data_ab1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H72 Li4 N4 O4' _chemical_formula_sum 'C52 H72 Li4 N4 O4' _chemical_formula_weight 844.90 _chemical_absolute_configuration unk loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.6188(7) _cell_length_b 21.8666(15) _cell_length_c 21.4263(13) _cell_angle_alpha 90.00 _cell_angle_beta 95.593(2) _cell_angle_gamma 90.00 _cell_volume 4951.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9973 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 19.47 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.133 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 0.070 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9661 _exptl_absorpt_correction_T_max 0.9983 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60393 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 0.95 _diffrn_reflns_theta_max 23.25 _reflns_number_total 6463 _reflns_number_gt 5396 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. c49-c52 group is disordered ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+0.4644P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0(10) _refine_ls_number_reflns 6463 _refine_ls_number_parameters 1222 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0810 _refine_ls_wR_factor_gt 0.0738 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL ab1 in P2(1) CELL 0.71073 10.6188 21.8666 21.4263 90.000 95.593 90.000 ZERR 4.00 0.0007 0.0015 0.0013 0.000 0.002 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H LI N O UNIT 208 288 16 16 16 TEMP -50 SIZE 0.025 0.25 0.50 SIMU c49a > c52a DELU c49a > C52a OMIT 1 0 0 SHEL 100 .9 L.S. 8 ACTA MERG 4 WGHT 0.046800 0.464400 FVAR 0.12068 0.55648 LI1 3 0.528966 0.900147 0.502083 11.00000 0.03978 0.03894 = 0.04598 0.00073 0.00957 -0.00304 LI2 3 0.672360 0.994227 0.506657 11.00000 0.03537 0.04021 = 0.04371 0.00196 0.00769 0.00081 LI3 3 0.582082 0.954122 0.605133 11.00000 0.03410 0.04058 = 0.04157 -0.00536 0.00942 -0.00436 LI4 3 0.749428 0.893217 0.558276 11.00000 0.03352 0.04676 = 0.04504 0.00601 0.00537 0.00834 O1 5 0.586652 0.866822 0.588262 11.00000 0.03759 0.03529 = 0.04105 -0.00211 0.00694 -0.00615 O2 5 0.691529 0.912062 0.473927 11.00000 0.04032 0.04499 = 0.03554 0.00275 0.01343 0.00582 O3 5 0.491356 0.981980 0.525598 11.00000 0.02705 0.04231 = 0.04412 -0.00424 0.00566 0.00351 O4 5 0.748628 0.977488 0.589509 11.00000 0.02862 0.04335 = 0.04126 0.00183 -0.00168 -0.00446 N1 4 0.409233 0.825768 0.479309 11.00000 0.03790 0.04362 = 0.04071 -0.00455 0.00386 -0.00114 N2 4 0.740639 1.023157 0.417344 11.00000 0.03926 0.04235 = 0.04516 0.00574 0.00586 -0.00365 N3 4 0.472781 1.010740 0.654814 11.00000 0.04392 0.03905 = 0.03974 -0.00234 0.01113 -0.00416 N4 4 0.931912 0.887375 0.615758 11.00000 0.03183 0.05291 = 0.09013 0.01760 -0.00286 0.00411 C1 1 0.456704 0.787222 0.533405 11.00000 0.04035 0.03516 = 0.05045 -0.00453 0.00725 -0.00784 C2 1 0.575051 0.751851 0.520679 11.00000 0.06446 0.04677 = 0.05540 -0.01351 0.00231 0.00868 AFIX 137 H2A 2 0.555621 0.724907 0.485078 11.00000 -1.50000 H2B 2 0.604077 0.727787 0.557314 11.00000 -1.50000 H2C 2 0.640845 0.780329 0.511538 11.00000 -1.50000 AFIX 0 C3 1 0.483095 0.828809 0.592845 11.00000 0.03396 0.03170 = 0.04497 -0.00006 0.00730 -0.00326 C4 1 0.488009 0.789289 0.650849 11.00000 0.05097 0.03763 = 0.04048 -0.00171 0.00536 -0.00910 C5 1 0.596175 0.760522 0.676064 11.00000 0.06271 0.06039 = 0.05985 0.01384 -0.00595 -0.01142 AFIX 43 H5A 2 0.672979 0.768514 0.659205 11.00000 -1.20000 AFIX 0 C6 1 0.594960 0.720087 0.725639 11.00000 0.08768 0.07563 = 0.07603 0.01202 -0.02745 -0.00078 AFIX 43 H6A 2 0.669693 0.700156 0.741586 11.00000 -1.20000 AFIX 0 C7 1 0.482044 0.709195 0.751681 11.00000 0.13226 0.05188 = 0.05547 0.00622 -0.00142 -0.03002 AFIX 43 H7A 2 0.479934 0.681335 0.784974 11.00000 -1.20000 AFIX 0 C8 1 0.376231 0.738480 0.729241 11.00000 0.09545 0.05275 = 0.06193 0.00721 0.02285 -0.02211 AFIX 43 H8A 2 0.300793 0.732379 0.747989 11.00000 -1.20000 AFIX 0 C9 1 0.377687 0.777545 0.678717 11.00000 0.06639 0.04159 = 0.05555 -0.00242 0.01444 -0.01164 AFIX 43 H9A 2 0.302085 0.796705 0.662743 11.00000 -1.20000 AFIX 0 C10 1 0.404468 0.795267 0.417685 11.00000 0.04996 0.06370 = 0.04877 -0.01737 0.00847 -0.00697 AFIX 23 H10A 2 0.367204 0.754368 0.419346 11.00000 -1.20000 H10B 2 0.489244 0.791742 0.403598 11.00000 -1.20000 AFIX 0 C11 1 0.322033 0.836715 0.375165 11.00000 0.06282 0.09625 = 0.04987 -0.00348 -0.00555 0.00294 AFIX 23 H11A 2 0.283675 0.814455 0.338413 11.00000 -1.20000 H11B 2 0.370614 0.871325 0.361073 11.00000 -1.20000 AFIX 0 C12 1 0.222280 0.858085 0.416069 11.00000 0.05295 0.08380 = 0.07219 0.00066 -0.01797 -0.00146 AFIX 23 H12A 2 0.142805 0.835859 0.405838 11.00000 -1.20000 H12B 2 0.206240 0.901964 0.410392 11.00000 -1.20000 AFIX 0 C13 1 0.276549 0.844532 0.482816 11.00000 0.03824 0.05660 = 0.06014 -0.00715 0.00735 0.00277 AFIX 23 H13A 2 0.272678 0.881027 0.509110 11.00000 -1.20000 H13B 2 0.228760 0.811649 0.500759 11.00000 -1.20000 AFIX 0 C14 1 0.783715 0.965229 0.390536 11.00000 0.04084 0.06089 = 0.03763 0.00206 0.00890 0.00015 AFIX 13 H14A 2 0.772535 0.968885 0.344273 11.00000 -1.20000 AFIX 0 C15 1 0.922855 0.951250 0.409970 11.00000 0.03682 0.07346 = 0.09976 -0.00057 0.01987 0.00018 AFIX 137 H15A 2 0.973981 0.986375 0.401098 11.00000 -1.50000 H15B 2 0.948747 0.916156 0.386650 11.00000 -1.50000 H15C 2 0.934259 0.942335 0.454510 11.00000 -1.50000 AFIX 0 C16 1 0.697121 0.912895 0.409610 11.00000 0.03098 0.04820 = 0.03667 0.00064 0.00629 0.00380 C17 1 0.736343 0.851129 0.385067 11.00000 0.04250 0.05051 = 0.04229 -0.00049 0.01553 0.00515 C18 1 0.811431 0.811011 0.421663 11.00000 0.07004 0.06382 = 0.05201 -0.00455 0.01619 0.01632 AFIX 43 H18A 2 0.842914 0.822753 0.462425 11.00000 -1.20000 AFIX 0 C19 1 0.841489 0.753962 0.399837 11.00000 0.08173 0.06372 = 0.08556 -0.00030 0.02587 0.02979 AFIX 43 H19A 2 0.894076 0.727954 0.425773 11.00000 -1.20000 AFIX 0 C20 1 0.796377 0.734578 0.341361 11.00000 0.08590 0.06195 = 0.08862 -0.02352 0.03486 0.00840 AFIX 43 H20A 2 0.815077 0.695210 0.327251 11.00000 -1.20000 AFIX 0 C21 1 0.722849 0.774177 0.303645 11.00000 0.07606 0.07111 = 0.06817 -0.02907 0.02661 -0.00949 AFIX 43 H21A 2 0.692141 0.762146 0.262861 11.00000 -1.20000 AFIX 0 C22 1 0.693751 0.831439 0.325163 11.00000 0.05974 0.06545 = 0.04681 -0.00629 0.01260 -0.00590 AFIX 43 H22A 2 0.643671 0.857843 0.298487 11.00000 -1.20000 AFIX 0 C23 1 0.629091 1.048391 0.380354 11.00000 0.05171 0.05423 = 0.06097 0.00949 -0.00166 0.00511 AFIX 23 H23A 2 0.553881 1.023714 0.385754 11.00000 -1.20000 H23B 2 0.642069 1.049473 0.335706 11.00000 -1.20000 AFIX 0 C24 1 0.614309 1.112260 0.405352 11.00000 0.07339 0.04993 = 0.08162 0.01916 0.00519 0.00326 AFIX 23 H24A 2 0.560703 1.112316 0.440084 11.00000 -1.20000 H24B 2 0.577341 1.139709 0.372345 11.00000 -1.20000 AFIX 0 C25 1 0.748993 1.131177 0.427686 11.00000 0.09430 0.04850 = 0.07222 0.00591 0.00088 -0.00767 AFIX 23 H25A 2 0.755669 1.142951 0.472017 11.00000 -1.20000 H25B 2 0.775750 1.165750 0.403037 11.00000 -1.20000 AFIX 0 C26 1 0.829930 1.074832 0.418121 11.00000 0.05557 0.06103 = 0.06305 0.00736 0.00555 -0.01394 AFIX 23 H26A 2 0.868244 1.077451 0.378405 11.00000 -1.20000 H26B 2 0.897287 1.070506 0.452498 11.00000 -1.20000 AFIX 0 C27 1 0.416064 1.050332 0.603169 11.00000 0.03700 0.03352 = 0.04392 -0.00153 0.00806 0.00450 C28 1 0.504938 1.101587 0.589314 11.00000 0.05502 0.03861 = 0.05102 -0.00048 0.00205 -0.00592 AFIX 137 H28A 2 0.511348 1.130559 0.623760 11.00000 -1.50000 H28B 2 0.472483 1.122201 0.550995 11.00000 -1.50000 H28C 2 0.587957 1.084860 0.584305 11.00000 -1.50000 AFIX 0 C29 1 0.383400 1.010183 0.544297 11.00000 0.02745 0.03763 = 0.05098 0.00058 0.01026 0.00020 C30 1 0.308610 1.045294 0.490669 11.00000 0.02637 0.04001 = 0.05512 0.00374 0.00462 -0.00122 C31 1 0.318251 1.027452 0.429901 11.00000 0.04570 0.07996 = 0.05065 0.00358 -0.00261 0.00524 AFIX 43 H31A 2 0.371724 0.994641 0.422102 11.00000 -1.20000 AFIX 0 C32 1 0.251155 1.056594 0.379819 11.00000 0.06297 0.11461 = 0.05651 0.00847 -0.00730 0.00255 AFIX 43 H32A 2 0.258863 1.043041 0.338732 11.00000 -1.20000 AFIX 0 C33 1 0.173245 1.105248 0.389662 11.00000 0.04964 0.08931 = 0.08927 0.02988 -0.01769 -0.00504 AFIX 43 H33A 2 0.129416 1.125812 0.355655 11.00000 -1.20000 AFIX 0 C34 1 0.161140 1.122761 0.449015 11.00000 0.05460 0.05913 = 0.09661 0.01549 -0.00693 0.01255 AFIX 43 H34A 2 0.106837 1.155370 0.456382 11.00000 -1.20000 AFIX 0 C35 1 0.227552 1.093466 0.499642 11.00000 0.04868 0.05802 = 0.07110 0.00801 -0.00085 0.01130 AFIX 43 H35A 2 0.217263 1.106571 0.540619 11.00000 -1.20000 AFIX 0 C36 1 0.531740 1.044647 0.709692 11.00000 0.05862 0.05579 = 0.04429 -0.00692 0.00594 0.00252 AFIX 23 H36A 2 