257 0.00015 0.00007 0.00007 0.00000 0.00073 0.00071 0.00074 0.00056 0.00055 0.00056 0.00034 Mo1 0.27042 0.11121 0.98773 1.00000 0.02838 0.02762 0.02558 0.00230 0.00233 0.00407 0.02742 0.00208 0.00012 0.00006 0.00006 0.00000 0.00060 0.00057 0.00059 0.00043 0.00044 0.00045 0.00029 I1 0.13249 0.33607 0.94860 1.00000 0.03394 0.02526 0.04527 -0.00212 -0.00115 0.00049 0.03566 0.00162 0.00010 0.00005 0.00005 0.00000 0.00051 0.00044 0.00056 0.00036 0.00039 0.00035 0.00027 I2 -0.18875 0.17754 0.95319 1.00000 0.02903 0.03288 0.05153 0.00354 0.01229 0.00214 0.03717 0.00180 0.00010 0.00005 0.00005 0.00000 0.00049 0.00049 0.00059 0.00040 0.00040 0.00037 0.00027 I3 0.01310 0.20168 0.77740 1.00000 0.03863 0.05125 0.02605 0.00016 -0.00268 -0.00260 0.03952 0.00171 0.00011 0.00006 0.00005 0.00000 0.00054 0.00059 0.00048 0.00039 0.00036 0.00042 0.00028 C10 0.80500 0.45240 0.83792 1.00000 0.04320 0.01890 0.01924 -0.00124 0.00464 0.00886 0.02716 0.02417 0.00151 0.00064 0.00063 0.00000 0.00720 0.00501 0.00566 0.00440 0.00473 0.00442 0.00240 H10 0.89641 0.45751 0.87344 1.00000 0.03259 0.00000 0.00000 C11 0.73138 0.52750 0.83548 1.00000 0.03461 0.02572 0.05089 -0.00179 0.01280 -0.00451 0.03642 0.02692 0.00158 0.00071 0.00082 0.00000 0.00762 0.00542 0.00858 0.00555 0.00605 0.00500 0.00300 H11A 0.64327 0.52753 0.79838 1.00000 0.04371 0.00000 0.00000 H11B 0.70069 0.53764 0.88207 1.00000 0.04371 0.00000 0.00000 C12 0.83361 0.58534 0.81927 1.00000 0.02666 0.02693 0.04708 0.00101 0.00657 -0.01163 0.03349 0.02466 0.00146 0.00072 0.00076 0.00000 0.00687 0.00580 0.00761 0.00551 0.00555 0.00514 0.00280 H12A 0.91585 0.58934 0.85935 1.00000 0.04019 0.00000 0.00000 H12B 0.78204 0.63244 0.81430 1.00000 0.04019 0.00000 0.00000 C13 0.89317 0.56826 0.74967 1.00000 0.06202 0.03200 0.03166 0.00191 0.00692 -0.01077 0.04197 0.02793 0.00186 0.00077 0.00076 0.00000 0.01006 0.00609 0.00723 0.00574 0.00620 0.00634 0.00329 H13A 0.81262 0.57164 0.70873 1.00000 0.05036 0.00000 0.00000 H13B 0.96728 0.60494 0.74273 1.00000 0.05036 0.00000 0.00000 C14 0.96211 0.49222 0.75077 1.00000 0.03303 0.04611 0.04803 -0.00417 0.01806 -0.00503 0.04111 0.02890 0.00163 0.00082 0.00085 0.00000 0.00772 0.00748 0.00848 0.00648 0.00612 0.00568 0.00320 H14A 0.98953 0.48162 0.70356 1.00000 0.04934 0.00000 0.00000 H14B 1.05167 0.49076 0.78693 1.00000 0.04934 0.00000 0.00000 C15 0.85546 0.43539 0.76831 1.00000 0.03493 0.03198 0.02235 -0.00088 0.00318 0.00181 0.02991 0.02409 0.00148 0.00071 0.00065 0.00000 0.00718 0.00604 0.00599 0.00481 0.00481 0.00513 0.00257 H15A 0.77028 0.43357 0.72958 1.00000 0.03590 0.00000 0.00000 H15B 0.90295 0.38725 0.77148 1.00000 0.03590 