#------------------------------------------------------------------------------ #$Date: 2019-11-30 03:26:34 +0200 (Sat, 30 Nov 2019) $ #$Revision: 244815 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125626.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7125626 loop_ _publ_author_name 'Steller, Beate' 'Fischer, Roland' 'Flock, Michaela' 'Hill, Michael' 'Liptrot, David' 'McMullin, Claire L.' 'Rajabi, Nasir A.' 'Tiefling, Kathrin' 'Wilson, Andrew SS' _publ_section_title ; Reductive Dehydrocoupling of Diphenyltin Dihydride with LiAlH4: Selective Synthesis and Structures of the First Bicyclo[2.2.1]heptastannane-1,4-diide and Bicyclo[2.2.2]octastannane-1,4-diide  ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C9CC07976A _journal_year 2019 _chemical_formula_moiety 'C60 H50 Sn7, 2(C16 H32 Li O8), C2 H4 O0.5' _chemical_formula_sum 'C98 H126 Li2 O17.5 Sn7' _chemical_formula_weight 2428.69 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2017-05-22 _audit_creation_method ; Olex2 1.2 (compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337) ; _audit_update_record ; 2017-07-11 deposited with the CCDC. 2019-11-28 downloaded from the CCDC. ; _cell_angle_alpha 82.634(2) _cell_angle_beta 76.623(3) _cell_angle_gamma 70.379(2) _cell_formula_units_Z 2 _cell_length_a 14.3301(9) _cell_length_b 15.1075(10) _cell_length_c 26.1181(19) _cell_measurement_reflns_used 5511 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.20 _cell_measurement_theta_min 2.61 _cell_volume 5173.7(6) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_temperature 100.01 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_unetI/netI 0.0275 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_number 145924 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.034 _diffrn_reflns_theta_min 1.875 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 1.722 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.723 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker software' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.559 _exptl_crystal_description Block _exptl_crystal_F_000 2420 _exptl_crystal_size_max 0.354 _exptl_crystal_size_mid 0.211 _exptl_crystal_size_min 0.136 _refine_diff_density_max 1.633 _refine_diff_density_min -1.389 _refine_diff_density_rms 0.125 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1399 _refine_ls_number_reflns 30024 _refine_ls_number_restraints 833 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0372 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+16.6424P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0912 _refine_ls_wR_factor_ref 0.1067 _reflns_Friedel_coverage 0.000 _reflns_number_gt 23308 _reflns_number_total 30024 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL RF244_0m in P-1 REM - ASU contents take account of 1 squeezed molecule of THF CELL 0.71073 14.3301 15.1075 26.1181 82.634 76.623 70.379 ZERR 2 0.0009 0.001 0.0019 0.002 0.003 0.002 LATT 1 SFAC C H Li O Sn UNIT 196 252 4 35 14 SADI 0.005 Sn6 C49A Sn6 C49 SADI 0.005 Sn2 C7A Sn2 C7 SADI 0.005 O7A C71A O7 C72 O7 C73 O7A C73A O8 C74 O8A C74A O8A C75A O8 C75 = O5A C76A O5A C69A O5 C76 O5 C69 O6 C70 O6A C70A O6 C71 O6A C72A SADI 0.005 C72A C71A C72 C71 C74A C73A C74 C73 C76A C75A C76 C75 C70 C69 = C70A C69A SADI 0.005 O5A Li1 O5 Li1 SADI 0.005 O8 Li1 O8A Li1 SADI 0.005 O7A Li1 O7 Li1 SADI 0.005 O6A Li1 O6 Li1 SADI 0.005 O9A Li2 O9 Li2 SADI 0.005 O10 Li2 O10A Li2 SADI 0.005 O11 Li2 O11A Li2 SADI 0.005 O12 Li2 O12A Li2 SADI 0.005 O9A C77A O9 C77 O9 C84 O9A C84A O12 C83 O12A C83A O12 C82 O12A = C82A O11 C81 O11A C81A O11 C80 O11A C80A O10 C79 O10A C79A O10A C78A O10 C78 SADI 0.005 C80 C79 C80A C79A C82A C81A C82 C81 C84A C83A C84 C83 C78A C77A = C78 C77 SADI 0.005 C95B C94A C95A C94 SIMU 0.02 0.01 2 O9 > O12 C77 > C84 SIMU 0.02 0.01 2 O9A > O12A C77A > C84A SIMU 0.02 0.01 2 C94 > C95B ISOR 0.01 0.02 C81A C81 C82A C82 O12A O12 C83A C83 O11 O11A C80 C80A C84A = C84 O10 O10A C78 C78A C77A C77 O9A O9 C79 C79A ISOR 0.01 0.02 C90 C92 C63 C64 O3 C65 C66 C62 ISOR 0.01 0.02 O5 O6 O7 O8 C69 C70 C71 C72 C73 C74 C75 C76 C74A O8A C76A O5A = C75A C69A C70A O6A C71A C72A O7A C73A EADP O6 O6A L.S. 30 PLAN 19 SIZE 0.136 0.211 0.354 TEMP -173.14 LIST 6 BOND BUMP ABIN fmap 2 acta SHEL 999 0.71 REM REM REM WGHT 0.043400 16.642403 FVAR 0.18256 SN1 5 0.785616 0.184666 0.841534 11.00000 0.02534 0.02597 = 0.01898 -0.00081 -0.00277 -0.00801 SN2 5 0.891611 0.085821 0.749367 11.00000 0.02107 0.02536 = 0.02267 -0.00473 -0.00741 -0.00142 SN3 5 0.799192 0.168386 0.662159 11.00000 0.02325 0.02676 = 0.02260 -0.00723 -0.00906 -0.00064 SN4 5 0.722772 0.437124 0.712159 11.00000 0.03037 0.02400 = 0.02563 -0.00006 -0.01310 -0.00482 SN5 5 0.817088 0.356939 0.798234 11.00000 0.02435 0.02513 = 0.01985 -0.00160 -0.00847 -0.00863 SN6 5 0.612545 0.248470 0.793013 11.00000 0.01842 0.02672 = 0.03141 -0.01019 -0.00156 -0.00661 SN7 5 0.619921 0.323293 0.686318 11.00000 0.02694 0.02917 = 0.03208 -0.01089 -0.01701 0.00275 C1 1 1.054975 0.057567 0.732182 11.00000 0.02499 0.03981 = 0.02932 -0.00856 -0.00884 -0.00463 C2 1 1.111167 0.008070 0.769250 11.00000 0.03411 0.11399 = 0.04521 0.02126 -0.02127 -0.02185 AFIX 43 H2 2 1.077581 -0.010523 0.802578 11.00000 -1.20000 AFIX 0 C3 1 1.216182 -0.014963 0.758518 11.00000 0.03729 0.17693 = 0.08323 0.03929 -0.03471 -0.02613 AFIX 43 H3 2 1.253281 -0.049683 0.784391 11.00000 -1.20000 AFIX 0 C4 1 1.266116 0.011798 0.711331 11.00000 0.02696 0.13201 = 0.08152 -0.00042 -0.01383 -0.01984 AFIX 43 H4 2 1.337806 -0.005151 0.704007 11.00000 -1.20000 AFIX 0 C5 1 1.212535 0.063074 0.674676 11.00000 0.03541 0.07809 = 0.05053 -0.01970 0.00464 -0.02266 AFIX 43 H5 2 1.246657 0.083737 0.642096 11.00000 -1.20000 AFIX 0 C6 1 1.108717 0.084953 0.684913 11.00000 0.03288 0.05121 = 0.03557 -0.01115 -0.00413 -0.01237 AFIX 43 H6 2 1.072656 0.119995 0.658715 11.00000 -1.20000 AFIX 0 C13 1 0.749682 0.057329 0.642787 11.00000 0.02964 0.03416 = 0.02084 -0.00560 -0.00557 -0.00768 C14 1 0.816400 -0.030163 0.627517 11.00000 0.03128 0.03734 = 0.05329 -0.01618 -0.00649 -0.00567 AFIX 43 H14 2 0.887074 -0.040639 0.622089 11.00000 -1.20000 AFIX 0 C15 1 0.782762 -0.102690 0.619966 11.00000 0.05069 0.03852 = 0.04070 -0.01695 0.00185 -0.01647 AFIX 43 H15 2 0.830242 -0.161822 0.609631 11.00000 -1.20000 AFIX 0 C16 1 0.680732 -0.089111 0.627422 11.00000 0.06033 0.05181 = 0.03351 -0.00491 -0.00588 -0.03380 AFIX 43 H16 2 0.657377 -0.138318 0.621892 11.00000 -1.20000 AFIX 0 C17 1 0.612857 -0.003196 0.643018 11.00000 0.03954 0.06029 = 0.05943 -0.00235 -0.00612 -0.02711 AFIX 43 H17 2 0.542284 0.006452 0.648884 11.00000 -1.20000 AFIX 0 C18 1 0.646825 0.069161 0.650198 11.00000 0.03224 0.04166 = 0.03441 -0.00338 -0.00301 -0.01309 AFIX 43 H18 2 0.598916 0.128179 0.660403 11.00000 -1.20000 AFIX 0 C19 1 0.918546 0.181213 0.594969 11.00000 0.02802 0.03167 = 0.02287 -0.00351 -0.01056 -0.00330 C20 1 0.958624 0.254005 0.593189 11.00000 0.04213 0.03714 = 0.02740 -0.00614 -0.01020 -0.01085 AFIX 43 H20 2 0.930171 0.298608 0.619652 11.00000 -1.20000 AFIX 0 C21 1 1.039026 0.263137 0.553788 11.00000 0.04482 0.04868 = 0.03168 -0.00004 -0.00925 -0.01837 AFIX 43 H21 2 1.065533 0.312914 0.553877 11.00000 -1.20000 AFIX 0 C22 1 1.080531 0.199948 0.514458 11.00000 0.03616 0.05089 = 0.02927 0.00174 -0.00571 -0.00838 AFIX 43 H22 2 1.135153 0.206374 0.487270 11.00000 -1.20000 AFIX 0 C23 1 1.042049 0.127427 0.514962 11.00000 0.03206 0.03704 = 0.02848 -0.00366 -0.00807 0.00498 AFIX 43 H23 2 1.070306 0.083753 0.488012 11.00000 -1.20000 AFIX 0 C24 1 0.961931 0.117946 0.554816 11.00000 0.02992 0.03019 = 0.02873 -0.00445 -0.01165 0.00091 AFIX 43 H24 2 0.936301 0.067581 0.554714 11.00000 -1.20000 AFIX 0 C25 1 0.824536 0.482460 0.647291 11.00000 0.04021 0.03324 = 0.02696 0.00070 -0.00985 -0.00949 C26 1 0.789136 0.520404 0.600944 11.00000 0.04756 0.05528 = 0.02975 0.00253 -0.01547 -0.01146 AFIX 43 H26 2 0.723243 0.522596 0.598542 11.00000 -1.20000 AFIX 0 C27 1 0.847620 0.554715 0.558643 11.00000 0.06240 0.06435 = 0.02762 0.00883 -0.01588 -0.02207 AFIX 43 H27 2 0.821277 0.581707 0.527990 11.00000 -1.20000 AFIX 0 C28 1 0.944784 0.549604 0.561104 11.00000 0.06801 0.05632 = 0.03110 0.00698 -0.00513 -0.02797 AFIX 43 H28 2 0.985142 0.573574 0.532251 11.00000 -1.20000 AFIX 0 C29 1 0.982913 0.509524 0.605664 11.00000 0.05304 0.06250 = 0.04857 0.01224 -0.01483 -0.03117 AFIX 43 H29 2 1.050240 0.504123 0.607137 11.00000 -1.20000 AFIX 0 C30 1 0.922125 0.477078 0.648414 11.00000 0.05218 0.05364 = 0.03896 0.01421 -0.01917 -0.02682 AFIX 43 H30 2 0.948526 0.450582 0.679110 11.00000 -1.20000 AFIX 0 C31 1 0.623283 0.575273 0.737942 11.00000 0.03300 0.02397 = 0.04040 -0.00125 -0.02187 -0.00622 C32 1 0.539362 0.583445 0.778960 11.00000 0.03530 0.02610 = 0.05083 -0.00727 -0.00900 -0.00622 AFIX 43 H32 2 0.519631 0.529271 0.791694 11.00000 -1.20000 AFIX 0 C33 1 0.484241 0.668004 0.801539 11.00000 0.03938 0.03435 = 0.06760 -0.01373 -0.00732 -0.00258 AFIX 43 H33 2 0.427625 0.671391 0.829528 11.00000 -1.20000 AFIX 0 C34 1 0.511313 0.747684 0.783483 11.00000 0.05939 0.02330 = 0.06726 -0.01152 -0.02961 -0.00527 AFIX 43 H34 2 0.474388 0.805600 0.799567 11.00000 -1.20000 AFIX 0 C35 1 0.592435 0.742980 0.741863 11.00000 0.06402 0.02521 = 0.06028 0.00647 -0.04016 -0.01762 AFIX 43 H35 2 0.610052 0.798073 0.728675 11.00000 -1.20000 AFIX 0 C36 1 0.647843 0.657862 0.719491 11.00000 0.04420 0.03026 = 0.03919 0.00518 -0.02154 -0.01382 AFIX 43 H36 2 0.703607 0.655243 0.691086 11.00000 -1.20000 AFIX 0 C37 1 0.970108 0.364925 0.784164 11.00000 0.02890 0.03845 = 0.02771 0.00541 -0.01192 -0.01415 C38 1 0.988048 0.446975 0.792184 11.00000 0.04365 0.04307 = 0.04865 0.00303 -0.01739 -0.02361 AFIX 43 H38 2 0.932266 0.501413 0.802386 11.00000 -1.20000 AFIX 0 C39 1 1.085658 0.450636 0.785561 11.00000 0.05582 0.07429 = 0.06755 0.00818 -0.02448 -0.04379 AFIX 43 H39 2 1.096066 0.507403 0.790841 11.00000 -1.20000 AFIX 0 C40 1 1.166746 0.372753 0.771467 11.00000 0.03826 0.09248 = 0.06923 0.00955 -0.01626 -0.03411 AFIX 43 H40 2 1.233642 0.374855 0.767200 11.00000 -1.20000 AFIX 0 C41 1 1.150638 0.291286 0.763514 11.00000 0.03237 0.06765 = 0.08557 0.00160 -0.00317 -0.00675 AFIX 43 H41 2 1.206750 0.236702 0.754067 11.00000 -1.20000 AFIX 0 C42 1 1.053245 0.288128 0.769163 11.00000 0.03353 0.04135 = 0.05788 -0.00042 -0.00535 -0.01033 AFIX 43 H42 2 1.043691 0.231706 0.762533 11.00000 -1.20000 AFIX 0 C43 1 0.747116 0.451804 0.862696 11.00000 0.03345 0.04114 = 0.04311 -0.01854 -0.00960 -0.00975 C44 1 0.732045 0.412379 0.914633 