0.475585 1.077076 0.722128 11.00000 -1.20000 H36B 2 0.612300 1.062885 0.700674 11.00000 -1.20000 AFIX 0 C37 1 0.552269 0.996261 0.760509 11.00000 0.07839 0.07950 = 0.04897 0.00295 0.00730 0.00486 AFIX 23 H37A 2 0.541477 1.013716 0.801777 11.00000 -1.20000 H37B 2 0.637377 0.978745 0.761426 11.00000 -1.20000 AFIX 0 C38 1 0.452311 0.947990 0.742923 11.00000 0.09591 0.06601 = 0.05239 0.01159 0.02090 0.00322 AFIX 23 H38A 2 0.395759 0.943371 0.776131 11.00000 -1.20000 H38B 2 0.491678 0.908388 0.735794 11.00000 -1.20000 AFIX 0 C39 1 0.380107 0.971502 0.682917 11.00000 0.06261 0.04852 = 0.05353 0.00237 0.02551 -0.00599 AFIX 23 H39A 2 0.352765 0.937632 0.654851 11.00000 -1.20000 H39B 2 0.305693 0.995123 0.692118 11.00000 -1.20000 AFIX 0 C40 1 0.962623 0.951905 0.630650 11.00000 0.03609 0.05991 = 0.06041 0.00838 -0.00830 -0.00458 AFIX 13 H40A 2 1.019473 0.953580 0.670080 11.00000 -1.20000 AFIX 0 C41 1 1.027139 0.983297 0.579060 11.00000 0.03769 0.07445 = 0.09624 0.00747 0.02528 -0.00309 AFIX 137 H41A 2 1.099421 0.959222 0.569334 11.00000 -1.50000 H41B 2 1.055338 1.023653 0.593065 11.00000 -1.50000 H41C 2 0.967833 0.987052 0.541857 11.00000 -1.50000 AFIX 0 C42 1 0.836832 0.985678 0.640749 11.00000 0.03336 0.05934 = 0.03573 0.00341 0.00090 -0.00722 AFIX 13 H42A 2 0.802208 0.966297 0.677182 11.00000 -1.20000 AFIX 0 C43 1 0.863147 1.051927 0.657629 11.00000 0.03656 0.06443 = 0.04511 -0.00697 0.00263 -0.01089 C44 1 0.845923 1.097875 0.613819 11.00000 0.04008 0.05252 = 0.07295 -0.00885 -0.00269 -0.00770 AFIX 43 H44A 2 0.818220 1.087835 0.572071 11.00000 -1.20000 AFIX 0 C45 1 0.868513 1.158973 0.629762 11.00000 0.05199 0.06043 = 0.12857 -0.01027 -0.00012 -0.01020 AFIX 43 H45A 2 0.856334 1.189738 0.599127 11.00000 -1.20000 AFIX 0 C46 1 0.908895 1.173712 0.690951 11.00000 0.08094 0.09239 = 0.14530 -0.06708 0.02115 -0.03163 AFIX 43 H46A 2 0.922979 1.214839 0.702349 11.00000 -1.20000 AFIX 0 C47 1 0.928505 1.128923 0.735017 11.00000 0.12414 0.14802 = 0.08754 -0.06358 0.02194 -0.06487 AFIX 43 H47A 2 0.957787 1.139020 0.776555 11.00000 -1.20000 AFIX 0 C48 1 0.905139 1.068388 0.718414 11.00000 0.09564 0.10058 = 0.05702 -0.02007 0.00341 -0.03616 AFIX 43 H48A 2 0.918159 1.037823 0.749216 11.00000 -1.20000 AFIX 0 PART 1 C49 1 0.890985 0.860363 0.680337 21.00000 0.06452 0.04293 = 0.08037 0.01750 -0.01139 0.00118 AFIX 23 H49A 2 0.927656 0.883775 0.716662 21.00000 -1.20000 H49B 2 0.798805 0.858690 0.680559 21.00000 -1.20000 AFIX 0 C50 1 0.950073 0.795509 0.677909 21.00000 0.08995 0.04542 = 0.18559 0.04083 -0.06520 -0.00453 AFIX 23 H50A 2 1.021046 0.791636 0.710507 21.00000 -1.20000 H50B 2 0.886733 0.764497 0.685541 21.00000 -1.20000 AFIX 0 C51 1 0.993248 0.786308 0.617719 21.00000 0.08192 AFIX 23 H51A 2 0.925111 0.772602 0.586736 21.00000 -1.20000 H51B 2 1.063922 0.757355 0.619200 21.00000 -1.20000 AFIX 0 C52 1 1.034508 0.850747 0.605345 21.00000 0.07697 AFIX 23 H52A 2 1.108768 0.861890 0.633854 21.00000 -1.20000 H52B 2 1.055626 0.855015 0.562043 21.00000 -1.20000 AFIX 0 PART 2 C49A 1 0.907503 0.843933 0.660896 -21.00000 0.05654 0.06562 = 0.06553 0.00713 0.01110 0.01158 AFIX 23 H49C 2 0.824596 0.852096 0.675610 -21.00000 -1.20000 H49D 2 0.971525 0.847336 0.696894 -21.00000 -1.20000 AFIX 0 C50A 1 0.909088 0.779456 0.634449 -21.00000 0.08499 0.05122 = 0.09218 0.02267 0.02917 0.00568 AFIX 23 H50C 2 0.934717 0.749386 0.667159 -21.00000 -1.20000 H50D 2 0.826465 0.767964 0.613322 -21.00000 -1.20000 AFIX 0 C51A 1 1.013054 0.786353 0.585887 -21.00000 0.05726 AFIX 23 H51C 2 0.981387 0.769393 0.545007 -21.00000 -1.20000 H51D 2 1.090605 0.764544 0.601187 -21.00000 -1.20000 AFIX 0 C52A 1 1.039187 0.853935 0.580213 -21.00000 0.04257 AFIX 23 H52C 2 1.123698 0.864045 0.600041 -21.00000 -1.20000 H52D 2 1.033666 0.866302 0.536068 -21.00000 -1.20000 AFIX 0 PART 0 LI1' 3 0.255878 0.953329 0.090857 11.00000 0.03415 0.04730 = 0.04690 -0.00128 0.00095 -0.00339 LI2' 3 0.057182 0.892437 0.084561 11.00000 0.03795 0.04121 = 0.04738 0.00702 0.00219 0.00176 LI3' 3 0.176639 0.906225 -0.013483 11.00000 0.04220 0.03993 = 0.04954 -0.00381 0.00753 -0.00030 LI4' 3 0.058731 0.994262 0.027238 11.00000 0.03480 0.03534 = 0.05021 0.00505 0.00512 0.00160 O1' 5 0.227368 0.989522 0.005393 11.00000 0.03286 0.04246 = 0.04668 0.00175 0.00428 -0.00804 O2' 5 0.091269 0.977746 0.115535 11.00000 0.04063 0.04286 = 0.04296 0.00435 0.01221 0.00237 O3' 5 0.225230 0.870194 0.068877 11.00000 0.03717 0.03862 = 0.04761 -0.00189 0.00464 0.00544 O4' 5 -0.006394 0.913170 0.000286 11.00000 0.02732 0.03979 = 0.04857 0.00551 -0.00464 -0.00044 N1' 4 0.432468 1.003782 0.101569 11.00000 0.03397 0.05343 = 0.05476 -0.00170 -0.00365 -0.00393 N2' 4 -0.034372 0.871678 0.165849 11.00000 0.04096 0.04176 = 0.05011 0.00961 0.00579 0.00283 N3' 4 0.260632 0.826115 -0.051291 11.00000 0.04404 0.04552 = 0.04638 -0.00190 0.01257 -0.00031 N4' 4 -0.087697 1.034512 -0.029305 11.00000 0.04570 0.03329 = 0.06604 0.01203 -0.00301 -0.00080 C1' 1 0.440736 1.024631 0.035665 11.00000 0.03161 0.04831 = 0.05736 -0.00114 0.00855 -0.00750 AFIX 13 H1'A 2 0.493195 1.062107 0.036570 11.00000 -1.20000 AFIX 0 C2' 1 0.498106 0.977462 -0.004646 11.00000 0.03827 0.05681 = 0.07339 -0.00238 0.01242 0.00637 AFIX 137 H2'1 2 0.579920 0.964953 0.015371 11.00000 -1.50000 H2'2 2 0.508557 0.994966 -0.045419 11.00000 -1.50000 H2'3 2 0.442665 0.942190 -0.009767 11.00000 -1.50000 AFIX 0 C3' 1 0.305606 1.040575 0.006292 11.00000 0.03352 0.03444 = 0.04740 -0.00496 0.00877 -0.00167 C4' 1 0.311862 1.070931 -0.056571 11.00000 0.03502 0.03994 = 0.05456 0.00257 0.01525 0.00131 C5' 1 0.270924 1.041757 -0.111862 11.00000 0.05468 0.05279 = 0.05463 0.00541 0.02107 -0.00123 AFIX 43 H5'A 2 0.239922 1.001564 -0.110488 11.00000 -1.20000 AFIX 0 C6' 1 0.274368 1.070298 -0.169534 11.00000 0.07383 0.07240 = 0.05535 0.00344 0.02249 0.00659 AFIX 43 H6'A 2 0.243415 1.049997 -0.206558 11.00000 -1.20000 AFIX 0 C7' 1 0.322846 1.127940 -0.172313 11.00000 0.08918 0.07086 = 0.07550 0.02907 0.03540 0.02534 AFIX 43 H7'A 2 0.326143 1.147316 -0.211282 11.00000 -1.20000 AFIX 0 C8' 1 0.366468 1.157309 -0.118361 11.00000 0.09540 0.04268 = 0.09900 0.01989 0.03318 0.00285 AFIX 43 H8'A 2 0.401191 1.196712 -0.120468 11.00000 -1.20000 AFIX 0 C9' 1 0.360334 1.130041 -0.060903 11.00000 0.06250 0.04386 = 0.07981 0.00603 0.01654 0.00156 AFIX 43 H9'A 2 0.389039 1.151376 -0.024160 11.00000 -1.20000 AFIX 0 C10' 1 0.419401 1.056170 0.144189 11.00000 0.05172 0.07086 = 0.05804 -0.01564 0.00011 -0.00055 AFIX 23 H10C 2 0.334291 1.073794 0.137583 11.00000 -1.20000 H10D 2 0.481552 1.088056 0.137529 11.00000 -1.20000 AFIX 0 C11' 1 0.443258 1.029376 0.209059 11.00000 0.08700 0.08507 = 0.06091 -0.00605 -0.01006 0.00156 AFIX 23 H11C 2 0.363513 1.017840 0.225364 11.00000 -1.20000 H11D 2 0.487769 1.058695 0.237942 11.00000 -1.20000 AFIX 0 C12' 1 0.524677 0.973413 0.200835 11.00000 0.06834 0.07539 = 0.06655 0.00356 -0.01883 -0.01202 AFIX 23 H12C 2 0.481466 0.936163 0.212624 11.00000 -1.20000 H12D 2 0.605719 0.976700 0.226724 11.00000 -1.20000 AFIX 0 C13' 1 0.545055 0.972386 0.131105 11.00000 0.04063 0.06744 = 0.07662 0.00128 -0.00781 0.00021 AFIX 23 H13C 2 0.622550 0.994239 0.123292 11.00000 -1.20000 H13D 2 0.549910 0.930351 0.115657 11.00000 -1.20000 AFIX 0 C14' 1 -0.002387 0.928817 0.201124 11.00000 0.04668 0.04921 = 0.04015 0.00606 0.01030 0.00780 C15' 1 0.125755 0.925852 0.238972 11.00000 0.06671 0.06270 = 0.05197 0.00792 -0.00631 0.00369 AFIX 137 H15D 2 0.123682 0.895277 0.271656 11.00000 -1.50000 H15E 2 0.145735 0.965430 0.257849 11.00000 -1.50000 H15F 2 0.189838 0.914950 0.211626 11.00000 -1.50000 AFIX 0 C16' 1 -0.007163 0.981886 0.153536 11.00000 0.03384 0.04426 = 0.03754 0.00519 0.00467 -0.00024 C17' 1 -0.017718 1.043643 0.184303 11.00000 0.04484 0.04577 = 0.03830 0.00563 0.00327 0.01030 C18' 1 0.068626 1.089464 0.178345 11.00000 0.05028 0.05196 = 0.08705 -0.01081 0.00435 0.00378 AFIX 43 H18B 2 0.140167 1.081643 0.156984 11.00000 -1.20000 AFIX 0 C19' 1 0.052058 1.147403 0.203424 11.00000 0.06912 0.05640 = 0.11252 -0.01436 -0.01381 -0.00504 AFIX 43 H19B 2 0.110910 1.178644 0.198174 11.00000 -1.20000 AFIX 0 C20' 1 -0.050642 1.158440 0.235771 11.00000 0.09557 0.06415 = 0.06792 -0.02411 -0.00499 0.02703 AFIX 43 H20B 2 -0.060507 1.196826 0.254434 11.00000 -1.20000 AFIX 0 C21' 1 -0.139037 1.113528 0.240937 11.00000 0.11216 0.06355 = 0.07745 0.00979 0.04440 0.02306 AFIX 43 H21B 2 -0.211560 1.121724 0.261416 11.00000 -1.20000 AFIX 0 C22' 1 -0.121871 1.057117 0.216450 11.00000 0.08458 0.05038 = 0.07812 0.00751 0.03795 0.01017 AFIX 43 H22B 2 -0.182037 1.026404 0.221388 11.00000 -1.20000 AFIX 0 C23' 1 -0.006135 0.814521 0.201418 11.00000 0.05339 0.05642 = 0.06571 0.02327 0.01162 0.00278 AFIX 23 H23C 2 -0.036036 0.816827 0.243205 11.00000 -1.20000 H23D 2 0.084878 0.805937 0.205810 11.00000 -1.20000 AFIX 0 C24' 1 -0.077956 0.766477 0.161687 11.00000 0.07763 0.04687 = 0.09466 0.01421 0.01800 -0.00964 AFIX 23 H24C 2 -0.097462 0.731116 0.187147 11.00000 -1.20000 H24D 2 -0.029148 0.752658 0.127802 11.00000 -1.20000 AFIX 0 C25' 1 -0.199293 0.799172 0.135346 11.00000 0.06799 0.06534 = 0.06988 0.01723 0.00648 -0.01729 AFIX 23 H25C 2 -0.217898 0.790735 0.090474 11.00000 -1.20000 H25D 2 -0.271437 0.786070 0.157297 11.00000 -1.20000 AFIX 0 C26' 1 -0.171835 0.866500 0.146538 11.00000 0.04267 0.06326 = 0.06682 0.01320 0.00511 -0.00378 AFIX 23 H26C 2 -0.194427 0.889973 0.108111 11.00000 -1.20000 H26D 2 -0.220735 0.882248 0.179560 11.00000 -1.20000 AFIX 0 C27' 1 0.322213 0.795649 0.005082 11.00000 0.04244 0.03763 = 0.05670 -0.00326 0.00779 0.00271 AFIX 13 H27A 2 0.321389 0.751041 -0.002848 11.00000 -1.20000 AFIX 0 C28' 1 0.459272 0.815237 0.021511 11.00000 0.04295 0.06534 = 0.07170 0.00246 0.01475 0.00274 AFIX 137 H28D 2 0.506077 0.809929 -0.014792 11.00000 -1.50000 H28E 2 0.497166 0.790338 0.055815 11.00000 -1.50000 H28F 2 0.461752 0.857903 0.033962 11.00000 -1.50000 AFIX 0 C29' 1 0.242528 0.808116 0.060704 11.00000 0.03336 0.03871 = 0.04921 0.00014 0.00153 0.00106 C30' 1 0.296976 0.775344 0.119760 11.00000 0.03218 0.03856 = 0.05424 0.00263 0.00188 0.00323 C31' 1 0.357066 0.807210 0.169349 11.00000 0.05164 0.05005 = 0.06187 -0.00117 -0.00562 0.01014 AFIX 43 H31B 2 0.365196 0.849898 0.166471 11.00000 -1.20000 AFIX 0 C32' 1 0.405653 0.777621 0.223274 11.00000 0.06523 0.07274 = 0.06135 -0.00204 -0.00501 0.01406 AFIX 43 H32B 2 0.447032 0.800314 0.256447 11.00000 -1.20000 AFIX 0 C33' 1 0.394247 0.715634 0.228970 11.00000 0.07442 0.08244 = 0.06051 0.02426 0.00061 0.01743 AFIX 43 H33B 2 0.426627 0.695759 0.266005 11.00000 -1.20000 AFIX 0 C34' 1 0.335305 0.682905 0.180275 11.00000 0.08739 0.05325 = 0.09316 0.02572 -0.00255 -0.00348 AFIX 43 H34B 2 0.327303 0.640229 0.183384 11.00000 -1.20000 AFIX 0 C35' 1 0.287390 0.713104 0.126249 11.00000 0.06398 0.05245 = 0.06829 0.00690 -0.01137 -0.00612 AFIX 43 H35B 2 0.246999 0.690224 0.092952 11.00000 -1.20000 AFIX 0 C36' 1 0.149633 0.790970 -0.079339 11.00000 0.06744 0.06480 = 0.05901 0.00103 0.00307 -0.01276 AFIX 23 H36C 2 0.077068 0.796872 -0.055011 11.00000 -1.20000 H36D 2 0.169369 0.747220 -0.080309 11.00000 -1.20000 AFIX 0 C37' 1 0.120890 0.815427 -0.144921 11.00000 0.09835 0.06694 = 0.05287 -0.00280 0.00064 -0.01165 AFIX 23 H37C 2 0.047033 0.842505 -0.147374 11.00000 -1.20000 H37D 2 0.103888 0.781873 -0.174880 11.00000 -1.20000 AFIX 0 C38' 1 0.238530 0.850554 -0.158778 11.00000 0.10077 0.06912 = 0.05114 -0.00838 0.01690 0.00178 AFIX 23 H38C 2 0.266264 0.838376 -0.199276 11.00000 -1.20000 H38D 2 0.223055 0.894741 -0.159114 11.00000 -1.20000 AFIX 0 C39' 1 0.335934 0.832745 -0.105092 11.00000 0.07371 0.05968 = 0.06766 -0.00699 0.03010 -0.00492 AFIX 23 H39C 2 0.377609 0.794182 -0.114063 11.00000 -1.20000 H39D 2 0.400306 0.864670 -0.097254 11.00000 -1.20000 AFIX 0 C40' 1 -0.131066 0.981710 -0.069386 11.00000 0.03833 0.04555 = 0.04997 0.01036 -0.00507 0.00162 C41' 1 -0.049395 0.971795 -0.122855 11.00000 0.07322 0.06614 = 0.05606 0.02059 0.00620 -0.00311 AFIX 137 H41D 2 -0.055112 1.007301 -0.150122 11.00000 -1.50000 H41E 2 -0.078766 0.935915 -0.146609 11.00000 -1.50000 H41F 2 0.037868 0.965833 -0.105994 11.00000 -1.50000 AFIX 0 C42' 1 -0.129068 0.924701 -0.026825 11.00000 0.03182 0.04038 = 0.04463 0.00193 -0.00031 -0.00023 C45' 1 -0.216208 0.758559 -0.058711 11.00000 0.05503 0.04468 = 0.09456 0.00085 -0.00685 -0.00229 AFIX 43 H45B 2 -0.194969 0.720638 -0.039872 11.00000 -1.20000 AFIX 0 C46' 1 -0.302737 0.761084 -0.110637 11.00000 0.05423 0.05433 = 0.08880 -0.01813 -0.00523 -0.00947 AFIX 43 H46B 2 -0.338241 0.725046 -0.128643 11.00000 -1.20000 AFIX 0 C47' 1 -0.336389 0.817005 -0.135723 11.00000 0.04853 0.07337 = 0.07566 -0.01026 -0.01415 -0.00299 AFIX 43 H47B 2 -0.397088 0.819496 -0.170622 11.00000 -1.20000 AFIX 0 C48' 1 -0.281376 0.870159 -0.109923 11.00000 0.04652 0.05336 = 0.06227 -0.00005 -0.01061 0.00094 AFIX 43 H48B 2 -0.306599 0.908158 -0.127453 11.00000 -1.20000 AFIX 0 C43' 1 -0.190288 0.868493 -0.059007 11.00000 0.03152 0.04784 = 0.04672 0.00331 0.00160 0.00144 C44' 1 -0.160289 0.811310 -0.034037 11.00000 0.03983 0.04847 = 0.06644 0.00223 -0.00790 -0.00624 AFIX 43 H44B 2 -0.099783 0.808359 0.000901 11.00000 -1.20000 AFIX 0 C49' 1 -0.049273 1.089552 -0.062842 11.00000 0.05434 0.04516 = 0.09486 0.02465 0.00362 0.00271 AFIX 23 H49E 2 -0.113817 1.101311 -0.096528 11.00000 -1.20000 H49F 2 0.031548 1.083222 -0.080411 11.00000 -1.20000 AFIX 0 C50' 1 -0.037322 1.136830 -0.010804 11.00000 0.06252 0.04136 = 0.12666 0.00404 -0.02617 -0.00006 AFIX 23 H50E 2 -0.048226 1.178241 -0.027973 11.00000 -1.20000 H50F 2 0.045556 1.134073 0.013522 11.00000 -1.20000 AFIX 0 C51' 1 -0.143355 1.121092 0.029935 11.00000 0.08573 0.04829 = 0.08682 0.00431 -0.01316 0.01066 AFIX 23 H51E 2 -0.111581 1.120278 0.074431 11.00000 -1.20000 H51F 2 -0.212365 1.150903 0.023818 11.00000 -1.20000 AFIX 0 C52' 1 -0.187682 1.058164 0.007674 11.00000 0.05547 0.04888 = 0.07090 -0.00102 -0.00279 0.00882 AFIX 23 H52E 2 -0.198156 1.031357 0.043457 11.00000 -1.20000 H52F 2 -0.268648 1.060887 -0.018359 11.00000 -1.20000 AFIX 0 H29 2 0.324041 0.978922 0.558271 11.00000 0.03376 H16' 2 -0.091911 0.977693 0.127268 11.00000 0.05020 H1 2 0.388940 0.758930 0.540786 11.00000 0.03716 H3' 2 0.274940 1.073197 0.032927 11.00000 0.02657 H29' 2 0.153898 0.788726 0.047884 11.00000 0.03093 H40' 2 -0.220734 0.989923 -0.088467 11.00000 0.05064 H16 2 0.611897 0.921624 0.387174 11.00000 0.03425 H14' 2 -0.066263 0.935553 0.230582 11.00000 0.04514 H42' 2 -0.186893 0.934342 0.009799 11.00000 0.03447 H3 2 0.402948 0.854526 0.594380 11.00000 0.03849 H27 2 0.337028 1.069045 0.615917 11.00000 0.04985 HKLF 4 REM ab1 in P2(1) REM R1 = 0.0339 for 5396 Fo > 4sig(Fo) and 0.0491 for all 6463 data REM 1222 parameters refined using 15 restraints END WGHT 0.0438 0.6172 REM Highest difference peak 0.109, deepest hole -0.165, 1-sigma level 0.029 Q1 1 0.9539 0.7417 0.4611 11.00000 0.05 0.11 Q2 1 0.3015 0.6815 0.0637 11.00000 0.05 0.10 Q3 1 0.0843 0.7518 -0.0449 11.00000 0.05 0.10 Q4 1 -0.3544 1.1249 -0.0615 11.00000 0.05 0.10 Q5 1 -0.1137 0.7001 -0.1073 11.00000 0.05 0.10 Q6 1 0.4050 0.7108 0.4505 11.00000 0.05 0.10 Q7 1 0.2736 0.9570 0.2849 11.00000 0.05 0.09 Q8 1 0.5181 0.6454 0.7094 11.00000 0.05 0.09 Q9 1 0.0853 0.8801 0.3031 11.00000 0.05 0.09 Q10 1 0.5065 0.8568 0.0662 11.00000 0.05 0.09 Q11 1 0.8856 0.7720 0.7050 11.00000 0.05 0.09 Q12 1 0.5001 0.8302 0.2672 11.00000 0.05 0.09 Q13 1 0.0567 1.0529 0.2926 11.00000 0.05 0.09 Q14 1 0.1014 0.8890 0.2915 11.00000 0.05 0.09 Q15 1 0.1628 1.0971 0.0511 11.00000 0.05 0.09 Q16 1 0.9080 0.7785 0.5003 11.00000 0.05 0.09 Q17 1 -0.0395 0.8307 0.3133 11.00000 0.05 0.09 Q18 1 -0.3579 1.0378 -0.1024 11.00000 0.05 0.09 Q19 1 0.3714 0.8805 0.3038 11.00000 0.05 0.09 Q20 1 1.0895 0.9528 0.5247 11.00000 0.05 0.09 ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.5290(5) 0.9001(3) 0.5021(2) 0.0412(13) Uani 1 1 d . . . Li2 Li 0.6724(5) 0.9942(3) 0.5067(2) 0.0395(13) Uani 1 1 d . . . Li3 Li 0.5821(4) 0.9541(3) 0.6051(2) 0.0384(13) Uani 1 1 d . . . Li4 Li 0.7494(5) 0.8932(3) 0.5583(2) 0.0417(14) Uani 1 1 d . A . O1 O 0.58665(18) 0.86682(10) 0.58826(9) 0.0378(5) Uani 1 1 d . . . O2 O 0.69153(18) 0.91206(10) 0.47393(9) 0.0396(5) Uani 1 1 d . . . O3 O 0.49136(17) 0.98198(10) 0.52560(9) 0.0377(5) Uani 1 1 d . . . O4 O 0.74863(17) 0.97749(10) 0.58951(9) 0.0381(5) Uani 1 1 d . A . N1 N 0.4092(2) 0.82577(13) 0.47931(12) 0.0407(7) Uani 1 1 d . . . N2 N 0.7406(2) 1.02316(13) 0.41734(12) 0.0421(7) Uani 1 1 d . . . N3 N 0.4728(2) 1.01074(13) 0.65481(12) 0.0404(7) Uani 1 1 d . . . N4 N 0.9319(2) 0.88738(16) 0.61576(16) 0.0589(9) Uani 1 1 d . . . C1 C 0.4567(3) 0.78722(16) 0.53340(16) 0.0418(9) Uani 1 1 d . . . C2 C 0.5751(3) 0.75185(18) 0.52068(17) 0.0558(10) Uani 1 1 d . . . H2A H 0.5556 0.7249 0.4851 0.084 Uiso 1 1 calc R . . H2B H 0.6041 0.7278 0.5573 0.084 Uiso 1 1 calc R . . H2C H 0.6408 0.7803 0.5115 0.084 Uiso 1 1 calc R . . C3 C 0.4831(3) 0.82881(16) 0.59285(14) 0.0366(8) Uani 1 1 d . . . C4 C 0.4880(3) 0.78929(16) 0.65085(15) 0.0430(9) Uani 1 1 d . . . C5 C 0.5962(4) 0.76052(19) 0.67606(18) 0.0618(11) Uani 1 1 d . . . H5A H 0.6730 0.7685 0.6592 0.074 Uiso 1 1 calc R . . C6 C 0.5950(5) 0.7201(2) 0.7256(2) 0.0821(14) Uani 1 1 d . . . H6A H 0.6697 0.7002 0.7416 0.099 Uiso 1 1 calc R . . C7 C 0.4820(6) 0.7092(2) 0.7517(2) 0.0806(15) Uani 1 1 d . . . H7A H 0.4799 0.6813 0.7850 0.097 Uiso 1 1 calc R . . C8 C 0.3762(5) 0.7385(2) 0.7292(2) 0.0690(12) Uani 1 1 d . . . H8A H 0.3008 0.7324 0.7480 0.083 Uiso 