0.00000 0.00000 C16 0.54238 0.34446 0.81438 1.00000 0.03504 0.01913 0.03164 -0.00813 -0.00591 0.00238 0.02986 0.02228 0.00148 0.00066 0.00070 0.00000 0.00640 0.00579 0.00639 0.00455 0.00477 0.00445 0.00265 H16 0.49067 0.31267 0.84484 1.00000 0.03583 0.00000 0.00000 C17 0.58334 0.29519 0.75393 1.00000 0.03087 0.04328 0.02511 0.00124 -0.00083 0.01294 0.03368 0.02552 0.00149 0.00078 0.00069 0.00000 0.00653 0.00761 0.00642 0.00487 0.00477 0.00534 0.00281 H17A 0.63443 0.32421 0.72174 1.00000 0.04042 0.00000 0.00000 H17B 0.64985 0.25623 0.77504 1.00000 0.04042 0.00000 0.00000 C18 0.44639 0.26217 0.71175 1.00000 0.04200 0.03443 0.03001 -0.00807 -0.00694 -0.00543 0.03690 0.02371 0.00160 0.00077 0.00073 0.00000 0.00773 0.00707 0.00708 0.00526 0.00556 0.00526 0.00301 H18A 0.40388 0.22764 0.74258 1.00000 0.04427 0.00000 0.00000 H18B 0.47249 0.23476 0.67080 1.00000 0.04427 0.00000 0.00000 C19 0.33240 0.31946 0.68403 1.00000 0.03320 0.04325 0.01934 0.00521 -0.00661 -0.01628 0.03313 0.02294 0.00151 0.00075 0.00066 0.00000 0.00664 0.00734 0.00613 0.00475 0.00485 0.00537 0.00274 H19A 0.24169 0.29505 0.66154 1.00000 0.03976 0.00000 0.00000 H19B 0.36854 0.34889 0.64695 1.00000 0.03976 0.00000 0.00000 C20 0.29795 0.36975 0.74378 1.00000 0.02336 0.04458 0.03927 0.00775 0.00075 -0.00060 0.03621 0.02594 0.00145 0.00081 0.00076 0.00000 0.00629 0.00771 0.00753 0.00561 0.00505 0.00528 0.00286 H20A 0.23023 0.40821 0.72261 1.00000 0.04346 0.00000 0.00000 H20B 0.24850 0.34151 0.77721 1.00000 0.04346 0.00000 0.00000 C21 0.43290 0.40421 0.78458 1.00000 0.04148 0.03228 0.02708 -0.00269 -0.00777 0.01237 0.03509 0.02499 0.00158 0.00074 0.00072 0.00000 0.00718 0.00680 0.00676 0.00504 0.00507 0.00527 0.00296 H21A 0.40707 0.43358 0.82435 1.00000 0.04211 0.00000 0.00000 H21B 0.47762 0.43664 0.75266 1.00000 0.04211 0.00000 0.00000 C22 0.65519 0.40935 0.95764 1.00000 0.03498 0.02416 0.02106 0.00162 0.00120 0.00753 0.02710 0.02329 0.00143 0.00067 0.00063 0.00000 0.00688 0.00595 0.00504 0.00420 0.00424 0.00494 0.00241 H22 0.58050 0.44858 0.94774 1.00000 0.03252 0.00000 0.00000 C23 0.58853 0.34693 0.99633 1.00000 0.04840 0.03315 0.02853 -0.01344 0.01270 -0.01566 0.03598 0.02449 0.00170 0.00074 0.00071 0.00000 0.00850 0.00702 0.00621 0.00519 0.00573 0.00592 0.00312 H23A 0.50017 0.32843 0.96539 1.00000 0.04317 0.00000 0.00000 H23B 0.65955 0.30671 1.00532 1.00000 0.04317 0.00000 0.00000 C24 0.54872 0.37270 1.06694 1.00000 0.05505 0.06227 0.02498 -0.00601 0.01711 -0.01021 0.04625 0.02879 0.00184 0.00097 0.00074 0.00000 0.00940 0.01001 0.00679 0.00634 0.00595 0.00710 0.00368 H24A 0.46969 0.40904 1.05719 1.00000 0.05551 0.00000 0.00000 