11.00000 0.08974 0.05868 = 0.03430 -0.01690 0.00287 -0.02367 AFIX 43 H44 2 0.751237 0.345917 0.920635 11.00000 -1.20000 AFIX 0 C45 1 0.689104 0.469980 0.957537 11.00000 0.12671 0.07716 = 0.04438 -0.03239 0.01457 -0.02503 AFIX 43 H45 2 0.681962 0.442383 0.992421 11.00000 -1.20000 AFIX 0 C46 1 0.657960 0.564175 0.949534 11.00000 0.10488 0.08020 = 0.05794 -0.04216 0.00534 -0.02719 AFIX 43 H46 2 0.626889 0.602632 0.978794 11.00000 -1.20000 AFIX 0 C47 1 0.670586 0.605220 0.899620 11.00000 0.06808 0.04717 = 0.09423 -0.03538 -0.01291 -0.01498 AFIX 43 H47 2 0.648996 0.671853 0.894484 11.00000 -1.20000 AFIX 0 C48 1 0.715359 0.549092 0.856008 11.00000 0.05243 0.04440 = 0.05744 -0.02061 -0.01725 -0.01515 AFIX 43 H48 2 0.723968 0.578160 0.821531 11.00000 -1.20000 AFIX 66 C60 1 0.512101 0.394920 0.881057 11.00000 0.03204 0.04395 = 0.04095 -0.01716 0.00980 -0.01615 AFIX 43 H60 2 0.573325 0.363838 0.893108 11.00000 -1.20000 AFIX 65 C59 1 0.441978 0.473493 0.905818 11.00000 0.04641 0.04965 = 0.04884 -0.02622 0.01337 -0.02143 AFIX 43 H59 2 0.455276 0.496112 0.934791 11.00000 -1.20000 AFIX 65 C58 1 0.352398 0.518972 0.888185 11.00000 0.04233 0.03827 = 0.06079 -0.02589 0.02043 -0.01009 AFIX 43 H58 2 0.304473 0.572673 0.905108 11.00000 -1.20000 AFIX 65 C57 1 0.332940 0.485878 0.845792 11.00000 0.03291 0.03461 = 0.05987 -0.01160 0.00751 -0.00693 AFIX 43 H57 2 0.271716 0.516961 0.833742 11.00000 -1.20000 AFIX 65 C56 1 0.403061 0.407305 0.821032 11.00000 0.02865 0.03291 = 0.04877 -0.01292 0.00415 -0.00943 AFIX 43 H56 2 0.389762 0.384687 0.792058 11.00000 -1.20000 AFIX 65 C55 1 0.492642 0.361826 0.838664 11.00000 0.02374 0.02730 = 0.03962 -0.01233 0.00697 -0.01069 AFIX 0 PART 1 C7 1 0.897715 -0.062222 0.754779 10.50000 0.02515 0.04239 = 0.01747 -0.00927 -0.00172 -0.01102 C8 1 0.983854 -0.136176 0.759192 10.50000 0.02969 0.02706 = 0.02390 -0.00024 -0.00542 -0.00362 AFIX 43 H8 2 1.042920 -0.122490 0.761180 10.50000 -1.20000 AFIX 0 C9 1 0.988788 -0.230363 0.760894 10.50000 0.04547 0.03182 = 0.03909 -0.00398 0.00420 -0.00875 AFIX 43 H9 2 1.049360 -0.279467 0.764728 10.50000 -1.20000 AFIX 0 C10 1 0.904313 -0.250517 0.756912 10.50000 0.05258 0.03243 = 0.02485 -0.00192 0.00357 -0.01289 AFIX 43 H10 2 0.907340 -0.314199 0.756423 10.50000 -1.20000 AFIX 0 C11 1 0.814350 -0.178825 0.753584 10.50000 0.04788 0.04842 = 0.03349 0.01110 -0.01918 -0.02769 AFIX 43 H11 2 0.755457 -0.193004 0.751798 10.50000 -1.20000 AFIX 0 C12 1 0.812190 -0.086814 0.752925 10.50000 0.02903 0.03542 = 0.04273 0.01177 -0.01974 -0.00758 AFIX 43 H12 2 0.750395 -0.037949 0.751146 10.50000 -1.20000 AFIX 0 C49 1 0.535323 0.142380 0.796458 10.65000 0.02406 0.02812 = 0.03153 -0.01375 -0.00732 -0.00552 C50 1 0.455337 0.161339 0.771246 10.65000 0.02320 0.02565 = 0.04153 -0.00577 -0.01005 -0.00250 AFIX 43 H50 2 0.431795 0.221150 0.753629 10.65000 -1.20000 AFIX 0 C51 1 0.409576 0.094917 0.771349 10.65000 0.03177 0.03082 = 0.06169 -0.00923 -0.02006 -0.00660 AFIX 43 H51 2 0.353219 0.108960 0.754945 10.65000 -1.20000 AFIX 0 C52 1 0.446724 0.006985 0.795731 10.65000 0.03918 0.02319 = 0.10129 0.00200 -0.02281 -0.01828 AFIX 43 H52 2 0.415816 -0.039782 0.796037 10.65000 -1.20000 AFIX 0 C53 1 0.526739 -0.012478 0.819069 10.65000 0.05795 0.03477 = 0.12949 0.01945 -0.05210 -0.02096 AFIX 43 H53 2 0.553281 -0.073463 0.834813 10.65000 -1.20000 AFIX 0 C54 1 0.570447 0.056809 0.820088 10.65000 0.04489 0.03412 = 0.08142 0.01096 -0.03759 -0.01647 AFIX 43 H54 2 0.625290 0.043498 0.837556 10.65000 -1.20000 AFIX 66 PART 0 PART 2 C7A 1 0.879197 -0.056727 0.759015 10.50000 0.02510 0.02362 = 0.02392 0.00024 -0.01216 -0.00179 C12A 1 0.782330 -0.064170 0.772576 10.50000 0.03323 0.03826 = 0.09038 -0.02218 -0.02718 -0.00518 AFIX 43 H12A 2 0.725697 -0.010142 0.782326 10.50000 -1.20000 AFIX 65 C11A 1 0.768326 -0.150664 0.771872 10.50000 0.04496 0.05196 = 0.06305 -0.01159 -0.02076 -0.01290 AFIX 43 H11A 2 0.702121 -0.155750 0.781140 10.50000 -1.20000 AFIX 65 C10A 1 0.851188 -0.229716 0.757607 10.50000 0.06434 0.03715 = 0.04115 -0.00737 -0.01393 -0.02037 AFIX 43 H10A 2 0.841616 -0.288830 0.757126 10.50000 -1.20000 AFIX 65 C9A 1 0.948056 -0.222274 0.744045 10.50000 0.05931 0.03288 = 0.03622 -0.00036 0.00236 -0.00802 AFIX 43 H9A 2 1.004689 -0.276303 0.734296 10.50000 -1.20000 AFIX 65 C8A 1 0.962062 -0.135781 0.744749 10.50000 0.03670 0.03602 = 0.02389 -0.00200 -0.00737 -0.00582 AFIX 43 H8A 2 1.028267 -0.130695 0.735480 10.50000 -1.20000 AFIX 66 C49A 1 0.544970 0.132153 0.821480 10.35000 0.01164 0.04415 = 0.03783 -0.02746 0.00091 -0.01122 C50A 1 0.510210 0.096196 0.785901 10.35000 0.04087 0.05023 = 0.02981 -0.00897 -0.00718 -0.02312 AFIX 43 H50A 2 0.510736 0.123806 0.751087 10.35000 -1.20000 AFIX 65 C51A 1 0.474682 0.019839 0.801259 10.35000 0.06011 0.05230 = 0.07110 -0.01967 -0.00059 -0.04596 AFIX 43 H51A 2 0.450926 -0.004736 0.776942 10.35000 -1.20000 AFIX 65 C52A 1 0.473912 -0.020560 0.852196 10.35000 0.05133 0.04077 = 0.06283 -0.00879 0.00438 -0.02726 AFIX 43 H52A 2 0.449630 -0.072747 0.862692 10.35000 -1.20000 AFIX 65 C53A 1 0.508671 0.015397 0.887776 10.35000 0.04832 0.04072 = 0.05392 0.01737 -0.01759 -0.02405 AFIX 43 H53A 2 0.508145 -0.012215 0.922589 10.35000 -1.20000 AFIX 65 C54A 1 0.544200 0.091753 0.872419 10.35000 0.04317 0.04948 = 0.03496 0.01091 -0.01716 -0.02764 AFIX 43 H54A 2 0.567956 0.116328 0.896736 10.35000 -1.20000 AFIX 0 PART 0 O1 4 0.828698 0.930438 0.961156 11.00000 0.07910 0.05967 = 0.06149 0.01355 -0.02963 -0.03779 O2 4 1.028201 0.830819 0.952236 11.00000 0.08630 0.06048 = 0.06694 0.00321 -0.01694 -0.00522 O3 4 0.989011 0.674183 0.928298 11.00000 0.20015 0.07456 = 0.11791 0.00063 -0.07480 -0.01967 O4 4 0.792230 0.777734 0.936036 11.00000 0.22501 0.11278 = 0.04121 0.02701 -0.05108 -0.12134 PART 1 O5 4 0.732195 0.835385 1.050278 10.60000 0.07876 0.08037 = 0.04603 0.01175 -0.02367 -0.04439 O6 4 0.887061 0.879328 1.067566 10.60000 0.06315 0.06735 = 0.04656 0.00322 -0.02320 -0.00976 O7 4 0.994146 0.695661 1.047640 10.60000 0.10115 0.03243 = 0.03427 0.01364 -0.02975 -0.01037 O8 4 0.823871 0.655041 1.033210 10.60000 0.06187 0.05675 = 0.03071 0.00610 -0.01240 -0.02231 PART 0 PART 2 O5A 4 0.745565 0.775573 1.051554 10.40000 0.06733 0.03593 = 0.04044 0.01297 -0.01928 -0.01892 O6A 4 0.878775 0.884485 1.067078 10.40000 0.06315 0.06735 = 0.04656 0.00322 -0.02320 -0.00976 O7A 4 1.026510 0.716716 1.031457 10.40000 0.11037 0.04895 = 0.06222 -0.00971 -0.04217 -0.02345 O8A 4 0.908026 0.620161 1.017654 10.40000 0.04520 0.03357 = 0.03895 0.00518 -0.00742 -0.01682 PART 0 C61 1 0.904099 0.976288 0.951250 11.00000 0.09055 0.04353 = 0.08195 0.02376 -0.03901 -0.03626 AFIX 23 H61A 2 0.913308 0.991620 0.985108 11.00000 -1.20000 H61B 2 0.881617 1.035916 0.930107 11.00000 -1.20000 AFIX 0 C62 1 1.001471 0.915071 0.922546 11.00000 0.08228 0.08540 = 0.09064 0.03259 0.00045 -0.04270 AFIX 23 H62A 2 0.994340 0.903418 0.887418 11.00000 -1.20000 H62B 2 1.054310 0.945761 0.917590 11.00000 -1.20000 AFIX 0 C63 1 1.105301 0.757801 0.922045 11.00000 0.09234 0.14035 = 0.11631 -0.05306 -0.05113 0.01971 AFIX 23 H63A 2 1.145709 0.712938 0.945962 11.00000 -1.20000 H63B 2 1.151206 0.786045 0.896181 11.00000 -1.20000 AFIX 0 C64 1 1.061376 0.702970 0.892082 11.00000 0.11673 0.13455 = 0.12176 -0.03481 -0.05919 0.01429 AFIX 23 H64A 2 1.030756 0.744239 0.863674 11.00000 -1.20000 H64B 2 1.115791 0.647779 0.876066 11.00000 -1.20000 AFIX 0 C65 1 0.917913 0.659169 0.900367 11.00000 0.20411 0.07458 = 0.08159 -0.00548 -0.08239 -0.03418 AFIX 23 H65A 2 0.956735 0.629555 0.866940 11.00000 -1.20000 H65B 2 0.886141 0.614199 0.922088 11.00000 -1.20000 AFIX 0 C66 1 0.840396 0.741308 0.888657 11.00000 0.14281 0.10601 = 0.06998 -0.00187 -0.04160 -0.06015 AFIX 23 H66A 2 0.869245 0.786367 0.864953 11.00000 -1.20000 H66B 2 0.793431 0.725607 0.871619 11.00000 -1.20000 AFIX 0 C67 1 0.720980 0.873345 0.930754 11.00000 0.14662 0.14622 = 0.09233 0.04638 -0.06558 -0.10551 AFIX 23 H67A 2 0.686819 0.877321 0.901248 11.00000 -1.20000 H67B 2 0.668626 0.887033 0.963466 11.00000 -1.20000 AFIX 0 C68 1 0.773635 0.941692 0.921074 11.00000 0.06829 0.07649 = 0.06496 0.00211 -0.02892 -0.02654 AFIX 23 H68A 2 0.820349 0.932948 0.886310 11.00000 -1.20000 H68B 2 0.724546 1.005978 0.920696 11.00000 -1.20000 AFIX 0 PART 1 C69 1 0.711432 0.919340 1.077371 10.60000 0.07726 0.07473 = 0.06284 -0.01665 -0.02506 -0.00784 AFIX 23 H69A 2 0.646415 0.930914 1.103055 10.60000 -1.20000 H69B 2 0.706094 0.974233 1.051752 10.60000 -1.20000 AFIX 0 C70 1 0.792141 0.907296 1.104314 10.60000 0.06736 0.04441 = 0.05306 -0.00868 0.00006 0.00511 AFIX 23 H70A 2 0.783301 0.967082 1.119467 10.60000 -1.20000 H70B 2 0.791027 0.858602 1.133475 10.60000 -1.20000 AFIX 0 C71 1 0.979883 0.831197 1.085404 10.60000 0.06870 0.05625 = 0.05570 -0.00313 -0.02757 -0.02091 AFIX 23 H71A 2 0.980524 0.859124 1.117552 10.60000 -1.20000 H71B 2 1.038247 0.836990 1.057831 10.60000 -1.20000 AFIX 0 C72 1 0.986595 0.733626 1.096590 10.60000 0.06140 0.04783 = 0.03344 0.00771 -0.02717 -0.01697 AFIX 23 H72A 2 1.046886 0.699188 1.111844 10.60000 -1.20000 H72B 2 0.925717 0.727882 1.122122 10.60000 -1.20000 AFIX 0 C73 1 0.983291 0.603278 1.054614 10.60000 0.05676 0.04484 = 0.04382 0.01116 -0.01394 -0.01341 AFIX 23 H73A 2 1.022874 0.566149 1.081018 10.60000 -1.20000 H73B 2 1.013716 0.572091 1.020857 10.60000 -1.20000 AFIX 0 C74 1 0.881419 0.599597 1.071154 10.60000 0.07497 0.04170 = 0.04684 0.01030 -0.01916 -0.02440 AFIX 23 H74A 2 0.881543 0.533677 1.073142 10.60000 -1.20000 H74B 2 0.851127 0.625011 1.106467 10.60000 -1.20000 AFIX 0 C75 1 0.716987 0.693550 1.052599 10.60000 0.05696 0.05391 = 0.03227 0.00510 -0.00927 -0.01868 AFIX 23 H75A 2 0.692961 0.643220 1.073655 10.60000 -1.20000 H75B 2 0.683313 0.711821 1.022002 10.60000 -1.20000 AFIX 0 C76 1 0.684490 0.773581 1.084362 10.60000 0.06524 0.07874 = 0.05157 -0.00228 0.00300 -0.02492 AFIX 23 H76A 2 0.609919 0.801590 1.091982 10.60000 -1.20000 H76B 2 0.708903 0.756954 1.117920 10.60000 -1.20000 AFIX 0 PART 0 PART 2 C69A 1 0.739067 0.807457 1.102178 10.40000 0.06183 0.06547 = 0.04969 -0.01460 -0.00385 -0.01397 AFIX 23 H69C 2 0.767882 0.751956 1.124935 10.40000 -1.20000 H69D 2 0.666673 0.834990 1.118346 10.40000 -1.20000 AFIX 0 C70A 1 0.788928 0.875515 1.102466 10.40000 0.09353 0.10853 = 0.09253 -0.01242 0.00839 -0.04260 AFIX 23 H70C 2 0.736699 0.937671 1.100128 10.40000 -1.20000 H70D 2 0.803678 0.868716 1.138233 10.40000 -1.20000 AFIX 0 C71A 1 1.045894 0.772608 1.066011 10.40000 0.06137 0.05257 = 0.05212 -0.01034 -0.01729 -0.02721 AFIX 23 H71C 2 1.086680 0.810831 