1 1 calc R . . C9 C 0.3777(4) 0.77755(17) 0.67872(17) 0.0540(10) Uani 1 1 d . . . H9A H 0.3021 0.7967 0.6627 0.065 Uiso 1 1 calc R . . C10 C 0.4045(3) 0.79527(19) 0.41768(16) 0.0539(10) Uani 1 1 d . . . H10A H 0.3672 0.7544 0.4193 0.065 Uiso 1 1 calc R . . H10B H 0.4892 0.7917 0.4036 0.065 Uiso 1 1 calc R . . C11 C 0.3220(4) 0.8367(2) 0.37516(18) 0.0704(12) Uani 1 1 d . . . H11A H 0.2837 0.8145 0.3384 0.084 Uiso 1 1 calc R . . H11B H 0.3706 0.8713 0.3611 0.084 Uiso 1 1 calc R . . C12 C 0.2223(4) 0.8581(2) 0.41607(18) 0.0712(12) Uani 1 1 d . . . H12A H 0.1428 0.8359 0.4058 0.085 Uiso 1 1 calc R . . H12B H 0.2062 0.9020 0.4104 0.085 Uiso 1 1 calc R . . C13 C 0.2765(3) 0.84453(18) 0.48282(17) 0.0515(10) Uani 1 1 d . . . H13A H 0.2727 0.8810 0.5091 0.062 Uiso 1 1 calc R . . H13B H 0.2288 0.8116 0.5008 0.062 Uiso 1 1 calc R . . C14 C 0.7837(3) 0.96523(17) 0.39054(15) 0.0461(9) Uani 1 1 d . . . H14A H 0.7725 0.9689 0.3443 0.055 Uiso 1 1 calc R . . C15 C 0.9229(3) 0.9513(2) 0.4100(2) 0.0691(12) Uani 1 1 d . . . H15A H 0.9740 0.9864 0.4011 0.104 Uiso 1 1 calc R . . H15B H 0.9487 0.9162 0.3866 0.104 Uiso 1 1 calc R . . H15C H 0.9343 0.9423 0.4545 0.104 Uiso 1 1 calc R . . C16 C 0.6971(3) 0.91289(16) 0.40961(15) 0.0384(8) Uani 1 1 d . . . C17 C 0.7363(3) 0.85113(17) 0.38507(15) 0.0444(9) Uani 1 1 d . . . C18 C 0.8114(4) 0.8110(2) 0.42166(18) 0.0613(11) Uani 1 1 d . . . H18A H 0.8429 0.8228 0.4624 0.074 Uiso 1 1 calc R . . C19 C 0.8415(4) 0.7540(2) 0.3998(2) 0.0758(13) Uani 1 1 d . . . H19A H 0.8941 0.7280 0.4258 0.091 Uiso 1 1 calc R . . C20 C 0.7964(5) 0.7346(2) 0.3414(2) 0.0771(13) Uani 1 1 d . . . H20A H 0.8151 0.6952 0.3273 0.093 Uiso 1 1 calc R . . C21 C 0.7228(4) 0.7742(2) 0.3036(2) 0.0705(12) Uani 1 1 d . . . H21A H 0.6921 0.7621 0.2629 0.085 Uiso 1 1 calc R . . C22 C 0.6938(3) 0.8314(2) 0.32516(17) 0.0568(10) Uani 1 1 d . . . H22A H 0.6437 0.8578 0.2985 0.068 Uiso 1 1 calc R . . C23 C 0.6291(3) 1.04839(18) 0.38035(18) 0.0561(10) Uani 1 1 d . . . H23A H 0.5539 1.0237 0.3858 0.067 Uiso 1 1 calc R . . H23B H 0.6421 1.0495 0.3357 0.067 Uiso 1 1 calc R . . C24 C 0.6143(4) 1.11226(19) 0.4054(2) 0.0685(12) Uani 1 1 d . . . H24A H 0.5607 1.1123 0.4401 0.082 Uiso 1 1 calc R . . H24B H 0.5773 1.1397 0.3723 0.082 Uiso 1 1 calc R . . C25 C 0.7490(4) 1.1312(2) 0.4277(2) 0.0721(12) Uani 1 1 d . . . H25A H 0.7557 1.1430 0.4720 0.087 Uiso 1 1 calc R . . H25B H 0.7757 1.1657 0.4030 0.087 Uiso 1 1 calc R . . C26 C 0.8299(3) 1.07483(19) 0.41812(19) 0.0599(11) Uani 1 1 d . . . H26A H 0.8682 1.0775 0.3784 0.072 Uiso 1 1 calc R . . H26B H 0.8973 1.0705 0.4525 0.072 Uiso 1 1 calc R . . C27 C 0.4161(3) 1.05033(16) 0.60317(15) 0.0379(8) Uani 1 1 d . . . C28 C 0.5049(3) 1.10159(16) 0.58931(16) 0.0484(9) Uani 1 1 d . . . H28A H 0.5113 1.1306 0.6238 0.073 Uiso 1 1 calc R . . H28B H 0.4725 1.1222 0.5510 0.073 Uiso 1 1 calc R . . H28C H 0.5880 1.0849 0.5843 0.073 Uiso 1 1 calc R . . C29 C 0.3834(3) 1.01018(16) 0.54430(15) 0.0383(8) Uani 1 1 d . . . C30 C 0.3086(3) 1.04529(16) 0.49067(16) 0.0405(9) Uani 1 1 d . . . C31 C 0.3183(3) 1.0275(2) 0.42990(17) 0.0592(11) Uani 1 1 d . . . H31A H 0.3717 0.9946 0.4221 0.071 Uiso 1 1 calc R . . C32 C 0.2512(4) 1.0566(3) 0.3798(2) 0.0789(14) Uani 1 1 d . . . H32A H 0.2589 1.0430 0.3387 0.095 Uiso 1 1 calc R . . C33 C 0.1732(4) 1.1052(2) 0.3897(3) 0.0777(14) Uani 1 1 d . . . H33A H 0.1294 1.1258 0.3557 0.093 Uiso 1 1 calc R . . C34 C 0.1611(4) 1.1228(2) 0.4490(2) 0.0711(12) Uani 1 1 d . . . H34A H 0.1068 1.1554 0.4564 0.085 Uiso 1 1 calc R . . C35 C 0.2276(3) 1.09347(19) 0.49964(19) 0.0597(11) Uani 1 1 d . . . H35A H 0.2173 1.1066 0.5406 0.072 Uiso 1 1 calc R . . C36 C 0.5317(3) 1.04465(18) 0.70969(15) 0.0528(10) Uani 1 1 d . . . H36A H 0.4756 1.0771 0.7221 0.063 Uiso 1 1 calc R . . H36B H 0.6123 1.0629 0.7007 0.063 Uiso 1 1 calc R . . C37 C 0.5523(4) 0.9963(2) 0.76051(17) 0.0689(12) Uani 1 1 d . . . H37A H 0.5415 1.0137 0.8018 0.083 Uiso 1 1 calc R . . H37B H 0.6374 0.9787 0.7614 0.083 Uiso 1 1 calc R . . C38 C 0.4523(4) 0.9480(2) 0.74292(18) 0.0705(12) Uani 1 1 d . . . H38A H 0.3958 0.9434 0.7761 0.085 Uiso 1 1 calc R . . H38B H 0.4917 0.9084 0.7358 0.085 Uiso 1 1 calc R . . C39 C 0.3801(3) 0.97150(18) 0.68292(16) 0.0536(10) Uani 1 1 d . . . H39A H 0.3528 0.9376 0.6549 0.064 Uiso 1 1 calc R . . H39B H 0.3057 0.9951 0.6921 0.064 Uiso 1 1 calc R . . C40 C 0.9626(3) 0.95190(19) 0.63065(18) 0.0530(10) Uani 1 1 d . A . H40A H 1.0195 0.9536 0.6701 0.064 Uiso 1 1 calc R . . C41 C 1.0271(3) 0.9833(2) 0.57906(19) 0.0682(12) Uani 1 1 d . . . H41A H 1.0994 0.9592 0.5693 0.102 Uiso 1 1 calc R A . H41B H 1.0553 1.0237 0.5931 0.102 Uiso 1 1 calc R . . H41C H 0.9678 0.9871 0.5419 0.102 Uiso 1 1 calc R . . C42 C 0.8368(3) 0.98568(18) 0.64075(14) 0.0430(9) Uani 1 1 d . . . H42A H 0.8022 0.9663 0.6772 0.052 Uiso 1 1 calc R A . C43 C 0.8631(3) 1.05193(19) 0.65763(16) 0.0488(10) Uani 1 1 d . A . C44 C 0.8459(3) 1.09787(19) 0.6138(2) 0.0557(10) Uani 1 1 d . . . H44A H 0.8182 1.0878 0.5721 0.067 Uiso 1 1 calc R A . C45 C 0.8685(4) 1.1590(2) 0.6298(3) 0.0809(14) Uani 1 1 d . A . H45A H 0.8563 1.1897 0.5991 0.097 Uiso 1 1 calc R . . C46 C 0.9089(5) 1.1737(3) 0.6910(4) 0.106(2) Uani 1 1 d . . . H46A H 0.9230 1.2148 0.7023 0.127 Uiso 1 1 calc R A . C47 C 0.9285(6) 1.1289(4) 0.7350(3) 0.119(2) Uani 1 1 d . A . H47A H 0.9578 1.1390 0.7766 0.143 Uiso 1 1 calc R . . C48 C 0.9051(4) 1.0684(3) 0.7184(2) 0.0847(15) Uani 1 1 d . . . H48A H 0.9182 1.0378 0.7492 0.102 Uiso 1 1 calc R A . C49 C 0.891(2) 0.8604(8) 0.6803(10) 0.064(5) Uani 0.556(16) 1 d P A 1 H49A H 0.9277 0.8838 0.7167 0.077 Uiso 0.556(16) 1 calc PR A 1 H49B H 0.7988 0.8587 0.6806 0.077 Uiso 0.556(16) 1 calc PR A 1 C50 C 0.9501(10) 0.7955(6) 0.6779(10) 0.112(6) Uani 0.556(16) 1 d P A 1 H50A H 1.0210 0.7916 0.7105 0.135 Uiso 0.556(16) 1 calc PR A 1 H50B H 0.8867 0.7645 0.6855 0.135 Uiso 0.556(16) 1 calc PR A 1 C51 C 0.9932(11) 0.7863(5) 0.6177(7) 0.082(4) Uiso 0.556(16) 1 d P A 1 H51A H 0.9251 0.7726 0.5867 0.098 Uiso 0.556(16) 1 calc PR A 1 H51B H 1.0639 0.7574 0.6192 0.098 Uiso 0.556(16) 1 calc PR A 1 C52 C 1.0345(10) 0.8507(5) 0.6053(7) 0.077(3) Uiso 0.556(16) 1 d P A 1 H52A H 1.1088 0.8619 0.6339 0.092 Uiso 0.556(16) 1 calc PR A 1 H52B H 1.0556 0.8550 0.5620 0.092 Uiso 0.556(16) 1 calc PR A 1 C49A C 0.908(3) 0.8439(12) 0.6609(12) 0.062(5) Uani 0.444(16) 1 d PU A 2 H49C H 0.8246 0.8521 0.6756 0.075 Uiso 0.444(16) 1 calc PR A 2 H49D H 0.9715 0.8473 0.6969 0.075 Uiso 0.444(16) 1 calc PR A 2 C50A C 0.9091(16) 0.7795(5) 0.6344(8) 0.075(5) Uani 0.444(16) 1 d PU A 2 H50C H 0.9347 0.7494 0.6672 0.090 Uiso 0.444(16) 1 calc PR A 2 H50D H 0.8265 0.7680 0.6133 0.090 Uiso 0.444(16) 1 calc PR A 2 C51A C 1.0131(9) 0.7864(4) 0.5859(7) 0.057(3) Uiso 0.444(16) 1 d PU A 2 H51C H 0.9814 0.7694 0.5450 0.069 Uiso 0.444(16) 1 calc PR A 2 H51D H 1.0906 0.7645 0.6012 0.069 Uiso 0.444(16) 1 calc PR A 2 C52A C 1.0392(8) 0.8539(4) 0.5802(6) 0.043(3) Uiso 0.444(16) 1 d PU A 2 H52C H 1.1237 0.8640 0.6000 0.051 Uiso 0.444(16) 1 calc PR A 2 H52D H 1.0337 0.8663 0.5361 0.051 Uiso 0.444(16) 1 calc PR A 2 Li1' Li 0.2559(5) 0.9533(3) 0.0909(3) 0.0430(14) Uani 1 1 d . . . Li2' Li 0.0572(5) 0.8924(3) 0.0846(2) 0.0423(14) Uani 1 1 d . . . Li3' Li 0.1766(5) 0.9062(3) -0.0135(3) 0.0437(13) Uani 1 1 d . . . Li4' Li 0.0587(4) 0.9943(3) 0.0272(2) 0.0401(13) Uani 1 1 d . . . O1' O 0.22737(18) 0.98952(11) 0.00539(9) 0.0406(5) Uani 1 1 d . . . O2' O 0.09127(18) 0.97775(10) 0.11554(9) 0.0416(6) Uani 1 1 d . . . O3' O 0.22523(18) 0.87019(11) 0.06888(9) 0.0411(6) Uani 1 1 d . . . O4' O -0.00639(17) 0.91317(10) 0.00029(10) 0.0391(5) Uani 1 1 d . . . N1' N 0.4325(2) 1.00378(14) 0.10157(13) 0.0479(8) Uani 1 1 d . . . N2' N -0.0344(2) 0.87168(14) 0.16585(12) 0.0442(7) Uani 1 1 d . . . N3' N 0.2606(2) 0.82612(13) -0.05129(12) 0.0448(7) Uani 1 1 d . . . N4' N -0.0877(3) 1.03451(13) -0.02931(14) 0.0489(8) Uani 1 1 d . . . C1' C 0.4407(3) 1.02463(17) 0.03567(15) 0.0455(9) Uani 1 1 d . . . H1'A H 0.4932 1.0621 0.0366 0.055 Uiso 1 1 calc R . . C2' C 0.4981(3) 0.97746(18) -0.00465(18) 0.0557(10) Uani 1 1 d . . . H2'1 H 0.5799 0.9650 0.0154 0.084 Uiso 1 1 calc R . . H2'2 H 0.5086 0.9950 -0.0454 0.084 Uiso 1 1 calc R . . H2'3 H 0.4427 0.9422 -0.0098 0.084 Uiso 1 1 calc R . . C3' C 0.3056(3) 1.04058(17) 0.00629(15) 0.0381(8) Uani 1 1 d . . . C4' C 0.3119(3) 1.07093(17) -0.05657(16) 0.0425(9) Uani 1 1 d . . . C5' C 0.2709(3) 1.04176(19) -0.11186(17) 0.0530(10) Uani 1 1 d . . . H5'A H 0.2399 1.0016 -0.1105 0.064 Uiso 1 1 calc R . . C6' C 0.2744(4) 1.0703(2) -0.16953(19) 0.0661(12) Uani 1 1 d . . . H6'A H 0.2434 1.0500 -0.2066 0.079 Uiso 1 1 calc R . . C7' C 0.3228(4) 1.1279(3) -0.1723(2) 0.0767(14) Uani 1 1 d . . . H7'A H 0.3261 1.1473 -0.2113 0.092 Uiso 