H24B 0.51120 0.33114 1.09147 1.00000 0.05551 0.00000 0.00000 C25 0.67663 0.40584 1.11589 1.00000 0.05073 0.03953 0.01928 -0.00019 0.00656 0.01215 0.03641 0.02687 0.00166 0.00078 0.00068 0.00000 0.00848 0.00734 0.00597 0.00491 0.00505 0.00603 0.00293 H25A 0.64399 0.42517 1.15933 1.00000 0.04370 0.00000 0.00000 H25B 0.75187 0.36848 1.13062 1.00000 0.04370 0.00000 0.00000 C26 0.73967 0.46620 1.07666 1.00000 0.04025 0.05903 0.01702 0.00491 0.00056 0.00184 0.03922 0.02759 0.00166 0.00088 0.00067 0.00000 0.00798 0.00901 0.00575 0.00530 0.00523 0.00606 0.00309 H26A 0.82490 0.48718 1.10806 1.00000 0.04706 0.00000 0.00000 H26B 0.66585 0.50491 1.06536 1.00000 0.04706 0.00000 0.00000 C27 0.78650 0.43997 1.00786 1.00000 0.05512 0.03803 0.02114 -0.00708 0.00666 -0.01616 0.03804 0.02431 0.00174 0.00080 0.00068 0.00000 0.00873 0.00753 0.00575 0.00524 0.00528 0.00625 0.00318 H27A 0.86200 0.40201 1.01885 1.00000 0.04565 0.00000 0.00000 H27B 0.82904 0.48074 0.98431 1.00000 0.04565 0.00000 0.00000 P1 0.70269 0.38023 0.87296 1.00000 0.02933 0.03069 0.02382 -0.00162 -0.00046 -0.00095 0.02847 0.00604 0.00038 0.00018 0.00017 0.00000 0.00177 0.00171 0.00165 0.00128 0.00128 0.00138 0.00071 H1 0.80083 0.32048 0.87621 1.00000 0.02780 0.24700 0.01341 0.00604 0.00701 0.00000 0.03458 Final Structure Factor Calculation for 2007src0196 in P2(1)/n Total number of l.s. parameters = 320 Maximum vector length = 511 Memory required = 5077 / 26061 wR2 = 0.2047 before cycle 11 for 5554 data and 0 / 320 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 144. 0. 0. 0. rms sigma 0.000 0.140 0.000 0.000 0.000 0.000 0.000 0.010 0.000 0.000 0.000 rms deviation 0.000 0.117 0.000 0.000 0.000 0.000 0.000 0.004 0.000 0.000 0.000 GooF = S = 1.077; Restrained GooF = 1.064 for 145 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0806 * P )^2 + 91.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0731 for 4422 Fo > 4sig(Fo) and 0.0947 for all 5554 data wR2 = 0.2047, GooF = S = 1.077, Restrained GooF = 1.064 for all data Occupancy sum of asymmetric unit = 35.00 for non-hydrogen and 41.00 for hydrogen atoms Principal mean square atomic displacements U 0.0439 0.0350 0.0251 C1 0.0567 0.0372 0.0251 C2 0.0626 0.0494 0.0229 C3 0.0505 0.0461 0.0228 C4 0.0438 0.0315 0.0228 C5 0.0605 0.0388 0.0233 C6 0.0711 0.0423 0.0226 C7 0.0794 0.0536 0.0189 C8 0.0772 0.0395 0.0210 C9 0.0871 0.0449 0.0312 O1 0.1018 0.0615 0.0299 O2 0.0314 0.0277 0.0221 Ga1 0.0322 0.0280 0.0221 Mo1 0.0507 0.0312 0.0250 I1 0.0529 0.0323 0.0263 I2 0.0521 0.0432 0.0233 I3 0.0465 0.0199 0.0151 C10 0.0523 0.0333 0.0237 C11 0.0473 0.0384 0.0147 C12 0.0660 0.0329 0.0270 C13 