1.044617 10.40000 -1.20000 H71D 2 1.086678 0.729910 1.090482 10.40000 -1.20000 AFIX 0 C72A 1 0.955975 0.834506 1.096449 10.40000 0.05055 0.04484 = 0.05383 -0.01472 -0.02801 -0.01064 AFIX 23 H72C 2 0.927470 0.796982 1.125960 10.40000 -1.20000 H72D 2 0.975057 0.880897 1.111866 10.40000 -1.20000 AFIX 0 C73A 1 1.032231 0.628514 1.061299 10.40000 0.07173 0.07709 = 0.09956 0.02431 -0.04960 -0.02913 AFIX 23 H73C 2 0.986536 0.639920 1.096259 10.40000 -1.20000 H73D 2 1.102113 0.596517 1.066757 10.40000 -1.20000 AFIX 0 C74A 1 1.003050 0.570384 1.032729 10.40000 0.06612 0.05237 = 0.06911 -0.00363 -0.01918 -0.00973 AFIX 23 H74C 2 1.055791 0.549922 1.000790 10.40000 -1.20000 H74D 2 0.997562 0.513459 1.054999 10.40000 -1.20000 AFIX 0 C75A 1 0.823198 0.607631 1.056098 10.40000 0.06385 0.04600 = 0.06163 0.01208 0.00452 -0.03221 AFIX 23 H75C 2 0.833898 0.607732 1.092202 10.40000 -1.20000 H75D 2 0.813639 0.547165 1.052037 10.40000 -1.20000 AFIX 0 C76A 1 0.736614 0.685268 1.046701 10.40000 0.06378 0.08481 = 0.09084 0.00330 -0.00377 -0.03969 AFIX 23 H76C 2 0.726455 0.682516 1.010786 10.40000 -1.20000 H76D 2 0.675927 0.678595 1.072048 10.40000 -1.20000 AFIX 0 PART 0 LI1 3 0.884679 0.785298 0.997978 11.00000 0.08571 0.04729 = 0.04752 0.01325 -0.02894 -0.03251 O13 4 0.178082 0.640629 0.576696 11.00000 0.04654 0.03888 = 0.04981 0.00298 -0.01296 0.00193 O14 4 0.327162 0.691373 0.502291 11.00000 0.03733 0.04699 = 0.03804 -0.00097 -0.01796 -0.00732 O15 4 0.297041 0.854153 0.548808 11.00000 0.04321 0.04814 = 0.04476 0.00116 -0.02145 -0.00977 O16 4 0.152876 0.803118 0.622999 11.00000 0.03512 0.04610 = 0.04727 -0.00955 -0.01507 -0.00016 PART 1 O9 4 0.355417 0.781074 0.648028 10.65000 0.04885 0.07376 = 0.02900 -0.00402 -0.01948 -0.00531 O10 4 0.483276 0.686057 0.564466 10.65000 0.04583 0.06143 = 0.05569 -0.02606 -0.03428 0.01547 O11 4 0.387940 0.552482 0.596872 10.65000 0.05295 0.06524 = 0.08257 0.03781 -0.04106 -0.00728 O12 4 0.261644 0.646918 0.684854 10.65000 0.08724 0.08283 = 0.05540 0.00680 -0.03643 -0.01915 PART 0 PART 2 O9A 4 0.349230 0.759661 0.659018 10.35000 0.04204 0.07870 = 0.03273 0.00979 -0.01748 0.00376 O10A 4 0.480229 0.698691 0.563192 10.35000 0.03996 0.04248 = 0.04926 -0.00980 -0.01934 -0.00083 O11A 4 0.403557 0.556536 0.581791 10.35000 0.05722 0.06765 = 0.06551 0.03844 -0.01269 -0.01743 O12A 4 0.266773 0.608301 0.672715 10.35000 0.05693 0.06941 = 0.05671 -0.00613 -0.01565 0.01427 PART 0 C85 1 0.183065 0.638376 0.523442 11.00000 0.11740 0.15433 = 0.06531 -0.04049 0.00188 -0.09387 AFIX 23 H85A 2 0.169769 0.580534 0.517761 11.00000 -1.20000 H85B 2 0.127390 0.692569 0.513322 11.00000 -1.20000 AFIX 0 C86 1 0.271124 0.640537 0.489601 11.00000 0.08557 0.12059 = 0.05947 -0.03952 0.00718 -0.06425 AFIX 23 H86A 2 0.254392 0.665976 0.454813 11.00000 -1.20000 H86B 2 0.315782 0.574686 0.485218 11.00000 -1.20000 AFIX 0 C87 1 0.312608 0.778316 0.472942 11.00000 0.17793 0.07295 = 0.03785 0.01510 -0.04285 -0.06070 AFIX 23 H87A 2 0.358699 0.767444 0.438066 11.00000 -1.20000 H87B 2 0.242523 0.800851 0.466861 11.00000 -1.20000 AFIX 0 C88 1 0.327947 0.847611 0.494799 11.00000 0.11840 0.05726 = 0.05185 -0.00384 0.02169 -0.03618 AFIX 23 H88A 2 0.292937 0.908472 0.477918 11.00000 -1.20000 H88B 2 0.401233 0.839516 0.485622 11.00000 -1.20000 AFIX 0 C89 1 0.201426 0.919500 0.566266 11.00000 0.09136 0.03745 = 0.04735 0.00274 -0.01106 0.00905 AFIX 23 H89A 2 0.210666 0.980529 0.569354 11.00000 -1.20000 H89B 2 0.160748 0.928916 0.538942 11.00000 -1.20000 AFIX 0 C90 1 0.146101 0.895125 0.614444 11.00000 0.06277 0.04870 = 0.13969 -0.02278 0.02464 -0.01608 AFIX 23 H90A 2 0.169111 0.913417 0.643242 11.00000 -1.20000 H90B 2 0.073995 0.932661 0.616610 11.00000 -1.20000 AFIX 0 C91 1 0.070198 0.782051 0.616189 11.00000 0.03392 0.05156 = 0.11066 -0.02312 0.00350 -0.01027 AFIX 23 H91A 2 0.042538 0.825272 0.587575 11.00000 -1.20000 H91B 2 0.017891 0.796789 0.648856 11.00000 -1.20000 AFIX 0 C92 1 0.083353 0.690345 0.604360 11.00000 0.05144 0.09767 = 0.14369 -0.06400 0.00318 -0.01910 AFIX 23 H92A 2 0.068577 0.654112 0.637879 11.00000 -1.20000 H92B 2 0.032493 0.693367 0.583636 11.00000 -1.20000 AFIX 0 PART 1 C77 1 0.447250 0.801879 0.626347 10.65000 0.05625 0.07323 = 0.06648 -0.01817 -0.03738 -0.00514 AFIX 23 H77A 2 0.473898 0.814499 0.655446 10.65000 -1.20000 H77B 2 0.432153 0.859971 0.603178 10.65000 -1.20000 AFIX 0 C78 1 0.524533 0.727684 0.596444 10.65000 0.05902 0.06930 = 0.04316 -0.00684 -0.01117 -0.02890 AFIX 23 H78A 2 0.575810 0.753587 0.573568 10.65000 -1.20000 H78B 2 0.558709 0.678560 0.620970 10.65000 -1.20000 AFIX 0 C79 1 0.531688 0.591944 0.547997 10.65000 0.06240 0.07098 = 0.08780 -0.00955 -0.02019 0.00139 AFIX 23 H79A 2 0.605238 0.575620 0.546282 10.65000 -1.20000 H79B 2 0.521939 0.589779 0.511925 10.65000 -1.20000 AFIX 0 C80 1 0.495897 0.521488 0.581515 10.65000 0.07192 0.04788 = 0.06979 0.01155 -0.01723 0.00023 AFIX 23 H80A 2 0.518374 0.462889 0.562544 10.65000 -1.20000 H80B 2 0.525758 0.507232 0.613401 10.65000 -1.20000 AFIX 0 C81 1 0.352559 0.504198 0.644161 10.65000 0.07757 0.07357 = 0.09621 0.02246 -0.01998 -0.01292 AFIX 23 H81A 2 0.403646 0.441853 0.648041 10.65000 -1.20000 H81B 2 0.289502 0.493634 0.641214 10.65000 -1.20000 AFIX 0 C82 1 0.333187 0.555137 0.690658 10.65000 0.10216 0.09672 = 0.08267 0.02013 -0.02428 -0.00864 AFIX 23 H82A 2 0.305995 0.520266 0.722027 10.65000 -1.20000 H82B 2 0.397071 0.561139 0.695801 10.65000 -1.20000 AFIX 0 C83 1 0.275886 0.704605 0.719912 10.65000 0.04305 0.09634 = 0.05021 -0.01158 -0.01677 -0.00427 AFIX 23 H83A 2 0.286225 0.667206 0.753329 10.65000 -1.20000 H83B 2 0.212888 0.758184 0.728077 10.65000 -1.20000 AFIX 0 C84 1 0.359411 0.741743 0.700814 10.65000 0.07039 0.09859 = 0.06118 -0.01067 -0.02488 -0.01134 AFIX 23 H84A 2 0.354566 0.790903 0.723881 10.65000 -1.20000 H84B 2 0.424380 0.690827 0.701218 10.65000 -1.20000 AFIX 0 PART 0 PART 2 C77A 1 0.448044 0.768512 0.642487 10.35000 0.04066 0.05263 = 0.04314 -0.01007 -0.00664 -0.00664 AFIX 23 H77C 2 0.475023 0.767034 0.674335 10.35000 -1.20000 H77D 2 0.441681 0.831096 0.624035 10.35000 -1.20000 AFIX 0 C78A 1 0.521258 0.698097 0.608361 10.35000 0.03386 0.04732 = 0.04198 -0.00064 -0.02064 0.00661 AFIX 23 H78C 2 0.585668 0.712641 0.597350 10.35000 -1.20000 H78D 2 0.534757 0.635273 0.627143 10.35000 -1.20000 AFIX 0 C79A 1 0.536488 0.610715 0.539892 10.35000 0.02534 0.03994 = 0.02039 0.00241 -0.01530 -0.00279 AFIX 23 H79C 2 0.610186 0.600246 0.533073 10.35000 -1.20000 H79D 2 0.516643 0.607048 0.506544 10.35000 -1.20000 AFIX 0 C80A 1 0.507771 0.544345 0.580149 10.35000 0.03840 0.05542 = 0.04575 0.02515 -0.00124 0.00760 AFIX 23 H80C 2 0.550114 0.479208 0.571505 10.35000 -1.20000 H80D 2 0.516752 0.556594 0.614748 10.35000 -1.20000 AFIX 0 C81A 1 0.364971 0.493097 0.619431 10.35000 0.05319 0.06560 = 0.05140 0.02290 -0.01111 -0.00203 AFIX 23 H81C 2 0.413648 0.428635 0.616046 10.35000 -1.20000 H81D 2 0.300392 0.492252 0.612274 10.35000 -1.20000 AFIX 0 C82A 1 0.348615 0.521797 0.672376 10.35000 0.05645 0.04016 = 0.04432 0.00354 -0.01826 0.00281 AFIX 23 H82C 2 0.329523 0.474718 0.699000 10.35000 -1.20000 H82D 2 0.409527 0.531877 0.678959 10.35000 -1.20000 AFIX 0 C83A 1 0.261645 0.666761 0.713063 10.35000 0.05418 0.05644 = 0.04068 0.00938 -0.01118 -0.00024 AFIX 23 H83C 2 0.254845 0.631164 0.747544 10.35000 -1.20000 H83D 2 0.200121 0.722322 0.714177 10.35000 -1.20000 AFIX 0 C84A 1 0.348459 0.698853 0.705844 10.35000 0.06076 0.07129 = 0.04780 0.00271 -0.01722 0.00162 AFIX 23 H84C 2 0.343697 0.733343 0.736613 10.35000 -1.20000 H84D 2 0.411454 0.644537 0.702183 10.35000 -1.20000 AFIX 0 PART 0 LI2 3 0.307137 0.708943 0.591289 11.00000 0.03734 0.05405 = 0.03585 0.00012 -0.01351 -0.00249 O20 4 0.254597 0.332292 0.572705 10.50000 0.06257 0.11992 = 0.04917 0.00651 -0.00809 -0.03602 C93 1 0.232842 0.317449 0.628019 10.50000 0.03604 0.07731 = 0.04919 -0.00098 -0.00614 -0.01789 AFIX 23 H93A 2 0.182434 0.283586 0.638859 10.50000 -1.20000 H93B 2 0.205824 0.378183 0.645215 10.50000 -1.20000 AFIX 0 C95 1 0.331700 0.259302 0.642725 10.50000 0.04117 0.04831 = 0.06199 0.01480 -0.01066 -0.01614 PART 1 AFIX 23 H95A 2 0.365359 0.298513 0.654294 10.25000 -1.20000 H95B 2 0.323462 0.209667 0.670413 10.25000 -1.20000 AFIX 23 PART 0 PART 2 H95C 2 0.345847 0.289063 0.670447 10.25000 -1.20000 H95D 2 0.329982 0.195387 0.656064 10.25000 -1.20000 AFIX 0 PART 0 PART 1 C94 1 0.383258 0.221790 0.594103 10.25000 0.03243 0.08183 = 0.05863 0.00867 0.00591 -0.00752 AFIX 23 H94A 2 0.406237 0.152253 0.598709 10.25000 -1.20000 H94B 2 0.444062 0.242046 0.581880 10.25000 -1.20000 AFIX 0 C95A 1 0.322406 0.250144 0.554162 10.25000 0.03295 0.06297 = 0.03690 0.01184 0.00787 -0.01547 AFIX 23 H95E 2 0.363084 0.260098 0.519036 10.25000 -1.20000 H95F 2 0.288727 0.203530 0.552225 10.25000 -1.20000 AFIX 0 PART 0 PART 2 C94A 1 0.408832 0.254626 0.594756 10.25000 0.02205 0.08413 = 0.04081 0.00216 0.00606 -0.00615 AFIX 23 H94C 2 0.457761 0.286056 0.597649 10.25000 -1.20000 H94D 2 0.445393 0.189125 0.584514 10.25000 -1.20000 AFIX 0 C95B 1 0.342588 0.306854 0.559484 10.25000 0.06339 0.10060 = 0.04449 0.01163 0.01321 -0.00139 AFIX 23 H95G 2 0.362514 0.363579 0.546031 10.25000 -1.20000 H95H 2 0.358973 0.267815 0.528946 10.25000 -1.20000 AFIX 0 HKLF 4 REM RF244_0m in P-1 REM R1 = 0.0372 for 23308 Fo > 4sig(Fo) and 0.0568 for all 30024 data REM 1399 parameters refined using 833 restraints END WGHT 0.0407 16.8540 REM Highest difference peak 1.633, deepest hole -1.389, 1-sigma level 0.125 Q1 1 0.1224 0.9002 0.5857 11.00000 0.05 1.63 Q2 1 0.7928 0.1256 0.6796 11.00000 0.05 1.53 Q3 1 0.6201 0.2878 0.7021 11.00000 0.05 1.48 Q4 1 0.2831 0.7886 0.7028 11.00000 0.05 1.43 Q5 1 0.0810 0.7257 0.5809 11.00000 0.05 1.32 Q6 1 0.6569 0.3285 0.6810 11.00000 0.05 1.19 Q7 1 0.2546 0.5576 0.6917 11.00000 0.05 1.16 Q8 1 0.7041 0.8418 1.0550 11.00000 0.05 1.11 Q9 1 0.5358 0.5824 0.5850 11.00000 0.05 1.10 Q10 1 0.7662 0.7794 1.0438 11.00000 0.05 1.07 Q11 1 0.7797 0.1406 0.8584 11.00000 0.05 1.06 Q12 1 0.8778 0.0628 0.7751 11.00000 0.05 1.03 Q13 1 0.7790 0.4153 0.7075 11.00000 0.05 0.97 Q14 1 0.6351 0.2711 0.7801 11.00000 0.05 0.96 Q15 1 0.5677 0.2626 0.7938 11.00000 0.05 0.96 Q16 1 1.0591 0.5891 1.0363 11.00000 0.05 0.95 Q17 1 1.0555 0.8601 0.8967 11.00000 0.05 0.94 Q18 1 0.3731 0.7389 0.4714 11.00000 0.05 0.93 Q19 1 0.9829 0.6595 0.8879 11.00000 0.05 0.92 REM The information below was added by Olex2. REM REM R1 = 0.0372 for 23308 Fo > 4sig(Fo) and 0.0568 for all 151767 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.63, deepest hole -1.39 REM Mean Shift 0, Max Shift 0.002. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0568 REM R1_gt = 0.0372 REM wR_ref = 0.1067 REM GOOF = 1.037 REM Shift_max = 0.002 REM Shift_mean = 0 REM Reflections_all = 151767 REM Reflections_gt = 23308 REM Parameters = n/a REM Hole = -1.39 REM Peak = 1.63 REM Flack = n/a ; _cod_data_source_file c9cc07976a2.cif _cod_data_source_block rf244_0m _cod_original_formula_sum 'C98 H126 Li2 O17.50 Sn7' _cod_database_code 7125626 _shelxl_version_number 2014-3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.800 _shelx_estimated_absorpt_t_min 0.581 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups 2. Restrained distances Sn6-C49A \\sim Sn6-C49 with sigma of 0.005 Sn2-C7A \\sim Sn2-C7 with sigma of 0.005 O7A-C71A \\sim O7-C72 \\sim O7-C73 \\sim O7A-C73A \\sim O8-C74 \\sim O8A-C74A \\sim O8A-C75A \\sim O8-C75 \\sim O5A-C76A \\sim O5A-C69A \\sim O5-C76 \\sim O5-C69 \\sim O6-C70 \\sim O6A-C70A \\sim O6-C71 \\sim O6A-C72A with sigma of 0.005 C72A-C71A \\sim C72-C71 \\sim C74A-C73A \\sim C74-C73 \\sim C76A-C75A \\sim C76-C75 \\sim C70-C69 C70A-C69A with sigma of 0.005 O5A-Li1 \\sim O5-Li1 with sigma of 0.005 O8-Li1 \\sim O8A-Li1 with sigma of 0.005 O7A-Li1 \\sim O7-Li1 with sigma of 0.005 O6A-Li1 \\sim O6-Li1 with sigma of 0.005 O9A-Li2 \\sim O9-Li2 with sigma of 0.005 O10-Li2 \\sim O10A-Li2 with sigma of 0.005 O11-Li2 \\sim O11A-Li2 with sigma of 0.005 O12-Li2 \\sim O12A-Li2 with sigma of 0.005 O9A-C77A \\sim O9-C77 \\sim O9-C84 \\sim O9A-C84A \\sim O12-C83 \\sim O12A-C83A \\sim O12-C82 \\sim O12A- C82A \\sim O11-C81 \\sim O11A-C81A \\sim O11-C80 \\sim O11A-C80A \\sim O10-C79 \\sim O10A-C79A \\sim O10A- C78A \\sim O10-C78 with sigma of 0.005 C80-C79 \\sim C80A-C79A \\sim C82A-C81A \\sim C82-C81 \\sim C84A-C83A \\sim C84-C83 \\sim C78A-C77A C78-C77 with sigma of 0.005 C95B-C94A \\sim C95A-C94 with sigma of 0.005 3. Uiso/Uaniso restraints and constraints O9 \\sim O10 \\sim O11 \\sim O12 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81 \\sim C82 \\sim C83 \\sim C84: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.01 O9A \\sim O10A \\sim O11A \\sim O12A \\sim C77A \\sim C78A \\sim C79A \\sim C80A \\sim C81A \\sim C82A \\sim C83A \\sim C84A: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.01 C94 \\sim C95A \\sim C94A \\sim C95B: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.01 Uanis(C81A) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C82A) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(O12A) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(C83A) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O11A) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C80A) \\sim Ueq, Uanis(C84A) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O10A) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C78A) \\sim Ueq, Uanis(C77A) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(O9A) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C79A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C90) \\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C62) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C74A) \\sim Ueq, Uanis(O8A) \\sim Ueq, Uanis(C76A) \\sim Ueq, Uanis(O5A) \\sim Ueq, Uanis(C75A) \\sim Ueq, Uanis(C69A) \\sim Ueq, Uanis(C70A) \\sim Ueq, Uanis(O6A) \\sim Ueq, Uanis(C71A) \\sim Ueq, Uanis(C72A) \\sim Ueq, Uanis(O7A) \\sim Ueq, Uanis(C73A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O6) = Uanis(O6A) 4. Others Fixed Sof: C7(0.5) C8(0.5) H8(0.5) C9(0.5) H9(0.5) C10(0.5) H10(0.5) C11(0.5) H11(0.5) C12(0.5) H12(0.5) C49(0.65) C50(0.65) H50(0.65) C51(0.65) H51(0.65) C52(0.65) H52(0.65) C53(0.65) H53(0.65) C54(0.65) H54(0.65) C7A(0.5) C12A(0.5) H12A(0.5) C11A(0.5) H11A(0.5) C10A(0.5) H10A(0.5) C9A(0.5) H9A(0.5) C8A(0.5) H8A(0.5) C49A(0.35) C50A(0.35) H50A(0.35) C51A(0.35) H51A(0.35) C52A(0.35) H52A(0.35) C53A(0.35) H53A(0.35) C54A(0.35) H54A(0.35) O5(0.6) O6(0.6) O7(0.6) O8(0.6) O5A(0.4) O6A(0.4) O7A(0.4) O8A(0.4) C69(0.6) H69A(0.6) H69B(0.6) C70(0.6) H70A(0.6) H70B(0.6) C71(0.6) H71A(0.6) H71B(0.6) C72(0.6) H72A(0.6) H72B(0.6) C73(0.6) H73A(0.6) H73B(0.6) C74(0.6) H74A(0.6) H74B(0.6) C75(0.6) H75A(0.6) H75B(0.6) C76(0.6) H76A(0.6) H76B(0.6) C69A(0.4) H69C(0.4) H69D(0.4) C70A(0.4) H70C(0.4) H70D(0.4) C71A(0.4) H71C(0.4) H71D(0.4) C72A(0.4) H72C(0.4) H72D(0.4) C73A(0.4) H73C(0.4) H73D(0.4) C74A(0.4) H74C(0.4) H74D(0.4) C75A(0.4) H75C(0.4) H75D(0.4) C76A(0.4) H76C(0.4) H76D(0.4) O9(0.65) O10(0.65) O11(0.65) O12(0.65) O9A(0.35) O10A(0.35) O11A(0.35) O12A(0.35) C77(0.65) H77A(0.65) H77B(0.65) C78(0.65) H78A(0.65) H78B(0.65) C79(0.65) H79A(0.65) H79B(0.65) C80(0.65) H80A(0.65) H80B(0.65) C81(0.65) H81A(0.65) H81B(0.65) C82(0.65) H82A(0.65) H82B(0.65) C83(0.65) H83A(0.65) H83B(0.65) C84(0.65) H84A(0.65) H84B(0.65) C77A(0.35) H77C(0.35) H77D(0.35) C78A(0.35) H78C(0.35) H78D(0.35) C79A(0.35) H79C(0.35) H79D(0.35) C80A(0.35) H80C(0.35) H80D(0.35) C81A(0.35) H81C(0.35) H81D(0.35) C82A(0.35) H82C(0.35) H82D(0.35) C83A(0.35) H83C(0.35) H83D(0.35) C84A(0.35) H84C(0.35) H84D(0.35) O20(0.5) C93(0.5) H93A(0.5) H93B(0.5) C95(0.5) H95A(0.25) H95B(0.25) H95C(0.25) H95D(0.25) C94(0.25) H94A(0.25) H94B(0.25) C95A(0.25) H95E(0.25) H95F(0.25) C94A(0.25) H94C(0.25) H94D(0.25) C95B(0.25) H95G(0.25) H95H(0.25) 5.a Secondary CH2 refined with riding coordinates: C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A, H65B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C69A(H69C,H69D), C70A(H70C,H70D), C71A(H71C, H71D), C72A(H72C,H72D), C73A(H73C,H73D), C74A(H74C,H74D), C75A(H75C,H75D), C76A(H76C,H76D), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B), C88(H88A, H88B), C89(H89A,H89B), C90(H90A,H90B), C91(H91A,H91B), C92(H92A,H92B), C77(H77A,H77B), C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B), C77A(H77C,H77D), C78A(H78C, H78D), C79A(H79C,H79D), C80A(H80C,H80D), C81A(H81C,H81D), C82A(H82C,H82D), C83A(H83C,H83D), C84A(H84C,H84D), C93(H93A,H93B), C95(H95A,H95B), C95(H95C, H95D), C94(H94A,H94B), C95A(H95E,H95F), C94A(H94C,H94D), C95B(H95G,H95H) 5.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C60(H60), C59(H59), C58(H58), C57(H57), C56(H56), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C12A(H12A), C11A(H11A), C10A(H10A), C9A(H9A), C8A(H8A), C50A(H50A), C51A(H51A), C52A(H52A), C53A(H53A), C54A(H54A) 5.c Fitted hexagon refined as free rotating group: C60(C59,C58,C57,C56,C55), C7A(C12A,C11A,C10A,C9A,C8A), C49A(C50A,C51A,C52A, C53A,C54A) ; _shelx_fab_file ; -19 -10 1 -1.1903 -0.2008 -19 -10 2 -0.2892 0.0197 -19 -9 1 -1.7730 -1.1203 -19 -9 2 -0.6180 -0.6960 -19 -9 3 -1.3318 -0.5644 -19 -8 1 0.1211 -0.5710 -19 -8 2 0.8092 -0.1879 -19 -8 3 0.1243 -0.1989 -19 -7 1 0.4862 0.9108 -19 -7 2 0.9029 0.8904 -19 -7 3 0.7202 0.4809 -19 -7 4 1.1936 0.2005 -19 -6 1 -1.1477 0.8848 -19 -6 2 -0.8503 0.6698 -19 -6 3 -0.6298 0.3216 -19 -6 4 -0.4112 0.1941 -19 -5 1 -0.8377 -0.2849 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19 9 4 -0.8518 0.1773 19 9 5 -0.1511 0.1124 19 9 6 -0.6736 0.0369 19 9 7 0.0315 -0.1173 19 9 8 0.0048 -0.2051 19 9 9 0.2853 -0.1062 19 9 10 0.4573 0.0044 19 9 11 -0.3505 0.0809 19 9 12 0.2986 0.0792 19 9 13 -0.4045 0.0265 19 9 14 1.1596 0.1120 19 9 15 0.2771 0.0987 19 9 16 1.6186 0.0981 19 9 17 0.4800 -0.0004 19 9 18 1.7357 -0.0831 19 9 19 0.7963 -0.0513 19 10 0 -0.0219 -0.0395 19 10 1 -0.2729 -0.0422 19 10 2 0.2927 -0.1672 19 10 3 0.5834 0.0042 19 10 4 0.1502 0.1537 19 10 5 0.8480 0.1935 19 10 6 -0.0504 0.0860 19 10 7 1.1107 -0.0055 19 10 8 0.2619 -0.0511 19 10 9 0.7738 0.0450 19 10 10 -0.1483 -0.0060 19 10 11 -0.2416 -0.0503 19 10 12 0.1564 -0.1122 19 10 13 0.0063 -0.0845 19 10 14 1.2926 0.0314 19 10 15 0.0868 0.0396 19 10 16 1.7029 0.0623 19 10 17 0.1227 0.0498 19 10 18 1.8323 0.0973 19 11 0 0.7083 -0.3019 19 11 1 0.4135 -0.2547 19 11 2 0.3835 -0.2718 19 11 3 0.3352 -0.0567 19 11 4 -0.4676 -0.0013 19 11 5 0.4096 -0.0092 19 11 6 -0.4794 -0.0621 19 11 7 1.0962 0.0309 19 11 8 -0.3118 0.0894 19 11 9 0.8054 0.1752 19 11 10 -0.5633 0.0237 19 11 11 0.5782 -0.0404 19 11 12 0.1880 -0.1131 19 11 13 0.4414 -0.0786 19 11 14 0.3872 -0.0643 19 11 15 -0.6497 -0.0874 19 11 16 0.3037 -0.0507 19 11 17 -1.1977 0.0178 19 12 1 0.3526 -0.0922 19 12 2 -0.2367 -0.0831 19 12 3 -0.1167 0.0184 19 12 4 -0.9704 -0.0435 19 12 5 0.0154 -0.0717 19 12 6 -1.0851 -0.0419 19 12 7 0.1001 0.1025 19 12 8 -1.6836 0.1179 19 12 9 -0.2587 0.1143 19 12 10 -1.5740 -0.0442 19 12 11 0.2591 -0.0319 19 12 12 -0.8110 -0.0580 19 12 13 0.0001 -0.0160 19 12 14 -0.7850 -0.0497 19 12 15 -0.7954 -0.0299 19 12 16 -0.5086 0.0215 19 13 5 0.3899 -0.0243 19 13 6 -0.7580 0.0461 19 13 7 -0.0221 0.0914 19 13 8 -1.3523 0.0052 19 13 9 0.0414 -0.0546 19 13 10 -0.8920 -0.1303 19 13 11 0.6097 -0.0397 19 13 12 -0.6771 -0.0318 19 13 13 0.3137 0.0216 20 5 6 0.2309 -0.1656 20 5 7 0.1673 -0.1548 20 5 8 0.4763 -0.0530 20 5 9 0.0243 0.0303 20 5 10 0.2835 0.1207 20 5 11 0.1525 0.0218 20 6 4 0.9464 0.0408 20 6 5 1.0945 -0.0262 20 6 6 0.9726 -0.1079 20 6 7 0.4035 -0.1020 20 6 8 0.1832 0.0026 20 6 9 -0.4284 0.0205 20 6 10 -0.5156 0.0486 20 6 11 -0.8321 -0.0481 20 6 12 -0.5853 -0.0190 20 7 4 -0.0228 0.1319 20 7 5 0.3500 0.1357 20 7 6 0.4099 0.1026 20 7 7 0.3064 0.1407 20 7 8 0.0125 0.1434 20 7 9 -0.1499 0.0402 20 7 10 -0.6913 -0.0416 20 7 11 -0.5744 -0.1072 20 7 12 -0.7799 -0.0505 20 7 13 -0.8209 0.0128 20 8 5 0.7188 0.0859 20 8 6 0.5729 0.1559 20 8 7 0.5780 0.2487 20 8 8 -0.0796 0.1751 20 8 9 0.2309 0.0399 20 8 10 -0.5634 -0.0594 20 8 11 0.3572 -0.0618 20 8 12 -0.4374 -0.0430 20 8 13 0.0861 -0.0032 20 9 6 -0.0859 -0.0069 20 9 7 -0.0705 0.0456 20 9 8 -0.5555 -0.0135 20 9 9 0.3450 -0.0223 20 9 10 -0.2078 0.0305 20 9 11 1.0376 0.1177 0 0 0 0.0 0.0 ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.78562(2) 0.18467(2) 0.84153(2) 0.02380(5) Uani 1 1 d . . . . . Sn2 Sn 0.89161(2) 0.08582(2) 0.74937(2) 0.02373(5) Uani 1 1 d D . . . . Sn3 Sn 0.79919(2) 0.16839(2) 0.66216(2) 0.02477(5) Uani 1 1 d . . . . . Sn4 Sn 0.72277(2) 0.43712(2) 0.71216(2) 0.02649(5) Uani 1 1 d . . . . . Sn5 Sn 0.81709(2) 0.35694(2) 0.79823(2) 0.02218(5) Uani 1 1 d . . . . . Sn6 Sn 0.61254(2) 0.24847(2) 0.79301(2) 0.02545(5) Uani 1 1 d D . . . . Sn7 Sn 0.61992(2) 0.32329(2) 0.68632(2) 0.02963(6) Uani 1 1 d . . . . . C1 C 1.0550(3) 0.0576(3) 0.73218(15) 0.0316(8) Uani 1 1 d . . . . . C2 C 1.1112(4) 0.0081(5) 0.7692(2) 0.0650(17) Uani 1 1 d . . . . . H2 H 1.0776 -0.0105 0.8026 0.078 Uiso 1 1 calc R . . . . C3 C 1.2162(4) -0.0150(7) 0.7585(3) 0.102(3) Uani 1 1 d . . . . . H3 H 1.2533 -0.0497 0.7844 0.122 Uiso 1 1 calc R . . . . C4 C 1.2661(4) 0.0118(6) 0.7113(3) 0.082(2) Uani 1 1 d . . . . . H4 H 1.3378 -0.0052 0.7040 0.098 Uiso 1 1 calc R . . . . C5 C 1.2125(4) 0.0631(4) 0.6747(2) 0.0543(13) Uani 1 1 d . . . . . H5 H 1.2467 0.0837 0.6421 0.065 Uiso 1 1 calc R . . . . C6 C 1.1087(3) 0.0850(3) 0.68491(18) 0.0398(9) Uani 1 1 d . . . . . H6 H 1.0727 0.1200 0.6587 0.048 Uiso 1 1 calc R . . . . C13 C 0.7497(3) 0.0573(3) 0.64279(14) 0.0284(7) Uani 1 1 d . . . . . C14 C 0.8164(3) -0.0302(3) 0.62752(19) 0.0411(10) Uani 1 1 d . . . . . H14 H 0.8871 -0.0406 0.6221 0.049 Uiso 1 1 calc R . . . . C15 C 0.7828(4) -0.1027(3) 0.61997(18) 0.0432(10) Uani 1 1 d . . . . . H15 H 0.8302 -0.1618 0.6096 0.052 Uiso 1 1 calc R . . . . C16 C 0.6807(4) -0.0891(3) 0.62742(18) 0.0448(11) Uani 1 1 d . . . . . H16 H 0.6574 -0.1383 0.6219 0.054 Uiso 1 1 calc R . . . . C17 C 0.6129(4) -0.0032(4) 0.6430(2) 0.0509(12) Uani 1 1 d . . . . . H17 H 0.5423 0.0065 0.6489 0.061 Uiso 1 1 calc R . . . . C18 C 0.6468(3) 0.0692(3) 0.65020(17) 0.0363(9) Uani 1 1 d . . . . . H18 H 0.5989 0.1282 0.6604 0.044 Uiso 1 1 calc R . . . . C19 C 0.9185(3) 0.1812(3) 0.59497(14) 0.0280(7) Uani 1 1 d . . . . . C20 C 0.9586(3) 0.2540(3) 0.59319(16) 0.0350(8) Uani 1 1 d . . . . . H20 H 0.9302 0.2986 0.6197 0.042 Uiso 1 1 calc R . . . . C21 C 1.0390(3) 0.2631(3) 0.55379(17) 0.0408(9) Uani 1 1 d . . . . . H21 H 1.0655 0.3129 0.5539 0.049 Uiso 1 1 calc R . . . . C22 C 1.0805(3) 0.1999(3) 0.51446(17) 0.0407(9) Uani 1 1 d . . . . . H22 H 1.1352 0.2064 0.4873 0.049 Uiso 1 1 calc R . . . . C23 C 1.0420(3) 0.1274(3) 0.51496(16) 0.0361(9) Uani 1 1 d . . . . . H23 H 1.0703 0.0838 0.4880 0.043 Uiso 1 1 calc R . . . . C24 C 0.9619(3) 0.1179(3) 0.55482(15) 0.0311(8) Uani 1 1 d . . . . . H24 H 0.9363 0.0676 0.5547 0.037 Uiso 1 1 calc R . . . . C25 C 0.8245(3) 0.4825(3) 0.64729(16) 0.0337(8) Uani 1 1 d . . . . . C26 C 0.7891(4) 0.5204(3) 0.60094(17) 0.0446(10) Uani 1 1 d . . . . . H26 H 0.7232 0.5226 0.5985 0.054 Uiso 1 1 calc R . . . . C27 C 0.8476(4) 0.5547(4) 0.55864(18) 0.0508(12) Uani 1 1 d . . . . . H27 H 0.8213 0.5817 0.5280 0.061 Uiso 1 1 calc R . . . . C28 C 0.9448(4) 0.5496(4) 0.56110(19) 0.0514(12) Uani 1 1 d . . . . . H28 H 0.9851 0.5736 0.5323 0.062 Uiso 1 1 calc R . . . . C29 C 0.9829(4) 0.5095(4) 0.6057(2) 0.0520(12) Uani 1 1 d . . . . . H29 H 1.0502 0.5041 0.6071 0.062 Uiso 1 1 calc R . . . . C30 C 0.9221(4) 0.4771(3) 0.64841(19) 0.0455(11) Uani 1 1 d . . . . . H30 H 0.9485 0.4506 0.6791 0.055 Uiso 1 1 calc R . . . . C31 C 0.6233(3) 0.5753(3) 0.73794(16) 0.0307(8) Uani 1 1 d . . . . . C32 C 0.5394(3) 0.5834(3) 0.77896(18) 0.0378(9) Uani 1 1 d . . . . . H32 H 0.5196 0.5293 0.7917 0.045 Uiso 1 1 calc R . . . . C33 C 0.4842(4) 0.6680(3) 0.8015(2) 0.0490(11) Uani 1 1 d . . . . . H33 H 0.4276 0.6714 0.8295 0.059 Uiso 1 1 calc R . . . . C34 C 0.5113(4) 0.7477(3) 0.7835(2) 0.0483(12) Uani 1 1 d . . . . . H34 H 0.4744 0.8056 0.7996 0.058 Uiso 1 1 calc R . . . . C35 C 0.5924(4) 0.7430(3) 0.7419(2) 0.0450(11) Uani 1 1 d . . . . . H35 H 0.6101 0.7981 0.7287 0.054 Uiso 1 1 calc R . . . . C36 C 0.6478(3) 0.6579(3) 0.71949(17) 0.0358(9) Uani 1 1 d . . . . . H36 H 0.7036 0.6552 0.6911 0.043 Uiso 1 1 calc R . . . . C37 C 0.9701(3) 0.3649(3) 0.78416(15) 0.0304(8) Uani 1 1 d . . . . . C38 C 0.9880(4) 0.4470(3) 0.79218(19) 0.0417(10) Uani 1 1 d . . . . . H38 H 0.9323 0.5014 0.8024 0.050 Uiso 1 1 calc R . . . . C39 C 1.0857(4) 0.4506(4) 0.7856(2) 0.0590(14) Uani 1 1 d . . . . . H39 H 1.0961 0.5074 0.7908 0.071 Uiso 1 1 calc R . . . . C40 C 1.1667(4) 0.3728(5) 0.7715(2) 0.0636(16) Uani 1 1 d . . . . . H40 H 1.2336 0.3749 0.7672 0.076 Uiso 1 1 calc R . . . . C41 C 1.1506(4) 0.2913(4) 0.7635(3) 0.0663(16) Uani 1 1 d . . . . . H41 H 1.2068 0.2367 0.7541 0.080 Uiso 1 1 calc R . . . . C42 C 1.0532(3) 0.2881(3) 0.7692(2) 0.0455(11) Uani 1 1 d . . . . . H42 H 1.0437 0.2317 0.7625 0.055 Uiso 1 1 calc R . . . . C43 C 0.7471(3) 0.4518(3) 0.86270(18) 0.0379(9) Uani 1 1 d . . . . . C44 C 0.7320(5) 0.4124(4) 0.9146(2) 0.0622(15) Uani 1 1 d . . . . . H44 H 0.7512 0.3459 0.9206 0.075 Uiso 1 1 calc R . . . . C45 C 0.6891(6) 0.4700(5) 0.9575(3) 0.087(2) Uani 1 1 d . . . . . H45 H 0.6820 0.4424 0.9924 0.105 Uiso 1 1 calc R . . . . C46 C 0.6580(6) 0.5642(5) 0.9495(3) 0.082(2) Uani 1 1 d . . . . . H46 H 0.6269 0.6026 0.9788 0.098 Uiso 1 1 calc R . . . . C47 C 0.6706(5) 0.6052(4) 0.8996(3) 0.0683(17) Uani 1 1 d . . . . . H47 H 0.6490 0.6719 0.8945 0.082 Uiso 1 1 calc R . . . . C48 C 0.7154(4) 0.5491(3) 0.8560(2) 0.0488(11) Uani 1 1 d . . . . . H48 H 0.7240 0.5782 0.8215 0.059 Uiso 1 1 calc R . . . . C60 C 0.51210(16) 0.39492(19) 0.88106(10) 0.0395(9) Uani 1 1 d . . . . . H60 H 0.5733 0.3638 0.8931 0.047 Uiso 1 1 calc R . . . . C59 C 0.4420(2) 0.4735(2) 0.90582(10) 0.0485(12) Uani 1 1 d G . . . . H59 H 0.4553 0.4961 0.9348 0.058 Uiso 1 1 calc R . . . . C58 C 0.35240(19) 0.51897(17) 0.88819(12) 0.0510(13) Uani 1 1 d G . . . . H58 H 0.3045 0.5727 0.9051 0.061 Uiso 1 1 calc R . . . . C57 C 0.33294(16) 0.48588(18) 0.84579(12) 0.0455(11) Uani 1 1 d G . . . . H57 H 0.2717 0.5170 0.8337 0.055 Uiso 1 1 calc R . . . . C56 C 0.40306(18) 0.40730(18) 0.82103(10) 0.0379(9) Uani 1 1 d G . . . . H56 H 0.3898 0.3847 0.7921 0.046 Uiso 1 1 calc R . . . . C55 C 0.49264(16) 0.36183(15) 0.83866(10) 0.0309(8) Uani 1 1 d G . . . . C7 C 0.8977(13) -0.0622(5) 0.7548(6) 0.028(3) Uani 0.5 1 d D . P A 1 C8 C 0.9839(8) -0.1362(7) 0.7592(4) 0.028(2) Uani 0.5 1 d . . P A 1 H8 H 1.0429 -0.1225 0.7612 0.034 Uiso 0.5 1 calc R . P A 1 C9 C 0.9888(8) -0.2304(7) 0.7609(4) 0.042(2) Uani 0.5 1 d . . P A 1 H9 H 1.0494 -0.2795 0.7647 0.050 Uiso 0.5 1 calc R . P A 1 C10 C 0.9043(9) -0.2505(7) 0.7569(4) 0.039(2) Uani 0.5 1 d . . P A 1 H10 H 0.9073 -0.3142 0.7564 0.046 Uiso 0.5 1 calc R . P A 1 C11 C 0.8143(9) -0.1788(9) 0.7536(4) 0.039(2) Uani 0.5 1 d . . P A 1 H11 H 0.7555 -0.1930 0.7518 0.047 Uiso 0.5 1 calc R . P A 1 C12 C 0.8122(8) -0.0868(7) 0.7529(4) 0.036(2) Uani 0.5 1 d . . P A 1 H12 H 0.7504 -0.0379 0.7511 0.043 Uiso 0.5 1 calc R . P A 1 C49 C 0.5353(4) 0.1424(4) 0.7965(3) 0.0272(13) Uani 0.65 1 d D . P B 1 C50 C 0.4553(4) 0.1613(4) 0.7712(3) 0.0305(12) Uani 0.65 1 d . . P B 1 H50 H 0.4318 0.2212 0.7536 0.037 Uiso 0.65 1 calc R . P B 1 C51 C 0.4096(5) 0.0949(4) 0.7713(3) 0.0398(15) Uani 0.65 1 d . . P B 1 H51 H 0.3532 0.1090 0.7549 0.048 Uiso 0.65 1 calc R . P B 1 C52 C 0.4467(6) 0.0070(5) 0.7957(4) 0.051(2) Uani 0.65 1 d . . P B 1 H52 H 0.4158 -0.0398 0.7960 0.062 Uiso 0.65 1 calc R . P B 1 C53 C 0.5267(7) -0.0125(6) 0.8191(5) 0.069(3) Uani 0.65 1 d . . P B 1 H53 H 0.5533 -0.0735 0.8348 0.083 Uiso 0.65 1 calc R . P B 1 C54 C 0.5704(6) 0.0568(5) 0.8201(4) 0.0495(19) Uani 0.65 1 d . . P B 1 H54 H 0.6253 0.0435 0.8376 0.059 Uiso 0.65 1 calc R . P B 1 C7A C 0.8792(7) -0.0567(4) 0.7590(5) 0.025(4) Uani 0.5 1 d D . P A 2 C12A C 0.7823(6) -0.0642(4) 0.7726(4) 0.051(4) Uani 0.5 1 d G . P A 2 H12A H 0.7257 -0.0101 0.7823 0.062 Uiso 0.5 1 calc R . P A 2 C11A C 0.7683(6) -0.1507(6) 0.7719(4) 0.051(3) Uani 0.5 1 d G . P A 2 H11A H 0.7021 -0.1558 0.7811 0.062 Uiso 0.5 1 calc R . P A 2 C10A C 0.8512(7) -0.2297(4) 0.7576(4) 0.045(3) Uani 0.5 1 d G . P A 2 H10A H 0.8416 -0.2888 0.7571 0.054 Uiso 0.5 1 calc R . P A 2 C9A C 0.9481(6) -0.2223(4) 0.7440(3) 0.047(3) Uani 0.5 1 d G . P A 2 H9A H 1.0047 -0.2763 0.7343 0.056 Uiso 0.5 1 calc R . P A 2 C8A C 0.9621(5) -0.1358(5) 0.7447(4) 0.033(2) Uani 0.5 1 d G . P A 2 H8A H 1.0283 -0.1307 0.7355 0.040 Uiso 0.5 1 calc R . P A 2 C49A C 0.5450(6) 0.1322(5) 0.8215(3) 0.029(3) Uani 0.35 1 d D . P B 2 C50A C 0.5102(7) 0.0962(6) 0.7859(2) 0.037(3) Uani 0.35 1 d G . P B 2 H50A H 0.5107 0.1238 0.7511 0.045 Uiso 0.35 1 calc R . P B 2 C51A C 0.4747(8) 0.0198(7) 0.8013(3) 0.055(5) Uani 0.35 1 d G . P B 2 H51A H 0.4509 -0.0047 0.7769 0.065 Uiso 0.35 1 calc R . P B 2 C52A C 0.4739(8) -0.0206(5) 0.8522(4) 0.051(4) Uani 0.35 1 d G . P B 2 H52A H 0.4496 -0.0727 0.8627 0.061 Uiso 0.35 1 calc R . P B 2 C53A C 0.5087(7) 0.0154(6) 0.8878(3) 0.046(3) Uani 0.35 1 d G . P B 2 H53A H 0.5081 -0.0122 0.9226 0.055 Uiso 0.35 1 calc R . P B 2 C54A C 0.5442(6) 0.0918(6) 0.8724(3) 0.039(3) Uani 0.35 1 d G . P B 2 H54A H 0.5680 0.1163 0.8967 0.047 Uiso 0.35 1 calc R . P B 2 O1 O 0.8287(3) 0.9304(3) 0.96116(16) 0.0616(10) Uani 1 1 d . . . . . O2 O 1.0282(4) 0.8308(3) 0.95224(18) 0.0763(12) Uani 1 1 d . . . . . O3 O 0.9890(7) 0.6742(4) 0.9283(3) 0.130(2) Uani 1 1 d . U . . . O4 O 0.7922(6) 0.7777(4) 0.93604(17) 0.108(2) Uani 1 1 d . . . . . O5 O 0.7322(4) 0.8354(5) 1.0503(2) 0.0630(17) Uani 0.6 1 d D U P C 1 O6 O 0.8871(9) 0.8793(11) 1.0676(5) 0.0603(12) Uani 0.6 1 d D U P C 1 O7 O 0.9941(5) 0.6957(4) 1.0476(2) 0.057(2) Uani 0.6 1 d D U P C 1 O8 O 0.8239(4) 0.6550(4) 1.0332(2) 0.0491(13) Uani 0.6 1 d D U P C 1 O5A O 0.7456(6) 0.7756(6) 1.0516(3) 0.047(2) Uani 0.4 1 d D U P C 2 O6A O 0.8788(15) 0.8845(17) 1.0671(8) 0.0603(12) Uani 0.4 1 d D U P C 2 O7A O 1.0265(7) 0.7167(6) 1.0315(5) 0.069(4) Uani 0.4 1 d D U P C 2 O8A O 0.9080(5) 0.6202(4) 1.0177(3) 0.0390(16) Uani 0.4 1 d D U P C 2 C61 C 0.9041(5) 0.9763(4) 0.9513(3) 0.0670(17) Uani 1 1 d . . . . . H61A H 0.9133 0.9916 0.9851 0.080 Uiso 1 1 calc R . . . . H61B H 0.8816 1.0359 0.9301 0.080 Uiso 1 1 calc R . . . . C62 C 1.0015(6) 0.9151(5) 0.9225(3) 0.089(2) Uani 1 1 d . U . . . H62A H 0.9943 0.9034 0.8874 0.106 Uiso 1 1 calc R . . . . H62B H 1.0543 0.9458 0.9176 0.106 Uiso 1 1 calc R . . . . C63 C 1.1053(7) 0.7578(7) 0.9220(4) 0.121(3) Uani 1 1 d . U . . . H63A H 1.1457 0.7129 0.9460 0.146 Uiso 1 1 calc R . . . . H63B H 1.1512 0.7860 0.8962 0.146 Uiso 1 1 calc R . . . . C64 C 1.0614(8) 0.7030(8) 0.8921(5) 0.130(4) Uani 1 1 d . U . . . H64A H 1.0308 0.7442 0.8637 0.156 Uiso 1 1 calc R . . . . H64B H 1.1158 0.6478 0.8761 0.156 Uiso 1 1 calc R . . . . C65 C 0.9179(9) 0.6592(6) 0.9004(3) 0.113(3) Uani 1 1 d . U . . . H65A H 0.9567 0.6296 0.8669 0.136 Uiso 1 1 calc R . . . . H65B H 0.8861 0.6142 0.9221 0.136 Uiso 1 1 calc R . . . . C66 C 0.8404(7) 0.7413(6) 0.8887(3) 0.098(2) Uani 1 1 d . U . . . H66A H 0.8692 0.7864 0.8650 0.117 Uiso 1 1 calc R . . . . H66B H 0.7934 0.7256 0.8716 0.117 Uiso 1 1 calc R . . . . C67 C 0.7210(8) 0.8733(7) 0.9308(4) 0.111(3) Uani 1 1 d . . . . . H67A H 0.6868 0.8773 0.9012 0.133 Uiso 1 1 calc R . . . . H67B H 0.6686 0.8870 0.9635 0.133 Uiso 1 1 calc R . . . . C68 C 0.7736(5) 0.9417(5) 0.9211(3) 0.0669(16) Uani 1 1 d . . . . . H68A H 0.8203 0.9329 0.8863 0.080 Uiso 1 1 calc R . . . . H68B H 0.7245 1.0060 0.9207 0.080 Uiso 