1 1 calc R . . C8' C 0.3665(4) 1.1573(2) -0.1184(3) 0.0775(13) Uani 1 1 d . . . H8'A H 0.4012 1.1967 -0.1205 0.093 Uiso 1 1 calc R . . C9' C 0.3603(3) 1.13004(19) -0.0609(2) 0.0614(11) Uani 1 1 d . . . H9'A H 0.3890 1.1514 -0.0242 0.074 Uiso 1 1 calc R . . C10' C 0.4194(4) 1.0562(2) 0.14419(17) 0.0606(11) Uani 1 1 d . . . H10C H 0.3343 1.0738 0.1376 0.073 Uiso 1 1 calc R . . H10D H 0.4816 1.0881 0.1375 0.073 Uiso 1 1 calc R . . C11' C 0.4433(5) 1.0294(2) 0.20906(19) 0.0788(13) Uani 1 1 d . . . H11C H 0.3635 1.0178 0.2254 0.095 Uiso 1 1 calc R . . H11D H 0.4878 1.0587 0.2379 0.095 Uiso 1 1 calc R . . C12' C 0.5247(4) 0.9734(2) 0.20083(18) 0.0718(12) Uani 1 1 d . . . H12C H 0.4815 0.9362 0.2126 0.086 Uiso 1 1 calc R . . H12D H 0.6057 0.9767 0.2267 0.086 Uiso 1 1 calc R . . C13' C 0.5451(3) 0.9724(2) 0.13111(18) 0.0624(11) Uani 1 1 d . . . H13C H 0.6225 0.9942 0.1233 0.075 Uiso 1 1 calc R . . H13D H 0.5499 0.9304 0.1157 0.075 Uiso 1 1 calc R . . C14' C -0.0024(3) 0.92882(17) 0.20112(16) 0.0450(9) Uani 1 1 d . . . C15' C 0.1258(3) 0.92585(19) 0.23897(17) 0.0613(11) Uani 1 1 d . . . H15D H 0.1237 0.8953 0.2717 0.092 Uiso 1 1 calc R . . H15E H 0.1457 0.9654 0.2578 0.092 Uiso 1 1 calc R . . H15F H 0.1898 0.9150 0.2116 0.092 Uiso 1 1 calc R . . C16' C -0.0072(3) 0.98189(17) 0.15354(14) 0.0385(8) Uani 1 1 d . . . C17' C -0.0177(3) 1.04364(17) 0.18430(15) 0.0430(9) Uani 1 1 d . . . C18' C 0.0686(4) 1.0895(2) 0.1783(2) 0.0632(11) Uani 1 1 d . . . H18B H 0.1402 1.0816 0.1570 0.076 Uiso 1 1 calc R . . C19' C 0.0521(4) 1.1474(2) 0.2034(2) 0.0808(14) Uani 1 1 d . . . H19B H 0.1109 1.1786 0.1982 0.097 Uiso 1 1 calc R . . C20' C -0.0506(5) 1.1584(2) 0.2358(2) 0.0767(13) Uani 1 1 d . . . H20B H -0.0605 1.1968 0.2544 0.092 Uiso 1 1 calc R . . C21' C -0.1390(5) 1.1135(3) 0.2409(2) 0.0821(14) Uani 1 1 d . . . H21B H -0.2116 1.1217 0.2614 0.098 Uiso 1 1 calc R . . C22' C -0.1219(4) 1.0571(2) 0.21645(19) 0.0691(12) Uani 1 1 d . . . H22B H -0.1820 1.0264 0.2214 0.083 Uiso 1 1 calc R . . C23' C -0.0061(3) 0.81452(18) 0.20142(18) 0.0581(11) Uani 1 1 d . . . H23C H -0.0360 0.8168 0.2432 0.070 Uiso 1 1 calc R . . H23D H 0.0849 0.8059 0.2058 0.070 Uiso 1 1 calc R . . C24' C -0.0780(4) 0.7665(2) 0.1617(2) 0.0724(12) Uani 1 1 d . . . H24C H -0.0975 0.7311 0.1871 0.087 Uiso 1 1 calc R . . H24D H -0.0291 0.7527 0.1278 0.087 Uiso 1 1 calc R . . C25' C -0.1993(4) 0.7992(2) 0.1353(2) 0.0678(12) Uani 1 1 d . . . H25C H -0.2179 0.7907 0.0905 0.081 Uiso 1 1 calc R . . H25D H -0.2714 0.7861 0.1573 0.081 Uiso 1 1 calc R . . C26' C -0.1718(3) 0.8665(2) 0.14654(18) 0.0576(10) Uani 1 1 d . . . H26C H -0.1944 0.8900 0.1081 0.069 Uiso 1 1 calc R . . H26D H -0.2207 0.8822 0.1796 0.069 Uiso 1 1 calc R . . C27' C 0.3222(3) 0.79565(17) 0.00508(16) 0.0454(9) Uani 1 1 d . . . H27A H 0.3214 0.7510 -0.0028 0.054 Uiso 1 1 calc R . . C28' C 0.4593(3) 0.8152(2) 0.02151(18) 0.0594(11) Uani 1 1 d . . . H28D H 0.5061 0.8099 -0.0148 0.089 Uiso 1 1 calc R . . H28E H 0.4972 0.7903 0.0558 0.089 Uiso 1 1 calc R . . H28F H 0.4618 0.8579 0.0340 0.089 Uiso 1 1 calc R . . C29' C 0.2425(3) 0.80812(17) 0.06070(15) 0.0406(8) Uani 1 1 d . . . C30' C 0.2970(3) 0.77534(17) 0.11976(16) 0.0418(9) Uani 1 1 d . . . C31' C 0.3571(3) 0.80721(19) 0.16935(17) 0.0553(10) Uani 1 1 d . . . H31B H 0.3652 0.8499 0.1665 0.066 Uiso 1 1 calc R . . C32' C 0.4057(4) 0.7776(2) 0.22327(19) 0.0672(12) Uani 1 1 d . . . H32B H 0.4470 0.8003 0.2564 0.081 Uiso 1 1 calc R . . C33' C 0.3942(4) 0.7156(3) 0.2290(2) 0.0728(13) Uani 1 1 d . . . H33B H 0.4266 0.6958 0.2660 0.087 Uiso 1 1 calc R . . C34' C 0.3353(4) 0.6829(2) 0.1803(2) 0.0787(13) Uani 1 1 d . . . H34B H 0.3273 0.6402 0.1834 0.094 Uiso 1 1 calc R . . C35' C 0.2874(4) 0.7131(2) 0.12625(19) 0.0627(11) Uani 1 1 d . . . H35B H 0.2470 0.6902 0.0930 0.075 Uiso 1 1 calc R . . C36' C 0.1496(4) 0.7910(2) -0.07934(17) 0.0640(11) Uani 1 1 d . . . H36C H 0.0771 0.7969 -0.0550 0.077 Uiso 1 1 calc R . . H36D H 0.1694 0.7472 -0.0803 0.077 Uiso 1 1 calc R . . C37' C 0.1209(4) 0.8154(2) -0.14492(18) 0.0732(12) Uani 1 1 d . . . H37C H 0.0470 0.8425 -0.1474 0.088 Uiso 1 1 calc R . . H37D H 0.1039 0.7819 -0.1749 0.088 Uiso 1 1 calc R . . C38' C 0.2385(4) 0.8506(2) -0.15878(18) 0.0731(13) Uani 1 1 d . . . H38C H 0.2663 0.8384 -0.1993 0.088 Uiso 1 1 calc R . . H38D H 0.2231 0.8947 -0.1591 0.088 Uiso 1 1 calc R . . C39' C 0.3359(4) 0.8327(2) -0.10509(18) 0.0655(11) Uani 1 1 d . . . H39C H 0.3776 0.7942 -0.1141 0.079 Uiso 1 1 calc R . . H39D H 0.4003 0.8647 -0.0973 0.079 Uiso 1 1 calc R . . C40' C -0.1311(3) 0.98171(17) -0.06939(15) 0.0452(9) Uani 1 1 d . . . C41' C -0.0494(4) 0.9718(2) -0.12286(17) 0.0651(11) Uani 1 1 d . . . H41D H -0.0551 1.0073 -0.1501 0.098 Uiso 1 1 calc R . . H41E H -0.0788 0.9359 -0.1466 0.098 Uiso 1 1 calc R . . H41F H 0.0379 0.9658 -0.1060 0.098 Uiso 1 1 calc R . . C42' C -0.1291(3) 0.92470(16) -0.02683(15) 0.0392(8) Uani 1 1 d . . . C45' C -0.2162(4) 0.75856(19) -0.0587(2) 0.0657(12) Uani 1 1 d . . . H45B H -0.1950 0.7206 -0.0399 0.079 Uiso 1 1 calc R . . C46' C -0.3027(4) 0.7611(2) -0.1106(2) 0.0666(12) Uani 1 1 d . . . H46B H -0.3382 0.7250 -0.1286 0.080 Uiso 1 1 calc R . . C47' C -0.3364(3) 0.8170(2) -0.1357(2) 0.0672(12) Uani 1 1 d . . . H47B H -0.3971 0.8195 -0.1706 0.081 Uiso 1 1 calc R . . C48' C -0.2814(3) 0.8702(2) -0.10992(17) 0.0551(10) Uani 1 1 d . . . H48B H -0.3066 0.9082 -0.1275 0.066 Uiso 1 1 calc R . . C43' C -0.1903(3) 0.86849(17) -0.05901(15) 0.0422(9) Uani 1 1 d . . . C44' C -0.1603(3) 0.81131(18) -0.03404(18) 0.0524(10) Uani 1 1 d . . . H44B H -0.0998 0.8084 0.0009 0.063 Uiso 1 1 calc R . . C49' C -0.0493(4) 1.08955(18) -0.0628(2) 0.0650(12) Uani 1 1 d . . . H49E H -0.1138 1.1013 -0.0965 0.078 Uiso 1 1 calc R . . H49F H 0.0315 1.0832 -0.0804 0.078 Uiso 1 1 calc R . . C50' C -0.0373(4) 1.1368(2) -0.0108(2) 0.0792(14) Uani 1 1 d . . . H50E H -0.0482 1.1782 -0.0280 0.095 Uiso 1 1 calc R . . H50F H 0.0456 1.1341 0.0135 0.095 Uiso 1 1 calc R . . C51' C -0.1434(4) 1.1211(2) 0.0299(2) 0.0750(13) Uani 1 1 d . . . H51E H -0.1116 1.1203 0.0744 0.090 Uiso 1 1 calc R . . H51F H -0.2124 1.1509 0.0238 0.090 Uiso 1 1 calc R . . C52' C -0.1877(3) 1.05816(18) 0.00767(19) 0.0590(10) Uani 1 1 d . . . H52E H -0.1982 1.0314 0.0435 0.071 Uiso 1 1 calc R . . H52F H -0.2686 1.0609 -0.0184 0.071 Uiso 1 1 calc R . . H29 H 0.324(3) 0.9789(15) 0.5583(12) 0.034(8) Uiso 1 1 d . . . H16' H -0.092(3) 0.9777(16) 0.1273(14) 0.050(9) Uiso 1 1 d . . . H1 H 0.389(3) 0.7589(15) 0.5408(13) 0.037(9) Uiso 1 1 d . . . H3' H 0.275(2) 1.0732(14) 0.0329(13) 0.027(8) Uiso 1 1 d . . . H29' H 0.154(3) 0.7887(13) 0.0479(12) 0.031(7) Uiso 1 1 d . . . H40' H -0.221(3) 0.9899(16) -0.0885(14) 0.051(9) Uiso 1 1 d . . . H16 H 0.612(3) 0.9216(14) 0.3872(13) 0.034(8) Uiso 1 1 d . . . H14' H -0.066(3) 0.9356(15) 0.2306(15) 0.045(9) Uiso 1 1 d . . . H42' H -0.187(3) 0.9343(13) 0.0098(14) 0.034(8) Uiso 1 1 d . . . H3 H 0.403(3) 0.8545(14) 0.5944(13) 0.038(8) Uiso 1 1 d . . . H27 H 0.337(3) 1.0690(16) 0.6159(14) 0.050(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.040(3) 0.039(4) 0.046(3) 0.001(3) 0.010(3) -0.003(3) Li2 0.035(3) 0.040(4) 0.044(3) 0.002(3) 0.008(2) 0.001(3) Li3 0.034(3) 0.041(3) 0.042(3) -0.005(3) 0.009(2) -0.004(3) Li4 0.034(3) 0.047(4) 0.045(3) 0.006(3) 0.005(2) 0.008(3) O1 0.0376(11) 0.0353(13) 0.0410(12) -0.0021(10) 0.0069(10) -0.0061(11) O2 0.0403(12) 0.0450(15) 0.0355(13) 0.0027(11) 0.0134(10) 0.0058(11) O3 0.0271(10) 0.0423(14) 0.0441(12) -0.0042(11) 0.0057(9) 0.0035(10) O4 0.0286(10) 0.0433(15) 0.0413(12) 0.0018(11) -0.0017(10) -0.0045(10) N1 0.0379(15) 0.0436(18) 0.0407(16) -0.0046(14) 0.0039(13) -0.0011(14) N2 0.0393(15) 0.0424(19) 0.0452(16) 0.0057(14) 0.0059(13) -0.0036(14) N3 0.0439(15) 0.0391(18) 0.0397(16) -0.0023(14) 0.0111(13) -0.0042(14) N4 0.0318(15) 0.053(2) 0.090(2) 0.0176(19) -0.0029(16) 0.0041(15) C1 0.0403(19) 0.035(2) 0.050(2) -0.0045(18) 0.0073(17) -0.0078(18) C2 0.064(2) 0.047(3) 0.055(2) -0.0135(18) 0.0023(19) 0.009(2) C3 0.0340(18) 0.032(2) 0.045(2) -0.0001(16) 0.0073(15) -0.0033(17) C4 0.051(2) 0.038(2) 0.0405(19) -0.0017(17) 0.0054(18) -0.0091(18) C5 0.063(3) 0.060(3) 0.060(2) 0.014(2) -0.006(2) -0.011(2) C6 0.088(3) 0.076(4) 0.076(3) 0.012(3) -0.027(3) -0.001(3) C7 0.132(5) 0.052(3) 0.055(3) 0.006(2) -0.001(3) -0.030(3) C8 0.095(3) 0.053(3) 0.062(3) 0.007(2) 0.023(3) -0.022(3) C9 0.066(2) 0.042(2) 0.056(2) -0.002(2) 0.014(2) -0.012(2) C10 0.050(2) 0.064(3) 0.049(2) -0.017(2) 0.0085(18) -0.007(2) C11 0.063(2) 0.096(4) 0.050(2) -0.003(2) -0.006(2) 0.003(2) C12 0.053(2) 0.084(3) 0.072(3) 0.001(2) -0.018(2) -0.001(2) C13 0.0382(19) 0.057(3) 0.060(2) -0.0072(19) 0.0073(18) 0.0028(18) C14 0.0408(18) 0.061(3) 0.0376(18) 0.0021(18) 0.0089(16) 0.0002(19) C15 