0.0559 0.0431 0.0243 C14 0.0364 0.0311 0.0223 C15 0.0491 0.0255 0.0150 C16 0.0520 0.0293 0.0197 C17 0.0526 0.0396 0.0185 C18 0.0603 0.0245 0.0146 C19 0.0510 0.0348 0.0228 C20 0.0584 0.0274 0.0195 C21 0.0397 0.0232 0.0184 C22 0.0612 0.0299 0.0169 C23 0.0709 0.0484 0.0194 C24 0.0587 0.0318 0.0187 C25 0.0596 0.0418 0.0162 C26 0.0649 0.0309 0.0184 C27 0.0330 0.0310 0.0214 P1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.019 0.037 0.057 0.077 0.098 0.124 0.158 0.204 0.284 1.000 Number in group 571. 555. 557. 558. 535. 569. 555. 548. 550. 556. GooF 1.148 1.170 1.090 1.082 0.970 1.061 1.026 1.022 0.963 1.204 K 3.755 1.443 1.061 0.994 0.999 0.978 1.003 1.011 1.019 1.031 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.25 1.43 1.79 inf Number in group 564. 559. 553. 549. 563. 551. 550. 558. 548. 559. GooF 1.222 1.081 1.073 1.057 1.030 0.903 1.068 1.005 1.009 1.270 K 1.060 1.062 1.053 1.024 1.042 1.035 1.003 1.007 1.009 1.030 R1 0.207 0.173 0.139 0.113 0.096 0.078 0.079 0.061 0.064 0.059 Recommended weighting scheme: WGHT 0.0807 91.1760 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) -8 10 3 1445.69 11851.12 8.79 0.241 0.98 3 11 3 4745.88 18531.88 8.05 0.301 1.41 0 7 1 5435.45 17590.74 6.97 0.293 2.61 0 2 18 -354.00 2787.62 6.04 0.117 1.03 1 2 18 -357.95 2507.08 5.75 0.111 1.01 1 3 1 22754.04 47618.84 5.70 0.483 4.82 1 2 1 29075.10 60780.64 5.67 0.545 5.94 5 3 18 808.29 5154.13 5.57 0.159 0.84 0 1 6 77408.72 145965.59 5.35 0.845 3.08 4 3 19 482.77 3827.69 5.15 0.137 0.85 2 2 18 36.86 1892.88 4.98 0.096 0.98 0 10 0 18733.88 36967.40 4.70 0.425 1.85 5 10 6 11123.02 23017.73 4.63 0.336 1.16 -6 9 1 2163.51 6059.86 4.39 0.172 1.23 0 13 4 15784.10 29519.72 4.33 0.380 1.36 -11 2 5 1361.55 2.57 4.27 0.004 0.84 -3 9 7 6336.37 12492.38 4.20 0.247 1.50 -7 2 2 16482.29 28852.72 4.08 0.376 1.31 -7 10 2 1070.02 3620.62 4.03 0.133 1.08 7 4 4 22505.35 38656.39 4.01 0.435 1.17 2 3 19 2584.05 129.82 3.94 0.025 0.92 4 7 4 11120.07 19554.55 3.91 0.309 1.56 1 8 5 3119.24 6874.45 3.90 0.183 1.89 -5 2 9 2651.89 5894.00 3.83 0.170 1.48 5 11 0 1395.90 4096.85 3.83 0.142 1.24 8 4 4 1291.07 3859.68 3.76 0.137 1.05 7 5 2 26003.73 42668.16 3.76 0.457 1.20 -3 0 3 97338.16 150556.02 3.66 0.858 2.94 5 9 5 3499.09 7339.03 3.62 0.190 1.24 2 9 2 6872.06 11838.11 3.59 0.241 1.81 3 2 15 723.17 0.74 3.50 0.002 1.09 2 21 4 958.49 12.15 3.44 0.008 0.84 -4 19 9 2613.49 1.58 3.41 0.003 0.84 -3 4 6 930.68 104.81 3.41 0.023 2.12 2 7 20 1921.22 418.83 3.34 0.045 0.84 -1 7 3 2981.28 5810.90 3.33 0.169 2.39 -6 5 2 8895.42 14186.07 3.30 0.264 1.43 -3 14 17 -67.01 967.18 3.28 0.069 0.84 -4 17 9 3156.59 6364.15 3.26 0.176 0.91 -2 