1 1 calc R . . . . C69 C 0.7114(8) 0.9193(6) 1.0774(4) 0.073(3) Uani 0.6 1 d D U P C 1 H69A H 0.6464 0.9309 1.1031 0.087 Uiso 0.6 1 calc R . P C 1 H69B H 0.7061 0.9742 1.0518 0.087 Uiso 0.6 1 calc R . P C 1 C70 C 0.7921(8) 0.9073(9) 1.1043(5) 0.062(3) Uani 0.6 1 d D U P C 1 H70A H 0.7833 0.9671 1.1195 0.075 Uiso 0.6 1 calc R . P C 1 H70B H 0.7910 0.8586 1.1335 0.075 Uiso 0.6 1 calc R . P C 1 C71 C 0.9799(11) 0.8312(7) 1.0854(7) 0.057(4) Uani 0.6 1 d D U P C 1 H71A H 0.9805 0.8591 1.1176 0.069 Uiso 0.6 1 calc R . P C 1 H71B H 1.0382 0.8370 1.0578 0.069 Uiso 0.6 1 calc R . P C 1 C72 C 0.9866(7) 0.7336(5) 1.0966(3) 0.0455(18) Uani 0.6 1 d D U P C 1 H72A H 1.0469 0.6992 1.1118 0.055 Uiso 0.6 1 calc R . P C 1 H72B H 0.9257 0.7279 1.1221 0.055 Uiso 0.6 1 calc R . P C 1 C73 C 0.9833(6) 0.6033(5) 1.0546(4) 0.050(2) Uani 0.6 1 d D U P C 1 H73A H 1.0229 0.5661 1.0810 0.060 Uiso 0.6 1 calc R . P C 1 H73B H 1.0137 0.5721 1.0209 0.060 Uiso 0.6 1 calc R . P C 1 C74 C 0.8814(6) 0.5996(6) 1.0712(3) 0.053(2) Uani 0.6 1 d D U P C 1 H74A H 0.8815 0.5337 1.0731 0.064 Uiso 0.6 1 calc R . P C 1 H74B H 0.8511 0.6250 1.1065 0.064 Uiso 0.6 1 calc R . P C 1 C75 C 0.7170(6) 0.6935(7) 1.0526(5) 0.048(3) Uani 0.6 1 d D U P C 1 H75A H 0.6930 0.6432 1.0737 0.058 Uiso 0.6 1 calc R . P C 1 H75B H 0.6833 0.7118 1.0220 0.058 Uiso 0.6 1 calc R . P C 1 C76 C 0.6845(8) 0.7736(6) 1.0844(4) 0.067(3) Uani 0.6 1 d D U P C 1 H76A H 0.6099 0.8016 1.0920 0.081 Uiso 0.6 1 calc R . P C 1 H76B H 0.7089 0.7570 1.1179 0.081 Uiso 0.6 1 calc R . P C 1 C69A C 0.7391(11) 0.8075(10) 1.1022(4) 0.061(3) Uani 0.4 1 d D U P C 2 H69C H 0.7679 0.7520 1.1249 0.073 Uiso 0.4 1 calc R . P C 2 H69D H 0.6667 0.8350 1.1183 0.073 Uiso 0.4 1 calc R . P C 2 C70A C 0.7889(18) 0.8755(17) 1.1025(12) 0.100(9) Uani 0.4 1 d D U P C 2 H70C H 0.7367 0.9377 1.1001 0.119 Uiso 0.4 1 calc R . P C 2 H70D H 0.8037 0.8687 1.1382 0.119 Uiso 0.4 1 calc R . P C 2 C71A C 1.0459(10) 0.7726(9) 1.0660(5) 0.051(3) Uani 0.4 1 d D U P C 2 H71C H 1.0867 0.8108 1.0446 0.062 Uiso 0.4 1 calc R . P C 2 H71D H 1.0867 0.7299 1.0905 0.062 Uiso 0.4 1 calc R . P C 2 C72A C 0.9560(13) 0.8345(11) 1.0964(9) 0.047(5) Uani 0.4 1 d D U P C 2 H72C H 0.9275 0.7970 1.1260 0.056 Uiso 0.4 1 calc R . P C 2 H72D H 0.9751 0.8809 1.1119 0.056 Uiso 0.4 1 calc R . P C 2 C73A C 1.0322(14) 0.6285(9) 1.0613(6) 0.079(5) Uani 0.4 1 d D U P C 2 H73C H 0.9865 0.6399 1.0963 0.094 Uiso 0.4 1 calc R . P C 2 H73D H 1.1021 0.5965 1.0668 0.094 Uiso 0.4 1 calc R . P C 2 C74A C 1.0031(9) 0.5704(9) 1.0327(7) 0.064(4) Uani 0.4 1 d D U P C 2 H74C H 1.0558 0.5499 1.0008 0.077 Uiso 0.4 1 calc R . P C 2 H74D H 0.9976 0.5135 1.0550 0.077 Uiso 0.4 1 calc R . P C 2 C75A C 0.8232(8) 0.6076(9) 1.0561(6) 0.058(3) Uani 0.4 1 d D U P C 2 H75C H 0.8339 0.6077 1.0922 0.069 Uiso 0.4 1 calc R . P C 2 H75D H 0.8136 0.5472 1.0520 0.069 Uiso 0.4 1 calc R . P C 2 C76A C 0.7366(15) 0.6853(8) 1.0467(13) 0.078(7) Uani 0.4 1 d D U P C 2 H76C H 0.7265 0.6825 1.0108 0.094 Uiso 0.4 1 calc R . P C 2 H76D H 0.6759 0.6786 1.0720 0.094 Uiso 0.4 1 calc R . P C 2 Li1 Li 0.8847(7) 0.7853(6) 0.9980(3) 0.056(2) Uani 1 1 d D . . . . O13 O 0.1781(3) 0.6406(2) 0.57670(14) 0.0490(8) Uani 1 1 d . . . . . O14 O 0.3272(2) 0.6914(2) 0.50229(12) 0.0407(7) Uani 1 1 d . . . . . O15 O 0.2970(2) 0.8542(2) 0.54881(13) 0.0448(7) Uani 1 1 d . . . . . O16 O 0.1529(2) 0.8031(2) 0.62300(13) 0.0443(7) Uani 1 1 d . . . . . O9 O 0.3554(7) 0.7811(6) 0.6480(3) 0.052(2) Uani 0.65 1 d D U P D 1 O10 O 0.4833(4) 0.6861(9) 0.5645(4) 0.056(3) Uani 0.65 1 d D U P D 1 O11 O 0.3879(6) 0.5525(4) 0.5969(4) 0.069(3) Uani 0.65 1 d D U P D 1 O12 O 0.2616(7) 0.6469(6) 0.6849(2) 0.074(2) Uani 0.65 1 d D U P D 1 O9A O 0.3492(12) 0.7597(11) 0.6590(4) 0.057(4) Uani 0.35 1 d D U P D 2 O10A O 0.4802(6) 0.6987(15) 0.5632(7) 0.045(5) Uani 0.35 1 d D U P D 2 O11A O 0.4036(12) 0.5565(5) 0.5818(8) 0.068(5) Uani 0.35 1 d D U P D 2 O12A O 0.2668(10) 0.6083(7) 0.6727(4) 0.069(4) Uani 0.35 1 d D U P D 2 C85 C 0.1831(6) 0.6384(7) 0.5234(3) 0.100(3) Uani 1 1 d . . . . . H85A H 0.1698 0.5805 0.5178 0.119 Uiso 1 1 calc R . . . . H85B H 0.1274 0.6926 0.5133 0.119 Uiso 1 1 calc R . . . . C86 C 0.2711(5) 0.6405(6) 0.4896(3) 0.081(2) Uani 1 1 d . . . . . H86A H 0.2544 0.6660 0.4548 0.097 Uiso 1 1 calc R . . . . H86B H 0.3158 0.5747 0.4852 0.097 Uiso 1 1 calc R . . . . C87 C 0.3126(7) 0.7783(5) 0.4729(2) 0.089(3) Uani 1 1 d . . . . . H87A H 0.3587 0.7674 0.4381 0.107 Uiso 1 1 calc R . . . . H87B H 0.2425 0.8009 0.4669 0.107 Uiso 1 1 calc R . . . . C88 C 0.3279(6) 0.8476(4) 0.4948(2) 0.080(2) Uani 1 1 d . . . . . H88A H 0.2929 0.9085 0.4779 0.096 Uiso 1 1 calc R . . . . H88B H 0.4012 0.8395 0.4856 0.096 Uiso 1 1 calc R . . . . C89 C 0.2014(5) 0.9195(4) 0.5663(2) 0.0673(17) Uani 1 1 d . . . . . H89A H 0.2107 0.9805 0.5694 0.081 Uiso 1 1 calc R . . . . H89B H 0.1607 0.9289 0.5389 0.081 Uiso 1 1 calc R . . . . C90 C 0.1461(5) 0.8951(4) 0.6144(4) 0.090(2) Uani 1 1 d . U . . . H90A H 0.1691 0.9134 0.6432 0.108 Uiso 1 1 calc R . . . . H90B H 0.0740 0.9327 0.6166 0.108 Uiso 1 1 calc R . . . . C91 C 0.0702(4) 0.7821(4) 0.6162(3) 0.0676(17) Uani 1 1 d . . . . . H91A H 0.0425 0.8253 0.5876 0.081 Uiso 1 1 calc R . . . . H91B H 0.0179 0.7968 0.6489 0.081 Uiso 1 1 calc R . . . . C92 C 0.0834(5) 0.6903(5) 0.6044(4) 0.097(3) Uani 1 1 d . U . . . H92A H 0.0686 0.6541 0.6379 0.117 Uiso 1 1 calc R . . . . H92B H 0.0325 0.6934 0.5836 0.117 Uiso 1 1 calc R . . . . C77 C 0.4473(6) 0.8019(7) 0.6263(4) 0.064(3) Uani 0.65 1 d D U P D 1 H77A H 0.4739 0.8145 0.6554 0.076 Uiso 0.65 1 calc R . P D 1 H77B H 0.4322 0.8600 0.6032 0.076 Uiso 0.65 1 calc R . P D 1 C78 C 0.5245(8) 0.7277(7) 0.5964(4) 0.054(3) Uani 0.65 1 d D U P D 1 H78A H 0.5758 0.7536 0.5736 0.065 Uiso 0.65 1 calc R . P D 1 H78B H 0.5587 0.6786 0.6210 0.065 Uiso 0.65 1 calc R . P D 1 C79 C 0.5317(13) 0.5919(8) 0.5480(6) 0.078(5) Uani 0.65 1 d D U P D 1 H79A H 0.6052 0.5756 0.5463 0.094 Uiso 0.65 1 calc R . P D 1 H79B H 0.5219 0.5898 0.5119 0.094 Uiso 0.65 1 calc R . P D 1 C80 C 0.4959(7) 0.5215(8) 0.5815(7) 0.069(3) Uani 0.65 1 d D U P D 1 H80A H 0.5184 0.4629 0.5625 0.083 Uiso 0.65 1 calc R . P D 1 H80B H 0.5258 0.5072 0.6134 0.083 Uiso 0.65 1 calc R . P D 1 C81 C 0.3526(11) 0.5042(9) 0.6442(4) 0.087(4) Uani 0.65 1 d D U P D 1 H81A H 0.4036 0.4419 0.6480 0.105 Uiso 0.65 1 calc R . P D 1 H81B H 0.2895 0.4936 0.6412 0.105 Uiso 0.65 1 calc R . P D 1 C82 C 0.3332(11) 0.5551(7) 0.6907(5) 0.101(4) Uani 0.65 1 d D U P D 1 H82A H 0.3060 0.5203 0.7220 0.121 Uiso 0.65 1 calc R . P D 1 H82B H 0.3971 0.5611 0.6958 0.121 Uiso 0.65 1 calc R . P D 1 C83 C 0.2759(7) 0.7046(8) 0.7199(4) 0.066(3) Uani 0.65 1 d D U P D 1 H83A H 0.2862 0.6672 0.7533 0.079 Uiso 0.65 1 calc R . P D 1 H83B H 0.2129 0.7582 0.7281 0.079 Uiso 0.65 1 calc R . P D 1 C84 C 0.3594(8) 0.7417(9) 0.7008(4) 0.078(3) Uani 0.65 1 d D U P D 1 H84A H 0.3546 0.7909 0.7239 0.094 Uiso 0.65 1 calc R . P D 1 H84B H 0.4244 0.6908 0.7012 0.094 Uiso 0.65 1 calc R . P D 1 C77A C 0.4480(11) 0.7685(11) 0.6425(6) 0.047(4) Uani 0.35 1 d D U P D 2 H77C H 0.4750 0.7670 0.6743 0.057 Uiso 0.35 1 calc R . P D 2 H77D H 0.4417 0.8311 0.6240 0.057 Uiso 0.35 1 calc R . P D 2 C78A C 0.5213(12) 0.6981(11) 0.6084(6) 0.044(4) Uani 0.35 1 d D U P D 2 H78C H 0.5857 0.7126 0.5974 0.053 Uiso 0.35 1 calc R . P D 2 H78D H 0.5348 0.6353 0.6271 0.053 Uiso 0.35 1 calc R . P D 2 C79A C 0.5365(13) 0.6107(12) 0.5399(6) 0.029(3) Uani 0.35 1 d D U P D 2 H79C H 0.6102 0.6002 0.5331 0.035 Uiso 0.35 1 calc R . P D 2 H79D H 0.5166 0.6070 0.5065 0.035 Uiso 0.35 1 calc R . P D 2 C80A C 0.5078(13) 0.5443(15) 0.5801(10) 0.056(5) Uani 0.35 1 d D U P D 2 H80C H 0.5501 0.4792 0.5715 0.067 Uiso 0.35 1 calc R . P D 2 H80D H 0.5168 0.5566 0.6147 0.067 Uiso 0.35 1 calc R . P D 2 C81A C 0.3650(15) 0.4931(13) 0.6194(5) 0.063(4) Uani 0.35 1 d D U P D 2 H81C H 0.4136 0.4286 0.6160 0.076 Uiso 0.35 1 calc R . P D 2 H81D H 0.3004 0.4923 0.6123 0.076 Uiso 0.35 1 calc R . P D 2 C82A C 0.3486(13) 0.5218(10) 0.6724(6) 0.051(4) Uani 0.35 1 d D U P D 2 H82C H 0.3295 0.4747 0.6990 0.061 Uiso 0.35 1 calc R . P D 2 H82D H 0.4095 0.5319 0.6790 0.061 Uiso 0.35 1 calc R . P D 2 C83A C 0.2616(13) 0.6668(12) 0.7131(6) 0.056(4) Uani 0.35 1 d D U P D 2 H83C H 0.2548 0.6312 0.7475 0.067 Uiso 0.35 1 calc R . P D 2 H83D H 0.2001 0.7223 0.7142 0.067 Uiso 0.35 1 calc R . P D 2 C84A C 0.3485(14) 0.6989(13) 0.7058(7) 0.065(5) Uani 0.35 1 d D U P D 2 H84C H 0.3437 0.7333 0.7366 0.078 Uiso 0.35 1 calc R . P D 2 H84D H 0.4115 0.6445 0.7022 0.078 Uiso 0.35 1 calc R . P D 2 Li2 Li 0.3071(6) 0.7089(6) 0.5913(3) 0.0447(18) Uani 1 1 d D . . . . O20 O 0.2546(7) 0.3323(8) 0.5727(3) 0.077(3) Uani 0.5 1 d . . P . . C93 C 0.2328(7) 0.3174(9) 0.6280(4) 0.055(3) Uani 0.5 1 d . . P G . H93A H 0.1824 0.2836 0.6389 0.066 Uiso 0.5 1 calc R . P . . H93B H 0.2058 0.3782 0.6452 0.066 Uiso 0.5 1 calc R . P . . C95 C 0.3317(7) 0.2593(7) 0.6427(4) 0.052(2) Uani 0.5 1 d . . P . . H95A H 0.3654 0.2985 0.6543 0.062 Uiso 0.25 1 calc R . P E 1 H95B H 0.3235 0.2097 0.6704 0.062 Uiso 0.25 1 calc R . P E 1 H95C H 0.3458 0.2891 0.6704 0.062 Uiso 0.25 1 calc R . P F 2 H95D H 0.3300 0.1954 0.6561 0.062 Uiso 0.25 1 calc R . P F 2 C94 C 0.3833(17) 0.222(2) 0.5941(10) 0.064(6) Uani 0.25 1 d D U P G 1 H94A H 0.4062 0.1523 0.5987 0.077 Uiso 0.25 1 calc R . P G 1 H94B H 0.4441 0.2420 0.5819 0.077 Uiso 0.25 1 calc R . P G 1 C95A C 0.3224(13) 0.2501(16) 0.5542(7) 0.048(4) Uani 0.25 1 d D U P G 1 H95E H 0.3631 0.2601 0.5190 0.058 Uiso 0.25 1 calc R . P G 1 H95F H 0.2887 0.2035 0.5522 0.058 Uiso 0.25 1 calc R . P G 1 C94A C 0.4088(15) 0.255(2) 0.5948(9) 0.054(5) Uani 0.25 1 d D U P G 2 H94C H 0.4578 0.2861 0.5976 0.065 Uiso 0.25 1 calc R . P G 2 H94D H 0.4454 0.1891 0.5845 0.065 Uiso 0.25 1 calc R . P G 2 C95B C 0.343(2) 0.307(2) 0.5595(9) 0.081(7) Uani 0.25 1 d D U P G 2 H95G H 0.3625 0.3636 0.5460 0.098 Uiso 0.25 1 calc R . P G 2 H95H H 0.3590 0.2678 0.5289 0.098 Uiso 0.25 1 calc R . P G 2 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 Sn1 0.02534(11) 0.02597(11) 0.01898(11) -0.00081(8) -0.00277(8) -0.00801(9) Sn2 0.02107(10) 0.02536(11) 0.02267(11) -0.00473(9) -0.00741(8) -0.00142(8) Sn3 0.02325(11) 0.02676(11) 0.02260(12) -0.00723(9) -0.00906(9) -0.00064(9) Sn4 0.03037(12) 0.02400(11) 0.02563(12) -0.00006(9) -0.01310(9) -0.00482(9) Sn5 0.02435(11) 0.02513(11) 0.01985(11) -0.00160(8) -0.00847(8) -0.00863(9) Sn6 0.01842(10) 0.02672(11) 0.03141(13) -0.01019(9) -0.00156(9) -0.00661(9) Sn7 0.02694(12) 0.02917(12) 0.03208(13) -0.01089(10) -0.01701(10) 