#------------------------------------------------------------------------------ #$Date: 2020-02-04 22:10:29 +0200 (Tue, 04 Feb 2020) $ #$Revision: 247621 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125628.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_7125628 loop_ _publ_author_name 'Steller, Beate G.' 'Fischer, Roland C.' 'Flock, Michaela' 'Hill, Michael S.' 'Liptrot, David J.' 'McMullin, Claire L.' 'Rajabi, Nasir A.' 'Tiefling, Kathrin' 'Wilson, Andrew S. S.' _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_issue 3 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 336 _journal_page_last 339 _journal_paper_doi 10.1039/c9cc07976a _journal_volume 56 _journal_year 2020 _chemical_formula_moiety 'C12 H26 Li O6, C18 H16 Al' _chemical_formula_sum 'C30 H42 Al Li O6' _chemical_formula_weight 532.55 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _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 90 _cell_angle_beta 106.3590(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.8667(4) _cell_length_b 20.5281(8) _cell_length_c 12.5639(5) _cell_measurement_reflns_used 5511 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.20 _cell_measurement_theta_min 2.61 _cell_volume 2936.67(19) _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 100.15 _diffrn_measured_fraction_theta_full 0.992 _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 0.0617 _diffrn_reflns_av_unetI/netI 0.0530 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 14532 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 26.000 _diffrn_reflns_theta_min 2.045 _diffrn_source 'sealed tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.109 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.205 _exptl_crystal_description Block _exptl_crystal_F_000 1144 _exptl_crystal_size_max 0.198 _exptl_crystal_size_mid 0.175 _exptl_crystal_size_min 0.139 _refine_diff_density_max 0.636 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.053 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 377 _refine_ls_number_reflns 5737 _refine_ls_number_restraints 20 _refine_ls_restrained_S_all 1.065 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0542 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0713P)^2^+1.5137P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1421 _refine_ls_wR_factor_ref 0.1531 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4290 _reflns_number_total 5737 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL RF224_0m in P2(1)/c CELL 0.71073 11.8667 20.5281 12.5639 90 106.359 90 ZERR 4 0.0004 0.0008 0.0005 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Al Li O UNIT 120 168 4 4 24 SADI 0.005 O4 C25 O4A C25 O3 C23A O3 C23 SADI 0.005 C24 C23 C24A C23A SADI 0.005 O6 C30 O6A C30A O5A C27A O5 C27 SADI 0.005 O5A C28A O5 C28 O6A C29A O6 C29 SADI 0.005 C29 C28 C29A C28A EADP C24A C24 EADP O4A O4 EADP C23A C23 EADP O6A O6 EADP C30 C30A EADP C29A C29 EADP C28 C28A EADP C27A C27 EADP O5A O5 L.S. 20 PLAN 5 SIZE 0.139 0.175 0.198 TEMP -173 LIST 6 CONF HTAB BOND fmap 2 acta 52 OMIT -3 52 REM REM REM WGHT 0.071300 1.513700 FVAR 0.11692 O1 5 0.819151 0.201429 -0.131504 11.00000 0.03185 0.03781 = 0.02906 -0.00053 0.00963 0.00570 O2 5 0.602572 0.197685 -0.097801 11.00000 0.03048 0.03228 = 0.03125 -0.00574 0.00574 0.00111 O3 5 0.692252 0.199033 0.124820 11.00000 0.02905 0.04790 = 0.03198 -0.00091 0.01007 -0.01054 PART 1 O4 5 0.908163 0.195823 0.087695 10.80000 0.01828 0.03349 = 0.02854 0.00489 0.00827 0.00074 O5 5 0.703164 0.332529 -0.024143 10.80000 0.02838 0.02377 = 0.05585 -0.00725 0.00126 0.00164 O6 5 0.929723 0.334850 0.134008 10.80000 0.05309 0.04596 = 0.06618 0.01441 0.03610 0.01019 PART 0 PART 2 O4A 5 0.869641 0.172822 0.084226 10.20000 0.01828 0.03349 = 0.02854 0.00489 0.00827 0.00074 O5A 5 0.676985 0.329907 -0.061473 10.20000 0.02838 0.02377 = 0.05585 -0.00725 0.00126 0.00164 O6A 5 0.891112 0.311042 0.091687 10.20000 0.05309 0.04596 = 0.06618 0.01441 0.03610 0.01019 PART 0 C19 1 0.737151 0.153190 -0.190403 11.00000 0.04123 0.05461 = 0.03261 -0.01992 0.00974 0.00083 AFIX 23 H19A 2 0.747695 0.111889 -0.148052 11.00000 -1.20000 H19B 2 0.749235 0.144573 -0.263940 11.00000 -1.20000 AFIX 0 C20 1 0.616790 0.180198 -0.203468 11.00000 0.04022 0.05411 = 0.03025 -0.00802 0.00088 0.00345 AFIX 23 H20A 2 0.604646 0.219071 -0.252017 11.00000 -1.20000 H20B 2 0.557162 0.147247 -0.239081 11.00000 -1.20000 AFIX 0 C21 1 0.569133 0.145558 -0.036431 11.00000 0.02425 0.02958 = 0.04544 -0.00857 0.00919 -0.00451 AFIX 23 H21A 2 0.623079 0.108048 -0.029990 11.00000 -1.20000 H21B 2 0.488090 0.130876 -0.073452 11.00000 -1.20000 AFIX 0 C22 1 0.576969 0.173442 0.075651 11.00000 0.02545 0.03730 = 0.04486 -0.00582 0.01613 -0.00551 AFIX 23 H22A 2 0.518104 0.208562 0.068375 11.00000 -1.20000 H22B 2 0.559522 0.139081 0.123991 11.00000 -1.20000 AFIX 0 C25 1 0.943770 0.144191 0.024524 11.00000 0.02238 0.04133 = 0.04261 0.00318 0.01088 0.01039 PART 1 AFIX 23 H25A 2 0.890529 0.106199 0.015612 10.80000 -1.20000 H25B 2 1.025221 0.129866 0.060761 10.80000 -1.20000 AFIX 23 PART 0 PART 2 H25C 2 0.923170 0.097555 0.011682 10.20000 -1.20000 H25D 2 1.026309 0.146667 0.070920 10.20000 -1.20000 AFIX 0 PART 0 C26 1 0.934591 0.175993 -0.084578 11.00000 0.02925 0.03444 = 0.04311 -0.00125 0.01856 0.00370 AFIX 23 H26A 2 0.992656 0.211757 -0.074138 11.00000 -1.20000 H26B 2 0.952745 0.143783 -0.136040 11.00000 -1.20000 AFIX 0 PART 1 C23 1 0.775227 0.147955 0.179043 10.80000 0.03741 0.04060 = 0.01781 0.00896 0.00459 -0.00433 AFIX 23 H23A 2 0.763803 0.108263 0.132462 10.80000 -1.20000 H23B 2 0.764073 0.136558 0.251970 10.80000 -1.20000 AFIX 0 C24 1 0.895723 0.175913 0.193192 10.80000 0.03149 0.03843 = 0.02566 0.00457 0.00309 -0.00084 AFIX 23 H24A 2 0.907809 0.213818 0.243877 10.80000 -1.20000 H24B 2 0.955930 0.142766 0.226489 10.80000 -1.20000 AFIX 0 C27 1 0.582164 0.349978 -0.055232 10.80000 0.03274 0.03574 = 0.08842 -0.01180 -0.00720 0.01122 AFIX 137 H27A 2 0.534011 0.310667 -0.075405 10.80000 -1.50000 H27B 2 0.565768 0.379641 -0.118876 10.80000 -1.50000 H27C 2 0.563418 0.371638 0.007184 10.80000 -1.50000 AFIX 0 C28 1 0.777604 0.388728 0.003692 10.80000 0.03259 0.01795 = 0.03376 0.00001 0.01418 -0.00717 AFIX 23 H28A 2 0.762726 0.411470 0.067899 10.80000 -1.20000 H28B 2 0.760213 0.419296 -0.059808 10.80000 -1.20000 AFIX 0 C29 1 0.903254 0.367829 0.031640 10.80000 0.03698 0.04367 = 0.03767 -0.00646 0.02481 -0.01747 AFIX 23 H29A 2 0.915533 0.338633 -0.026816 10.80000 -1.20000 H29B 2 0.954943 0.406280 0.037157 10.80000 -1.20000 AFIX 0 C30 1 1.051078 0.318582 