0.0368(19) 0.073(3) 0.100(3) -0.001(3) 0.020(2) 0.000(2) C16 0.0310(18) 0.048(2) 0.0367(19) 0.0006(17) 0.0063(16) 0.0038(17) C17 0.0425(19) 0.051(3) 0.042(2) -0.0005(18) 0.0155(17) 0.0051(18) C18 0.070(2) 0.064(3) 0.052(2) -0.005(2) 0.016(2) 0.016(2) C19 0.082(3) 0.064(3) 0.086(3) 0.000(3) 0.026(3) 0.030(3) C20 0.086(3) 0.062(3) 0.089(4) -0.024(3) 0.035(3) 0.008(3) C21 0.076(3) 0.071(4) 0.068(3) -0.029(3) 0.027(2) -0.009(3) C22 0.060(2) 0.065(3) 0.047(2) -0.006(2) 0.0126(19) -0.006(2) C23 0.052(2) 0.054(3) 0.061(2) 0.009(2) -0.0017(19) 0.005(2) C24 0.073(3) 0.050(3) 0.082(3) 0.019(2) 0.005(2) 0.003(2) C25 0.094(3) 0.048(3) 0.072(3) 0.006(2) 0.001(2) -0.008(3) C26 0.056(2) 0.061(3) 0.063(2) 0.007(2) 0.0055(19) -0.014(2) C27 0.0370(18) 0.034(2) 0.044(2) -0.0015(17) 0.0081(16) 0.0045(17) C28 0.055(2) 0.039(2) 0.051(2) -0.0005(18) 0.0020(18) -0.0059(18) C29 0.0275(16) 0.038(2) 0.051(2) 0.0006(17) 0.0103(16) 0.0002(17) C30 0.0264(16) 0.040(2) 0.055(2) 0.0037(18) 0.0046(16) -0.0012(17) C31 0.046(2) 0.080(3) 0.051(2) 0.004(2) -0.0026(19) 0.005(2) C32 0.063(3) 0.115(4) 0.057(3) 0.008(3) -0.007(2) 0.003(3) C33 0.050(2) 0.089(4) 0.089(4) 0.030(3) -0.018(3) -0.005(3) C34 0.055(2) 0.059(3) 0.097(4) 0.015(3) -0.007(3) 0.013(2) C35 0.049(2) 0.058(3) 0.071(3) 0.008(2) -0.001(2) 0.011(2) C36 0.059(2) 0.056(3) 0.044(2) -0.007(2) 0.0059(18) 0.003(2) C37 0.078(3) 0.079(3) 0.049(2) 0.003(2) 0.007(2) 0.005(3) C38 0.096(3) 0.066(3) 0.052(2) 0.012(2) 0.021(2) 0.003(3) C39 0.063(2) 0.049(3) 0.054(2) 0.0024(19) 0.0255(19) -0.006(2) C40 0.0361(19) 0.060(3) 0.060(2) 0.008(2) -0.0083(18) -0.0046(19) C41 0.0377(18) 0.074(3) 0.096(3) 0.007(3) 0.025(2) -0.003(2) C42 0.0334(17) 0.059(3) 0.0357(18) 0.0034(18) 0.0009(16) -0.0072(18) C43 0.0366(18) 0.064(3) 0.045(2) -0.007(2) 0.0026(17) -0.0109(19) C44 0.040(2) 0.053(3) 0.073(3) -0.009(2) -0.0027(19) -0.0077(19) C45 0.052(2) 0.060(3) 0.129(4) -0.010(3) 0.000(3) -0.010(2) C46 0.081(3) 0.092(5) 0.145(6) -0.067(5) 0.021(4) -0.032(3) C47 0.124(5) 0.148(7) 0.088(4) -0.064(5) 0.022(4) -0.065(5) C48 0.096(3) 0.101(4) 0.057(3) -0.020(3) 0.003(2) -0.036(3) C49 0.065(8) 0.043(9) 0.080(13) 0.018(6) -0.011(9) 0.001(7) C50 0.090(7) 0.045(7) 0.186(16) 0.041(9) -0.065(8) -0.005(5) C49A 0.057(8) 0.066(12) 0.066(12) 0.007(8) 0.011(8) 0.012(10) C50A 0.085(9) 0.051(7) 0.092(10) 0.023(6) 0.029(7) 0.006(7) Li1' 0.034(3) 0.047(4) 0.047(3) -0.001(3) 0.001(2) -0.003(3) Li2' 0.038(3) 0.041(4) 0.047(3) 0.007(3) 0.002(3) 0.002(3) Li3' 0.042(3) 0.040(4) 0.050(3) -0.004(3) 0.008(3) 0.000(3) Li4' 0.035(3) 0.035(3) 0.050(3) 0.005(3) 0.005(2) 0.002(2) O1' 0.0329(11) 0.0425(15) 0.0467(12) 0.0018(11) 0.0043(10) -0.0080(11) O2' 0.0406(12) 0.0429(15) 0.0430(12) 0.0044(11) 0.0122(10) 0.0024(11) O3' 0.0372(11) 0.0386(16) 0.0476(13) -0.0019(11) 0.0046(10) 0.0054(11) O4' 0.0273(11) 0.0398(14) 0.0486(12) 0.0055(11) -0.0046(10) -0.0004(10) N1' 0.0340(14) 0.053(2) 0.0548(18) -0.0017(16) -0.0037(13) -0.0039(14) N2' 0.0410(15) 0.0418(19) 0.0501(16) 0.0096(15) 0.0058(13) 0.0028(14) N3' 0.0440(16) 0.0455(19) 0.0464(16) -0.0019(15) 0.0126(14) -0.0003(15) N4' 0.0457(16) 0.0333(19) 0.0660(19) 0.0120(16) -0.0030(15) -0.0008(14) C1' 0.0316(17) 0.048(2) 0.057(2) -0.0011(19) 0.0085(17) -0.0075(17) C2' 0.0383(17) 0.057(3) 0.073(2) -0.002(2) 0.0124(18) 0.0064(19) C3' 0.0335(17) 0.034(2) 0.047(2) -0.0050(18) 0.0088(16) -0.0017(18) C4' 0.0350(17) 0.040(2) 0.055(2) 0.0026(19) 0.0152(17) 0.0013(17) C5' 0.055(2) 0.053(3) 0.055(2) 0.005(2) 0.0211(19) -0.001(2) C6' 0.074(3) 0.072(4) 0.055(3) 0.003(2) 0.022(2) 0.007(3) C7' 0.089(3) 0.071(4) 0.076(3) 0.029(3) 0.035(3) 0.025(3) C8' 0.095(3) 0.043(3) 0.099(4) 0.020(3) 0.033(3) 0.003(2) C9' 0.063(2) 0.044(3) 0.080(3) 0.006(2) 0.017(2) 0.002(2) C10' 0.052(2) 0.071(3) 0.058(2) -0.016(2) 0.0001(19) -0.001(2) C11' 0.087(3) 0.085(4) 0.061(3) -0.006(2) -0.010(2) 0.002(3) C12' 0.068(3) 0.075(3) 0.067(3) 0.004(2) -0.019(2) -0.012(3) C13' 0.0406(19) 0.067(3) 0.077(3) 0.001(2) -0.0078(19) 0.000(2) C14' 0.047(2) 0.049(3) 0.0402(19) 0.0061(18) 0.0103(19) 0.0078(18) C15' 0.067(2) 0.063(3) 0.052(2) 0.008(2) -0.006(2) 0.004(2) C16' 0.0338(17) 0.044(2) 0.0375(18) 0.0052(17) 0.0047(17) -0.0002(16) C17' 0.045(2) 0.046(3) 0.0383(18) 0.0056(18) 0.0033(17) 0.010(2) C18' 0.050(2) 0.052(3) 0.087(3) -0.011(2) 0.004(2) 0.004(2) C19' 0.069(3) 0.056(3) 0.113(4) -0.014(3) -0.014(3) -0.005(2) C20' 0.096(4) 0.064(4) 0.068(3) -0.024(3) -0.005(3) 0.027(3) C21' 0.112(4) 0.064(4) 0.077(3) 0.010(3) 0.044(3) 0.023(3) C22' 0.085(3) 0.050(3) 0.078(3) 0.008(2) 0.038(2) 0.010(2) C23' 0.053(2) 0.056(3) 0.066(2) 0.023(2) 0.0116(19) 0.003(2) C24' 0.078(3) 0.047(3) 0.095(3) 0.014(2) 0.018(3) -0.010(2) C25' 0.068(3) 0.065(3) 0.070(3) 0.017(2) 0.006(2) -0.017(2) C26' 0.043(2) 0.063(3) 0.067(2) 0.013(2) 0.0051(18) -0.004(2) C27' 0.0424(19) 0.038(2) 0.057(2) -0.0033(18) 0.0078(18) 0.0027(16) C28' 0.043(2) 0.065(3) 0.072(2) 0.002(2) 0.0148(19) 0.003(2) C29' 0.0334(18) 0.039(3) 0.049(2) 0.0001(17) 0.0015(16) 0.0011(17) C30' 0.0322(17) 0.039(3) 0.054(2) 0.0026(19) 0.0019(17) 0.0032(17) C31' 0.052(2) 0.050(3) 0.062(2) -0.001(2) -0.006(2) 0.010(2) C32' 0.065(3) 0.073(4) 0.061(3) -0.002(2) -0.005(2) 0.014(2) C33' 0.074(3) 0.082(4) 0.061(3) 0.024(3) 0.001(2) 0.017(3) C34' 0.087(3) 0.053(3) 0.093(4) 0.026(3) -0.003(3) -0.003(3) C35' 0.064(2) 0.052(3) 0.068(3) 0.007(2) -0.011(2) -0.006(2) C36' 0.067(3) 0.065(3) 0.059(2) 0.001(2) 0.003(2) -0.013(2) C37' 0.098(3) 0.067(3) 0.053(2) -0.003(2) 0.001(2) -0.012(3) C38' 0.101(3) 0.069(3) 0.051(2) -0.008(2) 0.017(2) 0.002(3) C39' 0.074(3) 0.060(3) 0.068(3) -0.007(2) 0.030(2) -0.005(2) C40' 0.0383(19) 0.046(2) 0.050(2) 0.0104(19) -0.0051(17) 0.0016(18) C41' 0.073(2) 0.066(3) 0.056(2) 0.021(2) 0.006(2) -0.003(2) C42' 0.0318(17) 0.040(2) 0.045(2) 0.0019(18) -0.0003(17) -0.0002(16) C45' 0.055(2) 0.045(3) 0.095(3) 0.001(2) -0.007(3) -0.002(2) C46' 0.054(2) 0.054(3) 0.089(3) -0.018(3) -0.005(2) -0.009(2) C47' 0.049(2) 0.073(4) 0.076(3) -0.010(3) -0.014(2) -0.003(2) C48' 0.047(2) 0.053(3) 0.062(2) 0.000(2) -0.011(2) 0.001(2) C43' 0.0315(17) 0.048(3) 0.047(2) 0.0033(19) 0.0016(17) 0.0014(17) C44' 0.0398(19) 0.048(3) 0.066(2) 0.002(2) -0.0079(18) -0.006(2) C49' 0.054(2) 0.045(3) 0.095(3) 0.025(2) 0.004(2) 0.003(2) C50' 0.063(3) 0.041(3) 0.127(4) 0.004(3) -0.026(3) 0.000(2) C51' 0.086(3) 0.048(3) 0.087(3) 0.004(2) -0.013(3) 0.011(2) C52' 0.055(2) 0.049(3) 0.071(2) -0.001(2) -0.003(2) 0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O2 1.901(5) . ? Li1 O3 1.912(6) . ? Li1 O1 2.024(6) . ? Li1 N1 2.093(6) . ? Li1 Li3 2.519(7) . ? Li1 Li4 2.531(7) . ? Li1 Li2 2.556(8) . ? Li1 C3 2.576(6) . ? Li1 C1 2.690(7) . ? Li2 O4 1.913(5) . ? Li2 O2 1.947(6) . ? Li2 O3 2.021(5) . ? Li2 N2 2.204(6) . ? Li2 Li3 2.556(7) . ? Li2 Li4 2.568(8) . ? Li2 C16 2.768(6) . ? Li3 O4 1.902(5) . ? Li3 O1 1.944(6) . ? Li3 O3 1.971(6) . ? Li3 N3 2.062(6) . ? Li3 Li4 2.507(7) . ? Li3 C29 2.668(6) . ? Li3 C27 2.742(6) . ? Li4 O2 1.897(5) . ? Li4 O4 1.961(6) . ? Li4 O1 1.987(5) . ? Li4 N4 2.196(6) . ? Li4 C42 2.784(7) . ? O1 C3 1.390(4) . ? O2 C16 1.385(4) . ? O3 C29 1.394(4) . ? O4 C42 1.384(4) . ? N1 C10 1.476(4) . ? N1 C13 1.476(4) . ? N1 C1 1.481(4) . ? N2 C23 1.467(4) . ? N2 C26 1.474(5) . ? N2 C14 1.481(4) . ? N3 C36 1.477(4) . ? N3 C39 1.477(4) . ? N3 C27 1.486(4) . ? N4 C52 1.388(11) . ? N4 C49A 1.40(3) . ? N4 C40 1.476(5) . ? N4 C49 1.60(2) . ? N4 C52A 1.607(10) . ? C1 C2 1.523(5) . ? C1 C3 1.568(5) . ? C3 C4 1.510(5) . ? C4 C5 1.373(5) . ? C4 C9 1.390(5) . ? C5 C6 1.383(6) . ? C6 C7 1.391(7) . ? C7 C8 1.341(7) . ? C8 C9 1.380(5) . ? C10 C11 1.504(5) . ? C11 C12 1.513(6) . ? C12 C13 1.518(5) . ? C14 C15 1.526(5) . ? C14 C16 1.548(5) . ? C16 C17 1.522(5) . ? C17 C18 1.378(5) . ? C17 C22 1.387(5) . ? C18 C19 1.381(6) . ? C19 C20 1.365(6) . ? C20 C21 1.375(6) . ? C21 C22 1.380(6) . ? C23 C24 1.509(6) . ? C24 C25 1.521(6) . ? C25 C26 1.527(6) . ? C27 C28 1.513(5) . ? C27 C29 1.548(5) . ? C29 C30 1.537(5) . ? C30 C31 1.373(5) . ? C30 C35 1.386(5) . ? C31 C32 1.384(6) . ? C32 C33 1.377(7) . ? C33 C34 1.346(6) . ? C34 C35 1.391(6) . ? C36 C37 1.519(5) . ? C37 C38 1.518(6) . ? C38 C39 1.521(5) . ? C40 C41 1.520(5) . ? C40 C42 1.560(5) . ? C42 C43 1.513(5) . ? C43 C44 1.375(5) . ? C43 C48 1.383(5) . ? C44 C45 1.394(6) . ? C45 C46 1.377(8) . ? C46 C47 1.362(9) . ? C47 C48 1.387(8) . ? C49 C50 1.55(2) . ? C50 C51 1.424(17) . ? C51 C52 1.507(14) . ? C49A C50A 1.52(2) . ? C50A C51A 1.596(18) . ? C51A C52A 1.511(14) . ? Li1' O3' 1.898(6) . ? Li1' O2' 1.949(5) . ? Li1' O1' 1.991(6) . ? Li1' N1' 2.168(6) . ? Li1' Li2' 2.487(7) . ? Li1' Li3' 2.530(8) . ? Li1' Li4' 2.547(7) . ? Li1' C3' 2.718(7) . ? Li2' O3' 1.911(5) . ? Li2' O4' 1.919(6) . ? Li2' O2' 2.001(6) . ? Li2' N2' 2.125(6) . ? Li2' Li4' 