0.00275(9) C1 0.0250(17) 0.040(2) 0.0293(19) -0.0086(16) -0.0088(14) -0.0046(15) C2 0.034(2) 0.114(5) 0.045(3) 0.021(3) -0.021(2) -0.022(3) C3 0.037(3) 0.177(9) 0.083(5) 0.039(5) -0.035(3) -0.026(4) C4 0.027(2) 0.132(6) 0.082(5) 0.000(4) -0.014(3) -0.020(3) C5 0.035(2) 0.078(4) 0.051(3) -0.020(3) 0.005(2) -0.023(2) C6 0.033(2) 0.051(3) 0.036(2) -0.0112(19) -0.0041(17) -0.0124(18) C13 0.0296(17) 0.0342(19) 0.0208(17) -0.0056(14) -0.0056(13) -0.0077(15) C14 0.0313(19) 0.037(2) 0.053(3) -0.0162(19) -0.0065(18) -0.0057(17) C15 0.051(3) 0.039(2) 0.041(2) -0.0169(19) 0.002(2) -0.016(2) C16 0.060(3) 0.052(3) 0.034(2) -0.0049(19) -0.006(2) -0.034(2) C17 0.040(2) 0.060(3) 0.059(3) -0.002(2) -0.006(2) -0.027(2) C18 0.0322(19) 0.042(2) 0.034(2) -0.0034(17) -0.0030(16) -0.0131(17) C19 0.0280(17) 0.0317(18) 0.0229(17) -0.0035(14) -0.0106(14) -0.0033(14) C20 0.042(2) 0.037(2) 0.0274(19) -0.0061(16) -0.0102(16) -0.0108(17) C21 0.045(2) 0.049(2) 0.032(2) 0.0000(18) -0.0093(18) -0.018(2) C22 0.036(2) 0.051(3) 0.029(2) 0.0017(18) -0.0057(16) -0.0084(19) C23 0.0321(19) 0.037(2) 0.028(2) -0.0037(16) -0.0081(15) 0.0050(16) C24 0.0299(18) 0.0302(18) 0.0287(19) -0.0044(14) -0.0117(15) 0.0009(14) C25 0.040(2) 0.0332(19) 0.0270(19) 0.0007(15) -0.0098(16) -0.0095(16) C26 0.048(2) 0.055(3) 0.030(2) 0.0025(19) -0.0155(19) -0.011(2) C27 0.062(3) 0.064(3) 0.028(2) 0.009(2) -0.016(2) -0.022(3) C28 0.068(3) 0.056(3) 0.031(2) 0.007(2) -0.005(2) -0.028(3) C29 0.053(3) 0.062(3) 0.049(3) 0.012(2) -0.015(2) -0.031(3) C30 0.052(3) 0.054(3) 0.039(2) 0.014(2) -0.019(2) -0.027(2) C31 0.0330(18) 0.0240(16) 0.040(2) -0.0013(15) -0.0219(16) -0.0062(14) C32 0.035(2) 0.0261(18) 0.051(3) -0.0073(17) -0.0090(18) -0.0062(16) C33 0.039(2) 0.034(2) 0.068(3) -0.014(2) -0.007(2) -0.0026(18) C34 0.059(3) 0.0233(19) 0.067(3) -0.012(2) -0.030(3) -0.0053(19) C35 0.064(3) 0.0252(19) 0.060(3) 0.0065(19) -0.040(3) -0.0176(19) C36 0.044(2) 0.0303(19) 0.039(2) 0.0052(16) -0.0215(18) -0.0138(17) C37 0.0289(17) 0.038(2) 0.0277(19) 0.0054(15) -0.0119(14) -0.0141(15) C38 0.044(2) 0.043(2) 0.049(3) 0.0030(19) -0.017(2) -0.024(2) C39 0.056(3) 0.074(4) 0.068(4) 0.008(3) -0.024(3) -0.044(3) C40 0.038(3) 0.092(4) 0.069(4) 0.010(3) -0.016(2) -0.034(3) C41 0.032(2) 0.068(4) 0.086(4) 0.002(3) -0.003(3) -0.007(2) C42 0.034(2) 0.041(2) 0.058(3) 0.000(2) -0.005(2) -0.0103(18) C43 0.0335(19) 0.041(2) 0.043(2) -0.0185(18) -0.0096(17) -0.0098(17) C44 0.090(4) 0.059(3) 0.034(3) -0.017(2) 0.003(3) -0.024(3) C45 0.127(6) 0.077(5) 0.044(3) -0.032(3) 0.015(4) -0.025(4) C46 0.105(5) 0.080(5) 0.058(4) -0.042(4) 0.005(4) -0.027(4) C47 0.068(4) 0.047(3) 0.094(5) -0.035(3) -0.013(3) -0.015(3) C48 0.052(3) 0.044(2) 0.057(3) -0.021(2) -0.017(2) -0.015(2) C60 0.0320(19) 0.044(2) 0.041(2) -0.0172(18) 0.0098(17) -0.0162(18) C59 0.046(3) 0.050(3) 0.049(3) -0.026(2) 0.013(2) -0.021(2) C58 0.042(2) 0.038(2) 0.061(3) -0.026(2) 0.020(2) -0.0101(19) C57 0.033(2) 0.035(2) 0.060(3) -0.012(2) 0.008(2) -0.0069(17) C56 0.0286(18) 0.033(2) 0.049(3) -0.0129(18) 0.0042(17) -0.0094(16) C55 0.0237(16) 0.0273(17) 0.040(2) -0.0123(15) 0.0070(14) -0.0107(14) C7 0.025(4) 0.042(7) 0.017(5) -0.009(4) -0.002(4) -0.011(4) C8 0.030(4) 0.027(4) 0.024(5) 0.000(3) -0.005(4) -0.004(3) C9 0.045(6) 0.032(4) 0.039(6) -0.004(4) 0.004(4) -0.009(4) C10 0.053(6) 0.032(5) 0.025(4) -0.002(4) 0.004(5) -0.013(5) C11 0.048(7) 0.048(7) 0.033(5) 0.011(5) -0.019(5) -0.028(6) C12 0.029(5) 0.035(5) 0.043(6) 0.012(4) -0.020(4) -0.008(4) C49 0.024(3) 0.028(3) 0.032(3) -0.014(3) -0.007(3) -0.006(2) C50 0.023(2) 0.026(3) 0.042(3) -0.006(2) -0.010(2) -0.002(2) C51 0.032(3) 0.031(3) 0.062(4) -0.009(3) -0.020(3) -0.007(2) C52 0.039(4) 0.023(3) 0.101(7) 0.002(4) -0.023(4) -0.018(3) C53 0.058(5) 0.035(4) 0.129(10) 0.019(5) -0.052(6) -0.021(4) C54 0.045(4) 0.034(4) 0.081(6) 0.011(3) -0.038(4) -0.016(3) C7A 0.025(6) 0.024(5) 0.024(7) 0.000(4) -0.012(5) -0.002(3) C12A 0.033(6) 0.038(6) 0.090(11) -0.022(6) -0.027(6) -0.005(4) C11A 0.045(6) 0.052(7) 0.063(8) -0.012(6) -0.021(5) -0.013(5) C10A 0.064(9) 0.037(7) 0.041(6) -0.007(6) -0.014(7) -0.020(7) C9A 0.059(8) 0.033(5) 0.036(6) 0.000(4) 0.002(5) -0.008(5) C8A 0.037(6) 0.036(5) 0.024(5) -0.002(4) -0.007(4) -0.006(4) C49A 0.012(4) 0.044(7) 0.038(7) -0.027(6) 0.001(5) -0.011(4) C50A 0.041(6) 0.050(7) 0.030(6) -0.009(5) -0.007(5) -0.023(6) C51A 0.060(12) 0.052(10) 0.071(11) -0.020(8) -0.001(9) -0.046(9) C52A 0.051(8) 0.041(7) 0.063(10) -0.009(6) 0.004(7) -0.027(6) C53A 0.048(7) 0.041(7) 0.054(8) 0.017(6) -0.018(6) -0.024(6) C54A 0.043(6) 0.049(7) 0.035(6) 0.011(5) -0.017(5) -0.028(6) O1 0.079(3) 0.060(2) 0.061(2) 0.0136(18) -0.030(2) -0.038(2) O2 0.086(3) 0.060(3) 0.067(3) 0.003(2) -0.017(2) -0.005(2) O3 0.200(7) 0.075(3) 0.118(5) 0.001(3) -0.075(5) -0.020(4) O4 0.225(7) 0.113(4) 0.041(2) 0.027(3) -0.051(3) -0.121(5) O5 0.079(4) 0.080(4) 0.046(3) 0.012(3) -0.024(3) -0.044(4) O6 0.063(3) 0.067(3) 0.047(2) 0.0032(19) -0.0232(19) -0.010(2) O7 0.101(5) 0.032(3) 0.034(3) 0.014(2) -0.030(3) -0.010(3) O8 0.062(4) 0.057(3) 0.031(3) 0.006(3) -0.012(2) -0.022(3) O5A 0.067(5) 0.036(4) 0.040(4) 0.013(3) -0.019(4) -0.019(4) O6A 0.063(3) 0.067(3) 0.047(2) 0.0032(19) -0.0232(19) -0.010(2) O7A 0.110(8) 0.049(5) 0.062(7) -0.010(5) -0.042(6) -0.023(5) O8A 0.045(4) 0.034(3) 0.039(4) 0.005(3) -0.007(3) -0.017(3) C61 0.091(4) 0.044(3) 0.082(4) 0.024(3) -0.039(4) -0.036(3) C62 0.082(4) 0.085(4) 0.091(5) 0.033(4) 0.000(4) -0.043(4) C63 0.092(5) 0.140(7) 0.116(6) -0.053(5) -0.051(5) 0.020(5) C64 0.117(6) 0.135(7) 0.122(7) -0.035(6) -0.059(6) 0.014(5) C65 0.204(8) 0.075(4) 0.082(5) -0.005(4) -0.082(5) -0.034(5) C66 0.143(6) 0.106(5) 0.070(4) -0.002(4) -0.042(4) -0.060(5) C67 0.147(8) 0.146(8) 0.092(6) 0.046(6) -0.066(6) -0.106(7) C68 0.068(4) 0.076(4) 0.065(4) 0.002(3) -0.029(3) -0.027(3) C69 0.077(6) 0.075(6) 0.063(6) -0.017(5) -0.025(5) -0.008(5) C70 0.067(6) 0.044(5) 0.053(5) -0.009(4) 0.000(4) 0.005(4) C71 0.069(7) 0.056(6) 0.056(7) -0.003(5) -0.028(5) -0.021(5) C72 0.061(4) 0.048(4) 0.033(4) 0.008(3) -0.027(3) -0.017(3) C73 0.057(5) 0.045(4) 0.044(5) 0.011(4) -0.014(4) -0.013(4) C74 0.075(5) 0.042(4) 0.047(4) 0.010(3) -0.019(4) -0.024(4) C75 0.057(6) 0.054(5) 0.032(4) 0.005(4) -0.009(4) -0.019(4) C76 0.065(5) 0.079(6) 0.052(5) -0.002(4) 0.003(4) -0.025(5) C69A 0.062(7) 0.065(7) 0.050(6) -0.015(5) -0.004(5) -0.014(6) C70A 0.094(11) 0.109(13) 0.093(12) -0.012(9) 0.008(8) -0.043(9) C71A 0.061(6) 0.053(6) 0.052(6) -0.010(5) -0.017(5) -0.027(5) C72A 0.051(7) 0.045(7) 0.054(9) -0.015(5) -0.028(6) -0.011(5) C73A 0.072(7) 0.077(8) 0.100(9) 0.024(7) -0.050(7) -0.029(7) C74A 0.066(7) 0.052(7) 0.069(8) -0.004(6) -0.019(6) -0.010(6) C75A 0.064(7) 0.046(6) 0.062(7) 0.012(5) 0.005(6) -0.032(5) C76A 0.064(9) 0.085(11) 0.091(11) 0.003(8) -0.004(7) -0.040(8) Li1 0.086(7) 0.047(5) 0.048(5) 0.013(4) -0.029(5) -0.033(5) O13 0.0465(18) 0.0389(17) 0.050(2) 0.0030(14) -0.0130(15) 0.0019(14) O14 0.0373(15) 0.0470(17) 0.0380(16) -0.0010(13) -0.0180(13) -0.0073(13) O15 0.0432(17) 0.0481(18) 0.0448(18) 0.0012(14) -0.0214(14) -0.0098(14) O16 0.0351(15) 0.0461(18) 0.0473(19) -0.0095(14) -0.0151(14) -0.0002(13) O9 0.049(4) 0.074(5) 0.029(3) -0.004(3) -0.019(3) -0.005(3) O10 0.046(4) 0.061(5) 0.056(5) -0.026(4) -0.034(4) 0.015(3) O11 0.053(4) 0.065(4) 0.083(6) 0.038(3) -0.041(4) -0.007(3) O12 0.087(5) 0.083(5) 0.055(4) 0.007(4) -0.036(4) -0.019(4) O9A 0.042(6) 0.079(7) 0.033(6) 0.010(5) -0.017(5) 0.004(5) O10A 0.040(7) 0.042(6) 0.049(7) -0.010(5) -0.019(6) -0.001(5) O11A 0.057(7) 0.068(7) 0.066(7) 0.038(5) -0.013(5) -0.017(5) O12A 0.057(6) 0.069(7) 0.057(6) -0.006(5) -0.016(5) 0.014(5) C85 0.117(6) 0.154(8) 0.065(4) -0.040(5) 0.002(4) -0.094(6) C86 0.086(5) 0.121(6) 0.059(4) -0.040(4) 0.007(3) -0.064(4) C87 0.178(8) 0.073(4) 0.038(3) 0.015(3) -0.043(4) -0.061(5) C88 0.118(6) 0.057(4) 0.052(4) -0.004(3) 0.022(4) -0.036(4) C89 0.091(4) 0.037(3) 0.047(3) 0.003(2) -0.011(3) 0.009(3) C90 0.063(4) 0.049(3) 0.140(6) -0.023(4) 0.025(4) -0.016(3) C91 0.034(2) 0.052(3) 0.111(5) -0.023(3) 0.003(3) -0.010(2) C92 0.051(3) 0.098(5) 0.144(6) -0.064(5) 0.003(4) -0.019(3) C77 0.056(4) 0.073(6) 0.066(5) -0.018(4) -0.037(4) -0.005(4) C78 0.059(5) 0.069(5) 0.043(5) -0.007(4) -0.011(4) -0.029(4) C79 0.062(6) 0.071(7) 0.088(8) -0.010(6) -0.020(6) 0.001(5) C80 0.072(6) 0.048(5) 0.070(6) 0.012(5) -0.017(5) 0.000(4) C81 0.078(6) 0.074(6) 0.096(7) 0.022(6) -0.020(6) -0.013(5) C82 0.102(7) 0.097(7) 0.083(7) 0.020(6) -0.024(6) -0.009(6) C83 0.043(4) 0.096(6) 0.050(5) -0.012(5) -0.017(4) -0.004(4) C84 0.070(5) 0.099(7) 0.061(5) -0.011(5) -0.025(4) -0.011(5) C77A 0.041(6) 0.053(7) 0.043(6) -0.010(5) -0.007(5) -0.007(5) C78A 0.034(6) 0.047(6) 0.042(7) -0.001(5) -0.021(5) 0.007(5) C79A 0.025(5) 0.040(6) 0.020(5) 0.002(4) -0.015(4) -0.003(4) C80A 0.038(6) 0.055(8) 0.046(7) 0.025(6) -0.001(5) 0.008(5) C81A 0.053(7) 0.066(7) 0.051(7) 0.023(6) -0.011(6) -0.002(6) C82A 0.056(6) 0.040(6) 0.044(7) 0.004(5) -0.018(6) 0.003(5) C83A 0.054(7) 0.056(7) 0.041(7) 0.009(6) -0.011(6) 0.000(6) C84A 0.061(7) 0.071(8) 0.048(7) 0.003(6) -0.017(6) 0.002(6) Li2 0.037(4) 0.054(5) 0.036(4) 0.000(3) -0.014(3) -0.002(3) O20 0.063(5) 0.120(8) 0.049(5) 0.007(5) -0.008(4) -0.036(5) C93 0.036(5) 0.077(7) 0.049(6) -0.001(5) -0.006(4) -0.018(5) C95 0.041(5) 0.048(5) 0.062(7) 0.015(5) -0.011(4) -0.016(4) C94 0.032(9) 0.082(13) 0.059(9) 0.009(10) 0.006(8) -0.008(8) C95A 0.033(7) 0.063(11) 0.037(8) 0.012(8) 0.008(6) -0.015(7) C94A 0.022(8) 0.084(13) 0.041(8) 0.002(9) 0.006(7) -0.006(7) C95B 0.063(10) 0.101(14) 0.044(9) 0.012(10) 0.013(9) -0.001(10) 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 0.0016 '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 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle Sn2 Sn1 Sn5 94.370(11) Sn2 Sn1 Sn6 86.753(10) Sn5 Sn1 Sn6 84.670(10) Sn1 Sn2 Sn3 111.103(11) C1 Sn2 Sn1 115.26(10) C1 Sn2 Sn3 113.65(11) C1 Sn2 C7 95.8(5) C1 Sn2 C7A 102.2(3) C7 Sn2 Sn1 114.8(5) C7 Sn2 Sn3 105.0(4) C7A Sn2 Sn1 110.0(3) C7A Sn2 Sn3 103.5(3) Sn2 Sn3 Sn7 114.521(11) C13 Sn3 Sn2 102.94(10) C13 Sn3 Sn7 105.20(10) C13 Sn3 C19 104.66(14) C19 Sn3 Sn2 107.84(9) C19 Sn3 Sn7 119.80(10) Sn5 Sn4 Sn7 111.833(11) C25 Sn4 Sn5 111.71(11) C25 Sn4 Sn7 116.06(11) C25 Sn4 C31 98.57(15) C31 Sn4 Sn5 103.61(10) C31 Sn4 Sn7 113.71(9) Sn4 Sn5 Sn1 114.199(10) C37 Sn5 Sn1 117.97(10) C37 Sn5 Sn4 111.68(10) C37 Sn5 C43 98.85(15) C43 Sn5 Sn1 104.07(12) C43 Sn5 Sn4 108.05(12) Sn7 Sn6 Sn1 123.185(11) C55 Sn6 Sn1 109.38(7) C55 Sn6 Sn7 103.33(7) C55 Sn6 C49 101.92(18) C55 Sn6 C49A 97.7(2) C49 Sn6 Sn1 