0.165882 10.80000 0.03967 0.05565 = 0.07953 -0.00158 0.02899 -0.00368 AFIX 137 H30A 2 1.069572 0.293897 0.106176 10.80000 -1.50000 H30B 2 1.069293 0.292054 0.233441 10.80000 -1.50000 H30C 2 1.098028 0.358581 0.180001 10.80000 -1.50000 AFIX 0 PART 0 PART 2 C23A 1 0.778682 0.175046 0.221146 10.20000 0.03741 0.04060 = 0.01781 0.00896 0.00459 -0.00433 AFIX 23 H23C 2 0.743774 0.149862 0.271147 10.20000 -1.20000 H23D 2 0.830071 0.209912 0.263006 10.20000 -1.20000 AFIX 0 C24A 1 0.839402 0.132686 0.157325 10.20000 0.03149 0.03843 = 0.02566 0.00457 0.00309 -0.00084 AFIX 23 H24C 2 0.910060 0.112273 0.207682 10.20000 -1.20000 H24D 2 0.786126 0.097882 0.117776 10.20000 -1.20000 AFIX 0 C27A 1 0.554488 0.338939 -0.109214 10.20000 0.03274 0.03574 = 0.08842 -0.01180 -0.00720 0.01122 AFIX 137 H27D 2 0.526348 0.308856 -0.171635 10.20000 -1.50000 H27E 2 0.539438 0.383887 -0.135680 10.20000 -1.50000 H27F 2 0.513132 0.330307 -0.053280 10.20000 -1.50000 AFIX 0 C28A 1 0.735672 0.384595 -0.000692 10.20000 0.03259 0.01795 = 0.03376 0.00001 0.01418 -0.00717 AFIX 23 H28C 2 0.706489 0.392305 0.064694 10.20000 -1.20000 H28D 2 0.719362 0.423986 -0.048020 10.20000 -1.20000 AFIX 0 C29A 1 0.865011 0.371924 0.036263 10.20000 0.03698 0.04367 = 0.03767 -0.00646 0.02481 -0.01747 AFIX 23 H29C 2 0.896063 0.372204 -0.029076 10.20000 -1.20000 H29D 2 0.904487 0.407215 0.086815 10.20000 -1.20000 AFIX 0 C30A 1 1.009262 0.294204 0.149086 10.20000 0.03967 0.05565 = 0.07953 -0.00158 0.02899 -0.00368 AFIX 137 H30D 2 1.054745 0.288795 0.095559 10.20000 -1.50000 H30E 2 1.009972 0.253333 0.189577 10.20000 -1.50000 H30F 2 1.044220 0.328921 0.201549 10.20000 -1.50000 AFIX 0 PART 0 LI1 4 0.756706 0.241640 0.000644 11.00000 0.02454 0.02462 = 0.02902 0.00042 0.00660 0.00654 AL1 3 1.272578 0.046745 0.130207 11.00000 0.01861 0.02922 = 0.02181 0.00221 0.00481 -0.00011 C1 1 1.282444 0.142051 0.093604 11.00000 0.01489 0.03633 = 0.03370 0.00618 0.00775 0.00193 C2 1 1.313797 0.190192 0.176250 11.00000 0.02807 0.03934 = 0.03554 0.00483 0.01150 0.00330 AFIX 43 H2 2 1.331034 0.176955 0.251585 11.00000 -1.20000 AFIX 0 C3 1 1.320956 0.256127 0.153740 11.00000 0.03264 0.03728 = 0.05382 -0.00106 0.01960 0.00219 AFIX 43 H3 2 1.342537 0.286733 0.212718 11.00000 -1.20000 AFIX 0 C4 1 1.296342 0.276903 0.044475 11.00000 0.03284 0.03589 = 0.06343 0.01359 0.02130 0.00420 AFIX 43 H4 2 1.301184 0.321820 0.028098 11.00000 -1.20000 AFIX 0 C5 1 1.264698 0.231700 -0.040428 11.00000 0.03116 0.05678 = 0.04074 0.02093 0.00974 -0.00186 AFIX 43 H5 2 1.247251 0.245508 -0.115485 11.00000 -1.20000 AFIX 0 C6 1 1.258456 0.165623 -0.015493 11.00000 0.02667 0.04695 = 0.03179 0.00708 0.00721 -0.00401 AFIX 43 H6 2 1.237044 0.135337 -0.074968 11.00000 -1.20000 AFIX 0 C7 1 1.431133 0.012016 0.214097 11.00000 0.02239 0.01994 = 0.02492 -0.00353 0.00574 -0.00423 C8 1 1.461764 -0.012685 0.323000 11.00000 0.02833 0.02771 = 0.02652 -0.00128 0.00822 -0.00192 AFIX 43 H8 2 1.404782 -0.011854 0.363057 11.00000 -1.20000 AFIX 0 C9 1 1.572621 -0.038339 0.374343 11.00000 0.03750 0.02946 = 0.02748 0.00243 -0.00426 0.00072 AFIX 43 H9 2 1.590298 -0.054028 0.448354 11.00000 -1.20000 AFIX 0 C10 1 1.656828 -0.040930 0.317456 11.00000 0.02109 0.03066 = 0.04905 -0.00444 -0.00231 0.00183 AFIX 43 H10 2 1.732088 -0.058881 