8 9 13201.60 20785.63 3.25 0.319 1.52 3 10 0 1888.25 4256.27 3.24 0.144 1.58 5 5 2 10317.53 16433.48 3.24 0.284 1.58 6 8 4 1185.94 2974.04 3.23 0.121 1.19 0 8 0 60818.01 88564.89 3.16 0.658 2.31 6 9 4 2520.55 4931.73 3.12 0.155 1.15 -2 8 10 19967.86 29453.08 3.10 0.380 1.44 -3 4 21 2143.40 207.56 3.09 0.032 0.88 -1 5 17 21.36 804.82 3.05 0.063 1.07 4 4 15 593.92 12.07 3.05 0.008 1.00 3 1 7 438.26 6.11 3.03 0.005 1.86 Bond lengths and angles C1 - Distance Angles O1 1.1390 (0.0169) Mo1 2.0068 (0.0141) 176.30 (1.28) C1 - O1 C2 - Distance Angles O2 1.0898 (0.0174) Mo1 2.0236 (0.0142) 176.57 (1.57) C2 - O2 C3 - Distance Angles C4 1.3744 (0.0218) C9 1.4078 (0.0234) 131.71 (1.52) Mo1 2.3189 (0.0143) 72.08 (0.82) 72.26 (0.84) H3 0.9500 114.15 114.15 138.47 C3 - C4 C9 Mo1 C4 - Distance Angles C3 1.3744 (0.0218) C5 1.4178 (0.0199) 127.31 (1.50) Mo1 2.3032 (0.0141) 73.33 (0.88) 70.14 (0.77) H4 0.9500 116.34 116.34 134.91 C4 - C3 C5 Mo1 C5 - Distance Angles C6 1.4167 (0.0211) C4 1.4178 (0.0199) 128.95 (1.39) Mo1 2.2575 (0.0132) 74.98 (0.84) 73.65 (0.80) H5 0.9500 115.53 115.53 128.85 C5 - C6 C4 Mo1 C6 - Distance Angles C7 1.3692 (0.0232) C5 1.4167 (0.0211) 126.50 (1.44) Mo1 2.3336 (0.0144) 71.37 (0.89) 69.12 (0.76) H6 0.9500 116.75 116.75 138.66 C6 - C7 C5 Mo1 C7 - Distance Angles C6 1.3692 (0.0231) C8 1.4203 (0.0246) 131.30 (1.54) Mo1 2.2976 (0.0148) 74.25 (0.86) 71.29 (0.88) H7 0.9500 114.35 114.35 135.89 C7 - C6 C8 Mo1 C8 - Distance Angles C9 1.4134 (0.0246) C7 1.4203 (0.0246) 127.79 (1.51) Mo1 2.2809 (0.0146) 73.51 (0.88) 72.57 (0.83) H8 0.9500 116.11 116.11 131.53 C8 - C9 C7 Mo1 C9 - Distance Angles C3 1.4078 (0.0234) C8 1.4134 (0.0246) 125.82 (1.46) Mo1 2.3173 (0.0141) 72.39 (0.84) 70.70 (0.82) H9 0.9500 117.09 117.09 134.03 C9 - C3 C8 Mo1 O1 - Distance Angles C1 1.1390 (0.0169) O1 - O2 - Distance Angles C2 1.0898 (0.0175) O2 - Ga1 - Distance Angles Mo1 2.6015 (0.0017) I3 2.6235 (0.0016) 124.36 (0.06) I2 2.6760 (0.0017) 112.47 (0.06) 101.66 (0.06) I1 2.6817 (0.0016) 111.72 (0.06) 101.08 (0.05) 103.00 (0.05) Ga1 - Mo1 I3 I2 Mo1 - Distance Angles C1 2.0068 (0.0142) C2 2.0236 (0.0143) 82.68 (0.61) C5 2.2575 (0.0132) 130.79 (0.55) 133.33 (0.59) C8 2.2809 (0.0147) 98.24 (0.59) 122.78 (0.63) 87.91 (0.57) C7 2.2976 (0.0150) 91.02 (0.58) 156.96 (0.63) 66.20 (0.56) 36.14 (0.63) C4 2.3032 (0.0141) 166.24 (0.56) 105.32 (0.60) 36.21 (0.51) 86.91 (0.58) 85.64 (0.57) C9 2.3173 (0.0142) 124.01 (0.58) 98.39 (0.59) 87.79 (0.51) 35.79 (0.62) 66.92 (0.60) 66.66 (0.54) C3 2.3189 (0.0144) 158.25 (0.58) 93.05 (0.59) 66.28 (0.52) 66.18 (0.61) 84.62 (0.58) 34.59 (0.54) 35.35 (0.58) C6 2.3336 (0.0145) 103.26 (0.57) 