114.22(17) C49 Sn6 Sn7 102.34(18) C49A Sn6 Sn1 100.3(2) C49A Sn6 Sn7 119.96(19) Sn3 Sn7 Sn6 85.410(10) Sn4 Sn7 Sn3 93.519(11) Sn4 Sn7 Sn6 85.685(10) C2 C1 Sn2 119.7(3) C2 C1 C6 116.4(4) C6 C1 Sn2 123.9(3) C1 C2 C3 121.1(5) C4 C3 C2 120.7(6) C3 C4 C5 119.5(5) C4 C5 C6 119.9(5) C5 C6 C1 122.4(5) C14 C13 Sn3 122.8(3) C14 C13 C18 116.8(4) C18 C13 Sn3 120.1(3) C15 C14 C13 121.9(4) C16 C15 C14 120.1(4) C15 C16 C17 119.2(4) C16 C17 C18 120.5(4) C17 C18 C13 121.5(4) C20 C19 Sn3 118.3(3) C20 C19 C24 117.1(4) C24 C19 Sn3 124.5(3) C21 C20 C19 121.8(4) C22 C21 C20 120.1(4) C21 C22 C23 119.5(4) C22 C23 C24 120.3(4) C23 C24 C19 121.2(4) C26 C25 Sn4 118.0(3) C30 C25 Sn4 124.6(3) C30 C25 C26 117.4(4) C27 C26 C25 121.7(4) C26 C27 C28 119.7(4) C29 C28 C27 119.8(4) C28 C29 C30 119.7(5) C25 C30 C29 121.7(4) C32 C31 Sn4 120.6(3) C32 C31 C36 117.0(4) C36 C31 Sn4 121.9(3) C33 C32 C31 121.8(4) C34 C33 C32 120.0(5) C33 C34 C35 119.8(4) C36 C35 C34 119.9(4) C35 C36 C31 121.4(4) C38 C37 Sn5 121.4(3) C42 C37 Sn5 121.3(3) C42 C37 C38 117.2(4) C39 C38 C37 121.4(5) C40 C39 C38 120.1(5) C39 C40 C41 119.4(5) C40 C41 C42 120.5(5) C37 C42 C41 121.4(5) C44 C43 Sn5 118.4(3) C48 C43 Sn5 124.3(4) C48 C43 C44 117.3(4) C45 C44 C43 120.8(6) C46 C45 C44 120.3(7) C45 C46 C47 120.7(6) C46 C47 C48 120.2(6) C43 C48 C47 120.7(5) C59 C60 C55 120.0 C58 C59 C60 120.0 C59 C58 C57 120.0 C56 C57 C58 120.0 C57 C56 C55 120.0 C60 C55 Sn6 119.70(13) C56 C55 Sn6 119.83(13) C56 C55 C60 120.0 C8 C7 Sn2 123.2(10) C8 C7 C12 115.8(7) C12 C7 Sn2 121.0(9) C7 C8 C9 123.3(10) C10 C9 C8 118.6(10) C9 C10 C11 120.8(9) C12 C11 C10 118.8(9) C11 C12 C7 122.7(9) C50 C49 Sn6 120.3(4) C54 C49 Sn6 120.0(4) C54 C49 C50 119.5(5) C51 C50 C49 120.8(6) C50 C51 C52 119.0(6) C53 C52 C51 120.2(6) C52 C53 C54 120.1(7) C49 C54 C53 120.3(7) C12A C7A Sn2 117.1(5) C12A C7A C8A 120.0 C8A C7A Sn2 122.2(5) C7A C12A C11A 120.0 C10A C11A C12A 120.0 C9A C10A C11A 120.0 C10A C9A C8A 120.0 C9A C8A C7A 120.0 C50A C49A Sn6 118.6(4) C50A C49A C54A 120.0 C54A C49A Sn6 121.2(4) C49A C50A C51A 120.0 C52A C51A C50A 120.0 C53A C52A C51A 120.0 C52A C53A C54A 120.0 C53A C54A C49A 120.0 C61 O1 Li1 111.3(4) C68 O1 C61 116.5(4) C68 O1 Li1 117.1(4) C62 O2 C63 112.1(7) C62 O2 Li1 112.6(4) C63 O2 Li1 113.5(6) C64 O3 C65 108.9(8) C64 O3 Li1 116.1(6) C65 O3 Li1 106.4(7) C66 O4 C67 112.2(6) C66 O4 Li1 120.6(6) C67 O4 Li1 105.6(5) C69 O5 Li1 116.0(6) C76 O5 C69 108.6(7) C76 O5 Li1 123.5(6) C70 O6 C71 121.0(11) C70 O6 Li1 112.7(8) C71 O6 Li1 105.8(10) C72 O7 C73 112.7(7) C72 O7 Li1 115.1(5) C73 O7 Li1 107.5(5) C74 O8 Li1 109.7(5) C75 O8 C74 115.6(7) C75 O8 Li1 107.0(6) C69A O5A Li1 109.8(7) C76A O5A C69A 121.1(16) C76A O5A Li1 108.0(13) C70A O6A C72A 102(2) C70A O6A Li1 98.5(15) C72A O6A Li1 109.1(13) C71A O7A C73A 104.0(10) C71A O7A Li1 115.6(8) C73A O7A Li1 115.7(8) C74A O8A C75A 112.8(11) C74A O8A Li1 112.6(8) C75A O8A Li1 109.9(6) O1 C61 C62 110.6(5) O2 C62 C61 107.8(5) O2 C63 C64 112.8(8) O3 C64 C63 107.5(9) C66 C65 O3 115.2(7) O4 C66 C65 104.6(7) C68 C67 O4 110.4(7) O1 C68 C67 109.2(5) O5 C69 C70 108.9(8) O6 C70 C69 109.1(10) O6 C71 C72 108.0(14) O7 C72 C71 107.2(9) O7 C73 C74 116.2(7) O8 C74 C73 108.0(6) O8 C75 C76 116.4(8) O5 C76 C75 100.9(7) O5A C69A C70A 116.3(16) O6A C70A C69A 127(2) O7A C71A C72A 114.1(13) O6A C72A C71A 114.5(18) O7A C73A C74A 108.8(11) O8A C74A C73A 111.2(11) O8A C75A C76A 106.3(15) O5A C76A C75A 113.5(12) O1 Li1 O2 71.7(3) O1 Li1 O3 109.7(4) O1 Li1 O4 72.6(3) O1 Li1 O6 79.8(5) O1 Li1 O7 143.0(5) O1 Li1 O8 139.3(5) O1 Li1 O6A 77.9(7) O1 Li1 O7A 129.2(5) O1 Li1 O8A 159.1(5) O2 Li1 O3 69.4(4) O2 Li1 O6 83.5(5) O2 Li1 O8 145.4(5) O2 Li1 O6A 84.9(6) O2 Li1 O8A 118.0(4) O4 Li1 O2 108.5(4) O4 Li1 O3 67.7(4) O4 Li1 O6 143.9(6) O4 Li1 O8 77.4(3) O4 Li1 O6A 141.1(7) O4 Li1 O8A 86.6(4) O5 Li1 O1 80.7(4) O5 Li1 O2 144.1(4) O5 Li1 O3 143.8(5) O5 Li1 O4 83.8(4) O5 Li1 O6 69.0(4) O5 Li1 O7 108.1(4) O5 Li1 O8 69.3(3) O6 Li1 O3 145.6(5) O7 Li1 O2 82.8(4) O7 Li1 O3 84.7(4) O7 Li1 O4 142.8(5) O7 Li1 O6 70.9(5) O7 Li1 O8 74.6(3) O8 Li1 O3 82.6(4) O8 Li1 O6 112.2(6) O5A Li1 O1 100.6(5) O5A Li1 O2 165.1(5) O5A Li1 O3 125.5(5) O5A Li1 O4 80.4(4) O5A Li1 O6A 80.9(6) O5A Li1 O7A 114.1(5) O5A Li1 O8A 73.6(4) O6A Li1 O3 148.2(6) O7A Li1 O2 65.3(4) O7A Li1 O3 79.6(4) O7A Li1 O4 146.2(5) O7A Li1 O6A 72.6(6) O7A Li1 O8A 70.1(4) O8A Li1 O3 61.9(3) O8A Li1 O6A 119.9(8) C85 O13 C92 114.1(6) C85 O13 Li2 110.3(4) C92 O13 Li2 109.1(4) C86 O14 C87 111.1(5) C86 O14 Li2 115.5(4) C87 O14 Li2 111.9(4) C88 O15 C89 115.8(5) C88 O15 Li2 111.5(4) C89 O15 Li2 110.3(4) C90 O16 C91 115.0(5) C90 O16 Li2 112.1(4) C91 O16 Li2 119.0(4) C77 O9 C84 108.1(7) C77 O9 Li2 113.6(6) C84 O9 Li2 119.8(7) C78 O10 Li2 115.3(6) C79 O10 C78 122.1(11) C79 O10 Li2 107.9(9) C80 O11 Li2 117.4(7) C81 O11 C80 112.6(9) C81 O11 Li2 115.0(7) C82 O12 Li2 107.5(7) C83 O12 C82 106.3(9) C83 O12 Li2 109.0(6) C77A O9A C84A 107.9(13) C77A O9A Li2 109.5(10) C84A O9A Li2 114.2(11) C78A O10A Li2 109.0(11) C79A O10A C78A 105.9(14) C79A O10A Li2 109.8(11) C80A O11A Li2 111.3(12) C81A O11A C80A 113.2(15) C81A O11A Li2 113.0(11) C82A O12A C83A 111.8(13) C82A O12A Li2 108.9(9) C83A O12A Li2 100.6(9) C86 C85 O13 117.8(6) C85 C86 O14 119.0(5) C88 C87 O14 116.1(5) C87 C88 O15 117.8(5) C90 C89 O15 115.8(5) O16 C90 C89 115.8(6) O16 C91 C92 118.6(5) O13 C92 C91 116.6(6) O9 C77 C78 113.9(9) O10 C78 C77 111.8(9) O10 C79 C80 114.9(13) O11 C80 C79 111.5(11) O11 C81 C82 112.9(11) O12 C82 C81 109.6(10) O12 C83 C84 115.9(9) O9 C84 C83 108.7(9) O9A C77A C78A 116.4(16) O10A C78A C77A 107.8(13) O10A C79A C80A 101.9(16) O11A C80A C79A 107.0(15) O11A C81A C82A 110.4(17) O12A C82A C81A 102.2(13) O12A C83A C84A 114.1(15) O9A C84A C83A 107.5(14) O13 Li2 O12 82.9(3) O13 Li2 O12A 72.5(4) O14 Li2 O13 70.1(2) O14 Li2 O10 80.5(4) O14 Li2 O12 147.9(5) O14 Li2 O10A 80.5(5) O14 Li2 O12A 132.8(5) O15 Li2 O13 114.0(3) O15 Li2 O14 72.9(3) O15 Li2 O10 82.0(4) O15 Li2 O12 136.3(4) O15 Li2 O10A 77.8(6) O15 Li2 O12A 150.9(5) O16 Li2 O13 70.7(2) O16 Li2 O14 110.6(3) O16 Li2 O15 74.2(3) O16 Li2 O9 84.0(4) O16 Li2 O10 148.7(5) O16 Li2 O11 135.4(5) O16 Li2 O12 74.6(3) O16 Li2 O9A 83.7(5) O16 Li2 O10A 144.7(6) O16 Li2 O11A 143.9(6) O16 Li2 O12A 82.2(4) O9 Li2 O13 146.8(4) O9 Li2 O14 141.3(5) O9 Li2 O15 77.6(4) O9 Li2 O10 71.1(4) O9 Li2 O12 69.5(3) O10 Li2 O13 139.1(4) O10 Li2 O12 112.0(5) O11 Li2 O13 77.4(4) O11 Li2 O14 85.9(4) O11 Li2 O15 149.3(5) O11 Li2 O9 109.1(5) O11 Li2 O10 72.6(5) O11 Li2 O12 71.1(4) O9A Li2 O13 139.0(5) O9A Li2 O14 150.7(5) O9A Li2 O15 87.7(5) O9A Li2 O10A 74.1(6) O9A Li2 O12A 72.7(5) O10A Li2 O13 142.0(5) O10A Li2 O12A 115.5(7) O11A Li2 O13 79.9(6) O11A Li2 O14 77.0(6) O11A Li2 O15 139.0(5) O11A Li2 O9A 106.8(8) O11A Li2 O10A 70.2(7) O11A Li2 O12A 69.0(5) C95A O20 C93 105.9(11) C95B O20 C93 106.8(14) O20 C93 C95 105.5(9) C94 C95 C93 99.2(12) C94A C95 C93 106.2(11) C95 C94 C95A 113.2(18) O20 C95A C94 100.8(19) C95B C94A C95 97.8(15) O20 C95B C94A 122.6(19) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Sn1 Sn2 2.8352(4) Sn1 Sn5 2.8379(4) Sn1 Sn6 2.8674(4) Sn2 Sn3 2.8382(4) Sn2 C1 2.181(4) Sn2 C7 2.196(5) Sn2 C7A 2.198(4) Sn3 Sn7 2.8400(4) Sn3 C13 2.181(4) Sn3 C19 2.188(4) Sn4 Sn5 2.8207(4) Sn4 Sn7 2.8364(4) Sn4 C25 2.167(4) Sn4 C31 2.182(4) Sn5 C37 2.180(4) Sn5 C43 2.183(4) Sn6 Sn7 2.8619(4) Sn6 C55 2.2150(17) Sn6 C49 2.216(4) Sn6 C49A 2.248(4) C1 C2 1.384(6) C1 C6 1.390(6) C2 C3 1.394(7) C3 C4 1.361(10) C4 C5 1.363(9) C5 C6 1.379(6) C13 C14 1.389(5) C13 C18 1.394(5) C14 C15 1.388(6) C15 C16 1.377(7) C16 C17 1.379(7) C17 C18 1.385(6) C19 C20 1.393(5) C19 C24 1.399(5) C20 C21 1.388(6) C21 C22 1.381(6) C22 C23 1.380(6) C23 C24 1.393(6) C25 C26 1.401(6) C25 C30 1.380(6) C26 C27 1.381(7) C27 C28 1.384(7) C28 C29 1.382(7) C29 C30 1.394(6) C31 C32 1.395(6) C31 C36 1.405(5) C32 C33 1.380(6) C33 C34 1.380(7) C34 C35 1.385(8) C35 C36 1.385(6) C37 C38 1.397(6) C37 C42 1.375(6) C38 C39 1.388(6) C39 C40 1.366(9) C40 C41 1.375(9) C41 C42 1.385(7) C43 C44 1.409(7) C43 C48 1.385(6) C44 C45 1.401(7) C45 C46 1.345(10) C46 C47 1.370(10) C47 C48 1.404(7) C60 C59 1.3900 C60 C55 1.3900 C59 C58 1.3900 C58 C57 1.3900 C57 C56 1.3900 C56 C55 1.3900 C7 C8 1.375(17) C7 C12 1.407(15) C8 C9 1.396(13) C9 C10 1.372(15) C10 C11 1.390(15) C11 C12 1.378(15) C49 C50 1.382(8) C49 C54 1.344(9) C50 C51 1.370(8) C51 C52 1.385(11) C52 C53 1.350(11) C53 C54 1.394(10) C7A C12A 1.3900 C7A C8A 1.3900 C12A C11A 1.3900 C11A C10A 1.3900 C10A C9A 1.3900 C9A C8A 1.3900 C49A C50A 1.3900 C49A C54A 1.3900 C50A C51A 1.3900 C51A C52A 1.3900 C52A C53A 1.3900 C53A C54A 1.3900 O1 C61 1.429(6) O1 C68 1.412(7) O1 Li1 2.239(9) O2 C62 1.387(8) O2 C63 1.436(9) O2 Li1 2.394(10) O3 C64 1.379(13) O3 C65 1.471(11) O3 Li1 2.491(12) O4 C66 1.355(10) O4 C67 1.474(11) O4 Li1 2.351(10) O5 C69 1.441(5) O5 C76 1.437(4) O5 Li1 2.233(11) O6 C70 1.437(4) O6 C71 1.437(4) O6 Li1 2.459(10) O7 C72 1.434(4) O7 C73 1.440(4) O7 Li1 2.245(10) O8 C74 1.437(4) O8 C75 1.435(5) O8 Li1 2.407(9) O5A C69A 1.437(5) O5A C76A 1.436(5) O5A Li1 2.192(11) O6A C70A 1.437(5) O6A C72A 1.437(5) O6A Li1 2.459(10) O7A C71A 1.440(5) O7A C73A 1.442(5) O7A Li1 2.268(10) O8A C74A 1.435(5) O8A C75A 1.436(5) O8A Li1 2.406(9) C61 C62 1.480(10) C63 C64 1.562(13) C65 C66 1.415(12) C67 C68 1.438(9) C69 C70 1.438(7) C71 C72 1.440(7) C73 C74 1.441(7) C75 C76 1.438(7) C69A C70A 1.437(8) C71A C72A 1.440(8) C73A C74A 1.436(8) C75A C76A 1.437(8) O13 C85 1.380(7) O13 C92 1.389(7) O13 Li2 2.518(9) O14 C86 1.395(6) O14 C87 1.410(6) O14 Li2 2.314(8) O15 C88 1.383(7) O15 C89 1.406(6) O15 Li2 2.303(9) O16 C90 1.353(7) O16 C91 1.379(6) O16 Li2 2.223(8) O9 C77 1.428(5) O9 C84 1.436(5) O9 Li2 2.293(9) O10 C78 1.434(5) O10 C79 1.430(5) O10 Li2 2.375(9) O11 C80 1.431(5) O11 C81 1.429(5) O11 Li2 2.259(10) O12 C82 1.435(5) O12 C83 1.432(5) O12 Li2 2.522(10) O9A C77A 1.428(5) O9A C84A 1.433(5) O9A Li2 2.287(10) O10A C78A 1.433(5) O10A C79A 1.431(5) O10A Li2 2.376(9) O11A C80A 1.433(5) O11A C81A 1.433(5) O11A Li2 2.263(10) O12A C82A 1.433(5) O12A C83A 1.434(5) O12A Li2 2.522(10) C85 C86 1.371(8) C87 C88 1.355(7) C89 C90 1.401(9) C91 C92 1.399(7) C77 C78 1.443(7) C79 C80 1.443(7) C81 C82 1.444(7) C83 C84 1.449(7) C77A C78A 1.445(7) C79A C80A 1.445(7) C81A C82A 1.446(7) C83A C84A 1.446(7) O20 C93 1.411(13) O20 C95A 1.36(2) O20 C95B 1.17(3) C93 C95 1.502(14) C95 C94 1.40(3) C95 C94A 1.46(2) C94 C95A 1.44(2) C94A C95B 1.44(2) loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons 1 0.135 0.314 0.344 9.9 0.0 2 0.500 0.000 0.000 319.9 77.6 3 0.500 0.000 0.500 106.6 23.8 4 0.865 0.686 0.656 9.9 0.0