2.544(8) . ? Li2' Li3' 2.575(8) . ? Li2' C16' 2.583(6) . ? Li2' C14' 2.753(6) . ? Li2' C29' 2.780(6) . ? Li3' O1' 1.931(6) . ? Li3' O3' 1.955(6) . ? Li3' O4' 2.000(5) . ? Li3' N3' 2.159(6) . ? Li3' Li4' 2.500(8) . ? Li3' C29' 2.721(7) . ? Li4' O1' 1.897(5) . ? Li4' O2' 1.924(5) . ? Li4' O4' 1.969(6) . ? Li4' N4' 2.072(6) . ? Li4' C42' 2.680(6) . ? Li4' C40' 2.759(6) . ? O1' C3' 1.391(4) . ? O2' C16' 1.389(3) . ? O3' C29' 1.383(4) . ? O4' C42' 1.397(4) . ? N1' C13' 1.468(4) . ? N1' C10' 1.480(5) . ? N1' C1' 1.495(4) . ? N2' C26' 1.482(4) . ? N2' C23' 1.479(5) . ? N2' C14' 1.482(5) . ? N3' C39' 1.473(4) . ? N3' C27' 1.475(4) . ? N3' C36' 1.484(5) . ? N4' C52' 1.479(5) . ? N4' C49' 1.479(5) . ? N4' C40' 1.485(5) . ? C1' C2' 1.511(5) . ? C1' C3' 1.549(4) . ? C3' C4' 1.509(5) . ? C4' C5' 1.378(5) . ? C4' C9' 1.398(5) . ? C5' C6' 1.388(5) . ? C6' C7' 1.365(6) . ? C7' C8' 1.363(6) . ? C8' C9' 1.375(6) . ? C10' C11' 1.507(6) . ? C11' C12' 1.518(6) . ? C12' C13' 1.531(5) . ? C14' C15' 1.516(5) . ? C14' C16' 1.542(5) . ? C16' C17' 1.512(5) . ? C17' C18' 1.372(5) . ? C17' C22' 1.390(5) . ? C18' C19' 1.394(6) . ? C19' C20' 1.369(6) . ? C20' C21' 1.370(7) . ? C21' C22' 1.360(6) . ? C23' C24' 1.511(6) . ? C24' C25' 1.532(6) . ? C25' C26' 1.515(6) . ? C27' C28' 1.525(5) . ? C27' C29' 1.552(5) . ? C29' C30' 1.519(5) . ? C30' C31' 1.375(5) . ? C30' C35' 1.373(5) . ? C31' C32' 1.380(5) . ? C32' C33' 1.367(6) . ? C33' C34' 1.366(6) . ? C34' C35' 1.386(6) . ? C36' C37' 1.507(5) . ? C37' C38' 1.520(6) . ? C38' C39' 1.521(6) . ? C40' C41' 1.518(5) . ? C40' C42' 1.543(5) . ? C42' C43' 1.524(5) . ? C45' C46' 1.373(6) . ? C45' C44' 1.379(5) . ? C46' C47' 1.369(6) . ? C47' C48' 1.391(6) . ? C48' C43' 1.386(5) . ? C43' C44' 1.385(5) . ? C49' C50' 1.517(6) . ? C50' C51' 1.530(6) . ? C51' C52' 1.516(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Li1 O3 100.1(3) . . ? O2 Li1 O1 97.8(2) . . ? O3 Li1 O1 98.6(3) . . ? O2 Li1 N1 125.6(3) . . ? O3 Li1 N1 130.6(3) . . ? O1 Li1 N1 93.2(2) . . ? O2 Li1 Li3 94.7(2) . . ? O3 Li1 Li3 50.58(19) . . ? O1 Li1 Li3 49.22(18) . . ? N1 Li1 Li3 130.4(3) . . ? O2 Li1 Li4 48.14(17) . . ? O3 Li1 Li4 97.9(3) . . ? O1 Li1 Li4 50.25(17) . . ? N1 Li1 Li4 125.3(3) . . ? Li3 Li1 Li4 59.5(2) . . ? O2 Li1 Li2 49.14(18) . . ? O3 Li1 Li2 51.35(18) . . ? O1 Li1 Li2 97.4(2) . . ? N1 Li1 Li2 168.8(3) . . ? Li3 Li1 Li2 60.5(2) . . ? Li4 Li1 Li2 60.6(2) . . ? O2 Li1 C3 124.5(3) . . ? O3 Li1 C3 107.9(2) . . ? O1 Li1 C3 32.42(12) . . ? N1 Li1 C3 63.26(17) . . ? Li3 Li1 C3 70.4(2) . . ? Li4 Li1 C3 80.7(2) . . ? Li2 Li1 C3 127.9(3) . . ? O2 Li1 C1 119.7(3) . . ? O3 Li1 C1 136.2(3) . . ? O1 Li1 C1 60.67(17) . . ? N1 Li1 C1 33.19(13) . . ? Li3 Li1 C1 104.9(2) . . ? Li4 Li1 C1 95.7(2) . . ? Li2 Li1 C1 155.9(3) . . ? C3 Li1 C1 34.55(12) . . ? O4 Li2 O2 96.2(3) . . ? O4 Li2 O3 96.5(2) . . ? O2 Li2 O3 94.9(2) . . ? O4 Li2 N2 135.7(3) . . ? O2 Li2 N2 84.1(2) . . ? O3 Li2 N2 127.8(3) . . ? O4 Li2 Li1 94.5(2) . . ? O2 Li2 Li1 47.63(18) . . ? O3 Li2 Li1 47.64(17) . . ? N2 Li2 Li1 116.3(3) . . ? O4 Li2 Li3 47.73(16) . . ? O2 Li2 Li3 92.4(2) . . ? O3 Li2 Li3 49.32(16) . . ? N2 Li2 Li3 175.3(3) . . ? Li1 Li2 Li3 59.0(2) . . ? O4 Li2 Li4 49.28(19) . . ? O2 Li2 Li4 47.25(18) . . ? O3 Li2 Li4 94.0(2) . . ? N2 Li2 Li4 120.2(3) . . ? Li1 Li2 Li4 59.2(2) . . ? Li3 Li2 Li4 58.6(2) . . ? O4 Li2 C16 120.8(3) . . ? O2 Li2 C16 27.80(12) . . ? O3 Li2 C16 103.2(2) . . ? N2 Li2 C16 57.92(16) . . ? Li1 Li2 C16 63.50(18) . . ? Li3 Li2 C16 118.1(3) . . ? Li4 Li2 C16 73.8(2) . . ? O4 Li3 O1 101.0(3) . . ? O4 Li3 O3 98.6(2) . . ? O1 Li3 O3 99.3(2) . . ? O4 Li3 N3 120.6(3) . . ? O1 Li3 N3 135.3(3) . . ? O3 Li3 N3 90.5(2) . . ? O4 Li3 Li4 50.56(19) . . ? O1 Li3 Li4 51.14(18) . . ? O3 Li3 Li4 97.1(2) . . ? N3 Li3 Li4 169.1(3) . . ? O4 Li3 Li1 96.0(2) . . ? O1 Li3 Li1 52.01(19) . . ? O3 Li3 Li1 48.54(18) . . ? N3 Li3 Li1 130.1(3) . . ? Li4 Li3 Li1 60.5(2) . . ? O4 Li3 Li2 48.12(17) . . ? O1 Li3 Li2 99.5(2) . . ? O3 Li3 Li2 51.04(17) . . ? N3 Li3 Li2 119.7(3) . . ? Li4 Li3 Li2 60.9(2) . . ? Li1 Li3 Li2 60.5(2) . . ? O4 Li3 C29 119.7(3) . . ? O1 Li3 C29 113.2(2) . . ? O3 Li3 C29 30.54(12) . . ? N3 Li3 C29 61.21(17) . . ? Li4 Li3 C29 127.3(2) . . ? Li1 Li3 C29 71.83(19) . . ? Li2 Li3 C29 77.4(2) . . ? O4 Li3 C27 113.5(3) . . ? O1 Li3 C27 141.1(3) . . ? O3 Li3 C27 59.35(17) . . ? N3 Li3 C27 32.24(13) . . ? Li4 Li3 C27 151.8(3) . . ? Li1 Li3 C27 104.9(2) . . ? Li2 Li3 C27 90.9(2) . . ? C29 Li3 C27 33.22(12) . . ? O2 Li4 O4 96.3(3) . . ? O2 Li4 O1 99.2(2) . . ? O4 Li4 O1 97.5(2) . . ? O2 Li4 N4 137.2(3) . . ? O4 Li4 N4 84.0(2) . . ? O1 Li4 N4 123.3(3) . . ? O2 Li4 Li3 95.1(2) . . ? O4 Li4 Li3 48.50(18) . . ? O1 Li4 Li3 49.62(18) . . ? N4 Li4 Li3 115.3(3) . . ? O2 Li4 Li1 48.29(17) . . ? O4 Li4 Li1 94.1(2) . . ? O1 Li4 Li1 51.52(17) . . ? N4 Li4 Li1 174.3(3) . . ? Li3 Li4 Li1 60.0(2) . . ? O2 Li4 Li2 48.90(18) . . ? O4 Li4 Li2 47.69(18) . . ? O1 Li4 Li2 98.0(2) . . ? N4 Li4 Li2 121.2(3) . . ? Li3 Li4 Li2 60.5(2) . . ? Li1 Li4 Li2 60.2(2) . . ? O2 Li4 C42 120.3(3) . . ? O4 Li4 C42 27.53(12) . . ? O1 Li4 C42 104.6(2) . . ? N4 Li4 C42 57.65(17) . . ? Li3 Li4 C42 64.25(18) . . ? Li1 Li4 C42 119.6(2) . . ? Li2 Li4 C42 73.8(2) . . ? C3 O1 Li3 122.7(2) . . ? C3 O1 Li4 156.3(3) . . ? Li3 O1 Li4 79.2(2) . . ? C3 O1 Li1 96.2(2) . . ? Li3 O1 Li1 78.8(2) . . ? Li4 O1 Li1 78.2(2) . . ? C16 O2 Li4 155.4(2) . . ? C16 O2 Li1 116.5(2) . . ? Li4 O2 Li1 83.6(2) . . ? C16 O2 Li2 111.2(2) . . ? Li4 O2 Li2 83.8(2) . . ? Li1 O2 Li2 83.2(2) . . ? C29 O3 Li1 133.5(3) . . ? C29 O3 Li3 103.6(2) . . ? Li1 O3 Li3 80.9(2) . . ? C29 O3 Li2 145.5(3) . . ? Li1 O3 Li2 81.0(2) . . ? Li3 O3 Li2 79.6(2) . . ? C42 O4 Li3 117.7(2) . . ? C42 O4 Li2 154.7(3) . . ? Li3 O4 Li2 84.1(2) . . ? C42 O4 Li4 111.6(3) . . ? Li3 O4 Li4 80.9(2) . . ? Li2 O4 Li4 83.0(2) . . ? C10 N1 C13 102.8(3) . . ? C10 N1 C1 115.0(3) . . ? C13 N1 C1 111.8(2) . . ? C10 N1 Li1 121.8(3) . . ? C13 N1 Li1 109.5(3) . . ? C1 N1 Li1 96.1(2) . . ? C23 N2 C26 101.7(3) . . ? C23 N2 C14 112.1(3) . . ? C26 N2 C14 115.9(3) . . ? C23 N2 Li2 105.1(2) . . ? C26 N2 Li2 118.4(3) . . ? C14 N2 Li2 103.4(2) . . ? C36 N3 C39 102.4(2) . . ? C36 N3 C27 114.2(3) . . ? C39 N3 C27 113.8(2) . . ? C36 N3 Li3 119.7(2) . . ? C39 N3 Li3 107.0(3) . . ? C27 N3 Li3 100.0(2) . . ? C52 N4 C49A 85.4(11) . . ? C52 N4 C40 115.2(5) . . ? C49A N4 C40 123.5(9) . . ? C52 N4 C49 102.1(8) . . ? C49A N4 C49 21.3(10) . . ? C40 N4 C49 103.8(6) . . ? C52 N4 C52A 19.5(6) . . ? C49A N4 C52A 101.9(10) . . ? C40 N4 C52A 112.7(4) . . ? C49 N4 C52A 120.4(8) . . ? C52 N4 Li4 127.4(6) . . ? C49A N4 Li4 102.4(13) . . ? C40 N4 Li4 103.3(3) . . ? C49 N4 Li4 101.9(8) . . ? C52A N4 Li4 112.8(5) . . ? N1 C1 C2 111.9(3) . . ? N1 C1 C3 109.0(3) . . ? C2 C1 C3 110.8(3) . . ? N1 C1 Li1 50.66(19) . . ? C2 C1 Li1 99.3(2) . . ? C3 C1 Li1 68.7(2) . . ? O1 C3 C4 115.9(3) . . ? O1 C3 C1 111.7(3) . . ? C4 C3 C1 109.0(3) . . ? O1 C3 Li1 51.34(17) . . ? C4 C3 Li1 166.8(3) . . ? C1 C3 Li1 76.7(2) . . ? C5 C4 C9 117.0(3) . . ? C5 C4 C3 123.1(3) . . ? C9 C4 C3 119.8(3) . . ? C4 C5 C6 121.7(4) . . ? C5 C6 C7 119.4(4) . . ? C8 C7 C6 119.9(4) . . ? C7 C8 C9 120.2(4) . . ? C8 C9 C4 121.7(4) . . ? N1 C10 C11 103.7(3) . . ? C10 C11 C12 103.5(3) . . ? C11 C12 C13 105.2(3) . . ? N1 C13 C12 106.4(3) . . ? N2 C14 C15 113.1(3) . . ? N2 C14 C16 108.4(2) . . ? C15 C14 C16 111.4(3) . . ? O2 C16 C17 111.8(3) . . ? O2 C16 C14 110.9(3) . . ? C17 C16 C14 112.0(2) . . ? O2 C16 Li2 40.95(17) . . ? C17 C16 Li2 151.5(3) . . ? C14 C16 Li2 80.0(2) . . ? C18 C17 C22 116.6(4) . . ? C18 C17 C16 122.1(3) . . ? C22 C17 C16 121.3(3) . . ? C17 C18 C19 121.5(4) . . ? C20 C19 C18 121.3(4) . . ? C19 C20 C21 118.2(4) . . ? C20 C21 C22 120.5(4) . . ? C21 C22 C17 121.8(4) . . ? N2 C23 C24 105.2(3) . . ? C23 C24 C25 103.7(3) . . ? C24 C25 C26 105.2(3) . . ? N2 C26 C25 104.5(3) . . ? N3 C27 C28 111.3(3) . . ? N3 C27 C29 108.6(3) . . ? C28 C27 C29 110.8(3) . . ? N3 C27 Li3 47.79(17) . . ? C28 C27 Li3 99.1(2) . . ? C29 C27 Li3 70.7(2) . . ? O3 C29 C30 112.7(3) . . ? O3 C29 C27 111.1(3) . . ? C30 C29 C27 112.6(3) . . ? O3 C29 Li3 45.90(16) . . ? C30 C29 Li3 157.1(2) . . ? C27 C29 Li3 76.0(2) . . ? C31 C30 C35 116.9(3) . . ? C31 C30 C29 119.1(3) . . ? C35 C30 C29 124.0(3) . . ? C30 C31 C32 121.6(4) . . ? C33 C32 C31 120.6(4) . . ? C34 C33 C32 118.6(4) . . ? C33 C34 C35 121.2(4) . . ? C34 C35 C30 121.1(4) . . ? N3 C36 C37 104.0(3) . . ? C36 C37 C38 105.0(3) . . ? C37 C38 C39 104.9(3) . . ? N3 C39 C38 103.9(3) . . ? N4 C40 C41 112.4(3) . . ? N4 C40 C42 108.0(3) . . ? C41 C40 C42 109.9(3) . . ? O4 C42 C43 114.1(3) . . ? O4 C42 C40 110.6(3) . . ? C43 C42 C40 110.2(3) . . ? O4 C42 Li4 40.92(18) . . ? C43 C42 Li4 152.8(3) . . ? C40 C42 Li4 78.8(2) . . ? C44 C43 C48 117.5(4) . . ? C44 