168.33 (0.62) 35.90 (0.54) 66.82 (0.61) 34.38 (0.58) 66.96 (0.55) 86.68 (0.55) Ga1 2.6015 (0.0017) 77.47 (0.40) 78.07 (0.42) 79.55 (0.35) 158.38 (0.48) 122.27 (0.43) 93.04 (0.38) 157.96 (0.43) Mo1 - C1 C2 C5 C8 C7 C4 C9 I1 - Distance Angles Ga1 2.6817 (0.0016) I1 - I2 - Distance Angles Ga1 2.6760 (0.0017) I2 - I3 - Distance Angles Ga1 2.6235 (0.0016) I3 - C10 - Distance Angles C15 1.5050 (0.0166) C11 1.5437 (0.0174) 111.15 (1.05) P1 1.8241 (0.0132) 115.01 (0.88) 114.34 (0.93) H10 1.0000 105.05 105.05 105.05 C10 - C15 C11 P1 C11 - Distance Angles C12 1.4946 (0.0177) C10 1.5437 (0.0174) 110.75 (1.16) H11A 0.9900 109.49 109.49 H11B 0.9900 109.49 109.49 108.07 C11 - C12 C10 H11A C12 - Distance Angles C11 1.4946 (0.0177) C13 1.5453 (0.0198) 110.98 (1.15) H12A 0.9900 109.44 109.44 H12B 0.9900 109.44 109.44 108.04 C12 - C11 C13 H12A C13 - Distance Angles C14 1.5421 (0.0209) C12 1.5453 (0.0198) 112.34 (1.16) H13A 0.9900 109.14 109.14 H13B 0.9900 109.14 109.13 107.86 C13 - C14 C12 H13A C14 - Distance Angles C15 1.5173 (0.0192) C13 1.5421 (0.0209) 110.34 (1.19) H14A 0.9900 109.59 109.59 H14B 0.9900 109.59 109.59 108.12 C14 - C15 C13 H14A C15 - Distance Angles C10 1.5050 (0.0166) C14 1.5173 (0.0192) 110.87 (1.12) H15A 0.9900 109.47 109.47 H15B 0.9900 109.47 109.47 108.05 C15 - C10 C14 H15A C16 - Distance Angles C21 1.5449 (0.0172) C17 1.5590 (0.0180) 111.86 (1.06) P1 1.8322 (0.0128) 112.81 (0.86) 112.66 (0.94) H16 1.0000 106.31 106.31 106.31 C16 - C21 C17 P1 C17 - Distance Angles C18 1.5178 (0.0189) C16 1.5590 (0.0180) 109.78 (1.12) H17A 0.9900 109.71 109.71 H17B 0.9900 109.71 109.71 108.19 C17 - C18 C16 H17A C18 - Distance Angles C17 1.5178 (0.0189) C19 1.5292 (0.0199) 112.28 (1.13) H18A 0.9900 109.15 109.15 H18B 0.9900 109.15 109.15 107.87 C18 - C17 C19 H18A C19 - Distance Angles C18 1.5292 (0.0199) C20 1.5391 (0.0203) 112.29 (1.05) H19A 0.9900 109.15 109.15 H19B 0.9900 109.15 109.15 107.87 C19 - C18 C20 H19A C20 - Distance Angles C21 1.5046 (0.0191) C19 1.5391 (0.0203) 112.24 (1.13) H20A 0.9900 109.16 109.16 H20B 0.9900 109.16 109.16 107.87 C20 - C21 C19 H20A C21 - Distance Angles C20 1.5046 (0.0191) C16 1.5449 (0.0173) 109.36 (1.13) H21A 0.9900 109.80 109.80 H21B 0.9900 109.80 109.80 108.25 C21 - C20 C16 H21A C22 - Distance Angles C27 1.5303 (0.0186) C23 1.5488 (0.0181) 108.65 (1.06) P1 1.8159 (0.0125) 112.13 (0.93) 111.88 (0.86) H22 1.0000 108.01 108.01 108.01 C22 - C27 C23 P1 C23 - Distance Angles C24 1.5233 (0.0182) C22 1.5488 (0.0182) 110.95 (1.12) H23A 0.9900 109.45 109.45 H23B 0.9900 109.45 109.45 108.04 C23 - C24 C22 H23A C24 - Distance Angles C25 1.5146 (0.0212) C23 1.5233 (0.0182) 112.79 (1.25) H24A 0.9900 109.03 109.03 H24B 0.9900 109.03 109.03 107.80 C24 - C25 C23 H24A C25 - Distance Angles C26 1.5104 (0.0205) C24 1.5146 (0.0212) 108.93 (1.15) H25A 0.9900 109.90 109.90 H25B 0.9900 109.90 109.90 108.31 C25 - C26 C24 H25A C26 - Distance Angles C25 1.5104 (0.0205) C27 1.5210 (0.0185) 112.11 (1.27) H26A 0.9900 109.19 109.19 H26B 0.9900 109.19 109.19 107.89 C26 - C25 C27 H26A C27 - Distance Angles C26 1.5210 (0.0185) C22 1.5303 (0.0186) 109.99 (1.21) H27A 0.9900 109.66 109.66 H27B 0.9900 109.66 109.66 108.17 C27 - C26 C22 H27A P1 - Distance Angles C22 1.8159 (0.0124) C10 1.8241 (0.0133) 108.81 (0.57) C16 1.8322 (0.0129) 110.69 (0.64) 117.59 (0.62) H1 1.4266 (0.0976) 115.87 (5.27) 102.29 (5.41) 101.49 (5.49) P1 - C22 C10 C16 FMAP and GRID set by program FMAP 2 3 22 GRID -1.316 -2 -2 1.316 2 2 R1 = 0.0933 for 5554 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 2.56 at 0.0740 0.7291 0.1108 [ 1.47 A from H1 ] Deepest hole -1.34 at 0.0160 0.8038 0.1059 [ 0.89 A from GA1 ] Mean = 0.00, Rms deviation from mean = 0.29 e/A^3, Highest memory used = 4940 / 25507 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9260 0.2709 0.8892 1.00000 0.05 2.56 1.47 H1 1.97 GA1 2.39 I1 2.45 I2 Q2 1 0.3025 0.2568 1.0536 1.00000 0.05 1.22 0.75 H6 1.30 C6 2.11 C5 2.17 H5 Q3 1 0.7069 0.4203 0.9963 1.00000 0.05 1.20 0.82 C27 0.83 C22 1.47 H22 1.48 H27A Q4 1 0.1678 0.3756 0.9193 1.00000 0.05 1.20 1.01 I1 2.59 H26A 2.68 H26B 2.95 H10 Q5 1 -0.0204 0.2343 0.7557 1.00000 0.05 1.19 0.77 I3 2.94 H15B 3.13 GA1 3.16 H20B Q6 1 0.1876 0.3675 0.9338 1.00000 0.05 1.17 0.85 I1 2.72 H26B 2.80 H26A 2.96 H23A Q7 1 -0.2038 0.1360 0.9675 1.00000 0.05 1.11 0.83 I2 2.48 H3 2.71 H9 2.97 H4 Q8 1 0.9441 0.3546 0.8634 1.00000 0.05 1.05 1.53 H1 1.83 H15B 1.97 H10 2.21 I1 Q9 1 0.0800 0.1337 0.9070 1.00000 0.05 1.04 1.17 GA1 1.86 C2 2.19 MO1 2.48 O2 Q10 1 0.7681 0.7110 0.7983 1.00000 0.05 1.02 1.48 H12B 1.89 H17B 2.33 H17A 2.40 C17 Shortest distances between peaks (including symmetry equivalents) 4 6 0.34 1 8 1.64 4 8 2.21 5 10 2.40 6 8 2.45 1 5 2.75 1 9 2.90 1 4 2.95 Time profile in seconds ----------------------- 0.08: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.02: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 1.14: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 4.70: Structure factors and derivatives 8.67: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.13: Apply other restraints 0.77: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.14: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0196 finished at 18:00:29 Total CPU time: 15.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++