C43 C42 121.8(3) . . ? C48 C43 C42 120.6(4) . . ? C43 C44 C45 121.7(4) . . ? C46 C45 C44 119.2(5) . . ? C47 C46 C45 120.3(5) . . ? C46 C47 C48 119.8(5) . . ? C43 C48 C47 121.6(5) . . ? C50 C49 N4 99.4(11) . . ? C51 C50 C49 109.0(11) . . ? C50 C51 C52 98.7(9) . . ? N4 C52 C51 105.4(8) . . ? N4 C49A C50A 111.3(14) . . ? C51A C50A C49A 100.9(13) . . ? C50A C51A C52A 106.8(8) . . ? N4 C52A C51A 105.2(7) . . ? O3' Li1' O2' 101.1(3) . . ? O3' Li1' O1' 98.4(3) . . ? O2' Li1' O1' 94.6(2) . . ? O3' Li1' N1' 129.7(3) . . ? O2' Li1' N1' 128.4(3) . . ? O1' Li1' N1' 87.0(2) . . ? O3' Li1' Li2' 49.45(19) . . ? O2' Li1' Li2' 51.91(19) . . ? O1' Li1' Li2' 96.4(2) . . ? N1' Li1' Li2' 176.6(3) . . ? O3' Li1' Li3' 49.95(19) . . ? O2' Li1' Li3' 97.0(2) . . ? O1' Li1' Li3' 48.80(19) . . ? N1' Li1' Li3' 120.7(3) . . ? Li2' Li1' Li3' 61.8(2) . . ? O3' Li1' Li4' 95.3(2) . . ? O2' Li1' Li4' 48.46(17) . . ? O1' Li1' Li4' 47.51(17) . . ? N1' Li1' Li4' 122.4(3) . . ? Li2' Li1' Li4' 60.7(2) . . ? Li3' Li1' Li4' 59.0(2) . . ? O3' Li1' C3' 123.1(3) . . ? O2' Li1' C3' 103.1(3) . . ? O1' Li1' C3' 29.52(12) . . ? N1' Li1' C3' 59.42(17) . . ? Li2' Li1' C3' 123.9(2) . . ? Li3' Li1' C3' 76.5(2) . . ? Li4' Li1' C3' 66.39(19) . . ? O3' Li2' O4' 98.3(3) . . ? O3' Li2' O2' 98.8(2) . . ? O4' Li2' O2' 97.3(3) . . ? O3' Li2' N2' 126.8(3) . . ? O4' Li2' N2' 132.4(3) . . ? O2' Li2' N2' 90.6(2) . . ? O3' Li2' Li1' 49.00(19) . . ? O4' Li2' Li1' 98.2(3) . . ? O2' Li2' Li1' 50.06(18) . . ? N2' Li2' Li1' 121.6(3) . . ? O3' Li2' Li4' 95.0(2) . . ? O4' Li2' Li4' 50.00(18) . . ? O2' Li2' Li4' 48.29(18) . . ? N2' Li2' Li4' 127.4(3) . . ? Li1' Li2' Li4' 60.8(2) . . ? O3' Li2' Li3' 48.98(18) . . ? O4' Li2' Li3' 50.28(18) . . ? O2' Li2' Li3' 94.2(2) . . ? N2' Li2' Li3' 174.1(3) . . ? Li1' Li2' Li3' 59.9(2) . . ? Li4' Li2' Li3' 58.5(2) . . ? O3' Li2' C16' 126.7(3) . . ? O4' Li2' C16' 105.7(2) . . ? O2' Li2' C16' 32.20(12) . . ? N2' Li2' C16' 61.65(18) . . ? Li1' Li2' C16' 80.4(2) . . ? Li4' Li2' C16' 68.2(2) . . ? Li3' Li2' C16' 123.8(3) . . ? O3' Li2' C14' 122.3(2) . . ? O4' Li2' C14' 134.0(3) . . ? O2' Li2' C14' 58.66(16) . . ? N2' Li2' C14' 32.24(14) . . ? Li1' Li2' C14' 93.7(2) . . ? Li4' Li2' C14' 101.4(2) . . ? Li3' Li2' C14' 151.8(3) . . ? C16' Li2' C14' 33.41(12) . . ? O3' Li2' C29' 26.99(13) . . ? O4' Li2' C29' 100.0(2) . . ? O2' Li2' C29' 124.8(2) . . ? N2' Li2' C29' 113.4(2) . . ? Li1' Li2' C29' 75.7(2) . . ? Li4' Li2' C29' 117.0(2) . . ? Li3' Li2' C29' 60.92(18) . . ? C16' Li2' C29' 147.0(2) . . ? C14' Li2' C29' 126.0(2) . . ? O1' Li3' O3' 98.5(3) . . ? O1' Li3' O4' 98.8(3) . . ? O3' Li3' O4' 94.1(2) . . ? O1' Li3' N3' 136.6(3) . . ? O3' Li3' N3' 86.0(2) . . ? O4' Li3' N3' 124.1(3) . . ? O1' Li3' Li4' 48.66(18) . . ? O3' Li3' Li4' 95.3(2) . . ? O4' Li3' Li4' 50.43(18) . . ? N3' Li3' Li4' 174.4(3) . . ? O1' Li3' Li1' 50.9(2) . . ? O3' Li3' Li1' 47.99(19) . . ? O4' Li3' Li1' 94.8(2) . . ? N3' Li3' Li1' 123.2(3) . . ? Li4' Li3' Li1' 60.8(2) . . ? O1' Li3' Li2' 95.1(3) . . ? O3' Li3' Li2' 47.49(17) . . ? O4' Li3' Li2' 47.59(17) . . ? N3' Li3' Li2' 117.7(3) . . ? Li4' Li3' Li2' 60.1(2) . . ? Li1' Li3' Li2' 58.3(2) . . ? O1' Li3' C29' 124.8(3) . . ? O3' Li3' C29' 28.93(13) . . ? O4' Li3' C29' 99.9(2) . . ? N3' Li3' C29' 59.16(17) . . ? Li4' Li3' C29' 120.8(3) . . ? Li1' Li3' C29' 76.1(2) . . ? Li2' Li3' C29' 63.27(19) . . ? O1' Li4' O2' 98.6(2) . . ? O1' Li4' O4' 101.0(3) . . ? O2' Li4' O4' 98.3(3) . . ? O1' Li4' N4' 123.5(3) . . ? O2' Li4' N4' 135.0(3) . . ? O4' Li4' N4' 89.4(2) . . ? O1' Li4' Li3' 49.83(19) . . ? O2' Li4' Li3' 98.7(3) . . ? O4' Li4' Li3' 51.52(18) . . ? N4' Li4' Li3' 119.7(3) . . ? O1' Li4' Li2' 97.0(2) . . ? O2' Li4' Li2' 50.94(19) . . ? O4' Li4' Li2' 48.30(18) . . ? N4' Li4' Li2' 127.9(3) . . ? Li3' Li4' Li2' 61.4(2) . . ? O1' Li4' Li1' 50.69(18) . . ? O2' Li4' Li1' 49.32(17) . . ? O4' Li4' Li1' 95.0(2) . . ? N4' Li4' Li1' 173.3(3) . . ? Li3' Li4' Li1' 60.2(2) . . ? Li2' Li4' Li1' 58.5(2) . . ? O1' Li4' C42' 122.9(3) . . ? O2' Li4' C42' 111.9(2) . . ? O4' Li4' C42' 30.34(12) . . ? N4' Li4' C42' 60.26(16) . . ? Li3' Li4' C42' 77.8(2) . . ? Li2' Li4' C42' 70.9(2) . . ? Li1' Li4' C42' 124.8(3) . . ? O1' Li4' C40' 116.6(2) . . ? O2' Li4' C40' 140.1(3) . . ? O4' Li4' C40' 58.69(16) . . ? N4' Li4' C40' 31.97(14) . . ? Li3' Li4' C40' 90.9(2) . . ? Li2' Li4' C40' 103.7(2) . . ? Li1' Li4' C40' 150.3(3) . . ? C42' Li4' C40' 32.93(12) . . ? C3' O1' Li4' 122.0(3) . . ? C3' O1' Li3' 156.1(3) . . ? Li4' O1' Li3' 81.5(2) . . ? C3' O1' Li1' 105.6(2) . . ? Li4' O1' Li1' 81.8(2) . . ? Li3' O1' Li1' 80.3(2) . . ? C16' O2' Li4' 119.4(2) . . ? C16' O2' Li1' 157.3(3) . . ? Li4' O2' Li1' 82.2(2) . . ? C16' O2' Li2' 97.6(2) . . ? Li4' O2' Li2' 80.8(2) . . ? Li1' O2' Li2' 78.0(2) . . ? C29' O3' Li1' 161.7(2) . . ? C29' O3' Li2' 114.2(3) . . ? Li1' O3' Li2' 81.5(2) . . ? C29' O3' Li3' 107.9(2) . . ? Li1' O3' Li3' 82.1(2) . . ? Li2' O3' Li3' 83.5(2) . . ? C42' O4' Li2' 131.5(2) . . ? C42' O4' Li4' 104.2(2) . . ? Li2' O4' Li4' 81.7(2) . . ? C42' O4' Li3' 146.4(3) . . ? Li2' O4' Li3' 82.1(2) . . ? Li4' O4' Li3' 78.1(2) . . ? C13' N1' C10' 102.6(3) . . ? C13' N1' C1' 115.5(3) . . ? C10' N1' C1' 111.4(3) . . ? C13' N1' Li1' 117.9(3) . . ? C10' N1' Li1' 109.1(3) . . ? C1' N1' Li1' 100.7(2) . . ? C26' N2' C23' 102.9(3) . . ? C26' N2' C14' 112.2(3) . . ? C23' N2' C14' 115.1(3) . . ? C26' N2' Li2' 107.7(3) . . ? C23' N2' Li2' 121.1(3) . . ? C14' N2' Li2' 97.9(2) . . ? C39' N3' C27' 117.0(3) . . ? C39' N3' C36' 101.8(3) . . ? C27' N3' C36' 111.6(3) . . ? C39' N3' Li3' 119.3(3) . . ? C27' N3' Li3' 103.0(2) . . ? C36' N3' Li3' 103.4(3) . . ? C52' N4' C49' 102.8(3) . . ? C52' N4' C40' 112.5(3) . . ? C49' N4' C40' 115.9(3) . . ? C52' N4' Li4' 111.9(3) . . ? C49' N4' Li4' 113.8(3) . . ? C40' N4' Li4' 100.4(3) . . ? N1' C1' C2' 113.3(3) . . ? N1' C1' C3' 108.4(2) . . ? C2' C1' C3' 109.3(3) . . ? O1' C3' C4' 114.8(3) . . ? O1' C3' C1' 110.7(3) . . ? C4' C3' C1' 110.0(3) . . ? O1' C3' Li1' 44.86(17) . . ? C4' C3' Li1' 158.8(3) . . ? C1' C3' Li1' 78.7(2) . . ? C5' C4' C9' 117.3(3) . . ? C5' C4' C3' 121.7(3) . . ? C9' C4' C3' 121.0(3) . . ? C4' C5' C6' 121.6(4) . . ? C7' C6' C5' 119.8(4) . . ? C6' C7' C8' 119.8(4) . . ? C7' C8' C9' 120.9(4) . . ? C8' C9' C4' 120.7(4) . . ? N1' C10' C11' 104.5(3) . . ? C10' C11' C12' 104.6(3) . . ? C11' C12' C13' 105.2(3) . . ? N1' C13' C12' 103.1(3) . . ? N2' C14' C15' 112.7(3) . . ? N2' C14' C16' 107.8(3) . . ? C15' C14' C16' 110.8(3) . . ? N2' C14' Li2' 49.86(18) . . ? C15' C14' Li2' 101.5(2) . . ? C16' C14' Li2' 67.3(2) . . ? O2' C16' C17' 113.9(3) . . ? O2' C16' C14' 111.1(3) . . ? C17' C16' C14' 112.5(3) . . ? O2' C16' Li2' 50.15(19) . . ? C17' C16' Li2' 163.9(2) . . ? C14' C16' Li2' 79.3(2) . . ? C18' C17' C22' 117.5(4) . . ? C18' C17' C16' 122.2(3) . . ? C22' C17' C16' 120.1(3) . . ? C17' C18' C19' 121.1(4) . . ? C20' C19' C18' 119.5(5) . . ? C21' C20' C19' 120.0(4) . . ? C22' C21' C20' 120.0(4) . . ? C21' C22' C17' 121.8(4) . . ? N2' C23' C24' 103.4(3) . . ? C23' C24' C25' 104.1(3) . . ? C26' C25' C24' 104.7(3) . . ? N2' C26' C25' 106.7(3) . . ? N3' C27' C28' 113.5(3) . . ? N3' C27' C29' 108.6(3) . . ? C28' C27' C29' 110.7(3) . . ? O3' C29' C30' 113.7(3) . . ? O3' C29' C27' 111.0(3) . . ? C30' C29' C27' 111.4(3) . . ? O3' C29' Li3' 43.14(17) . . ? C30' C29' Li3' 156.1(3) . . ? C27' C29' Li3' 79.5(2) . . ? O3' C29' Li2' 38.82(16) . . ? C30' C29' Li2' 112.2(2) . . ? C27' C29' Li2' 135.0(2) . . ? Li3' C29' Li2' 55.82(17) . . ? C31' C30' C35' 117.2(3) . . ? C31' C30' C29' 121.0(3) . . ? C35' C30' C29' 121.7(3) . . ? C30' C31' C32' 121.1(4) . . ? C33' C32' C31' 120.7(4) . . ? C34' C33' C32' 119.3(4) . . ? C33' C34' C35' 119.5(4) . . ? C30' C35' C34' 122.2(4) . . ? N3' C36' C37' 105.9(3) . . ? C36' C37' C38' 105.4(3) . . ? C39' C38' C37' 103.5(3) . . ? N3' C39' C38' 103.7(3) . . ? N4' C40' C41' 112.3(3) . . ? N4' C40' C42' 107.5(2) . . ? C41' C40' C42' 110.8(3) . . ? N4' C40' Li4' 47.62(18) . . ? C41' C40' Li4' 98.7(2) . . ? C42' C40' Li4' 70.7(2) . . ? O4' C42' C43' 112.5(3) . . ? O4' C42' C40' 110.5(3) . . ? C43' C42' C40' 113.8(3) . . ? O4' C42' Li4' 45.42(17) . . ? C43' C42' Li4' 157.0(2) . . ? C40' C42' Li4' 76.3(2) . . ? C46' C45' C44' 120.4(4) . . ? C47' C46' C45' 118.8(4) . . ? C46' C47' C48' 120.5(4) . . ? C43' C48' C47' 121.6(4) . . ? C48' C43' C44' 116.4(3) . . ? C48' C43' C42' 124.7(3) . . ? C44' C43' C42' 118.8(3) . . ? C45' C44' C43' 122.2(3) . . ? N4' C49' C50' 101.8(3) . . ? C49' C50' C51' 104.6(3) . . ? C52' C51' C50' 104.4(4) . . ? N4' C52' C51' 105.6(3) . . ? _diffrn_measured_fraction_theta_max 0.883 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.883 _refine_diff_density_max 0.109 _refine_diff_density_min -0.165 _refine_diff_density_rms 0.029