0.351798 11.00000 -1.20000 AFIX 0 C11 1 1.630648 -0.017200 0.210256 11.00000 0.02402 0.03257 = 0.04945 -0.00716 0.01386 -0.00351 AFIX 43 H11 2 1.687950 -0.018641 0.170591 11.00000 -1.20000 AFIX 0 C12 1 1.520188 0.008751 0.160842 11.00000 0.02823 0.02618 = 0.02640 -0.00225 0.00809 -0.00294 AFIX 43 H12 2 1.504160 0.025097 0.087346 11.00000 -1.20000 AFIX 0 C13 1 1.159658 0.035004 0.221423 11.00000 0.02247 0.02620 = 0.02387 0.00525 0.00584 0.00454 C14 1 1.178356 0.061283 0.328368 11.00000 0.02315 0.03396 = 0.02622 0.00293 0.00230 0.00154 AFIX 43 H14 2 1.249258 0.084297 0.360443 11.00000 -1.20000 AFIX 0 C15 1 1.097421 0.055015 0.389233 11.00000 0.03167 0.03805 = 0.02284 0.00097 0.00744 0.00725 AFIX 43 H15 2 1.113433 0.073893 0.460986 11.00000 -1.20000 AFIX 0 C16 1 0.994044 0.021455 0.345571 11.00000 0.02826 0.03535 = 0.03604 0.00919 0.01665 0.00590 AFIX 43 H16 2 0.938871 0.016812 0.387104 11.00000 -1.20000 AFIX 0 C17 1 0.971512 -0.005373 0.240704 11.00000 0.02665 0.03234 = 0.04045 0.00099 0.01138 -0.00284 AFIX 43 H17 2 0.900393 -0.028405 0.209653 11.00000 -1.20000 AFIX 0 C18 1 1.053255 0.001411 0.180598 11.00000 0.02624 0.02713 = 0.02645 0.00047 0.00671 0.00175 AFIX 43 H18 2 1.036157 -0.017548 0.108835 11.00000 -1.20000 AFIX 0 H1 2 1.223748 0.009456 0.009308 11.00000 -1.20000 HKLF 4 REM RF224_0m in P2(1)/c REM R1 = 0.0542 for 4290 Fo > 4sig(Fo) and 0.0745 for all 5737 data REM 377 parameters refined using 20 restraints END WGHT 0.0715 1.5116 REM Instructions for potential hydrogen bonds HTAB C27 O2 EQIV $1 x, -y+1/2, z+1/2 HTAB C23A O5A_$1 HTAB C23A O1_$1 HTAB C30A O4A REM Highest difference peak 0.636, deepest hole -0.420, 1-sigma level 0.053 Q1 1 0.8590 0.3324 0.0709 11.00000 0.05 0.64 Q2 1 0.6593 0.3753 -0.0132 11.00000 0.05 0.50 Q3 1 0.7379 0.1858 0.1921 11.00000 0.05 0.45 Q4 1 0.6244 0.3242 -0.0976 11.00000 0.05 0.38 Q5 1 0.6779 0.1419 -0.1648 11.00000 0.05 0.36 REM The information below was added by Olex2. REM REM R1 = 0.0542 for 4290 Fo > 4sig(Fo) and 0.0745 for all 16128 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.64, deepest hole -0.42 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0745 REM R1_gt = 0.0542 REM wR_ref = 0.1531 REM GOOF = 1.049 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 16128 REM Reflections_gt = 4290 REM Parameters = n/a REM Hole = -0.42 REM Peak = 0.64 REM Flack = n/a ; _cod_data_source_file c9cc07976a2.cif _cod_data_source_block rf224_0m _cod_depositor_comments 'Adding full bibliography for 7125626--7125630.cif.' _cod_database_code 7125628 _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 0.985 _shelx_estimated_absorpt_t_min 0.979 _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 At 1.5 times of: All C(H,H,H) groups 2. Restrained distances O4-C25 \\sim O4A-C25 \\sim O3-C23A \\sim O3-C23 with sigma of 0.005 C24-C23 \\sim C24A-C23A with sigma of 0.005 O6-C30 \\sim O6A-C30A \\sim O5A-C27A \\sim O5-C27 with sigma of 0.005 O5A-C28A \\sim O5-C28 \\sim O6A-C29A \\sim O6-C29 with sigma of 0.005 C29-C28 \\sim C29A-C28A with sigma of 0.005 3. Uiso/Uaniso restraints and constraints Uanis(C24A) = Uanis(C24) Uanis(O4A) = Uanis(O4) Uanis(C23A) = Uanis(C23) Uanis(O6A) = Uanis(O6) Uanis(C30) = Uanis(C30A) Uanis(C29A) = Uanis(C29) Uanis(C28) = Uanis(C28A) Uanis(C27A) = Uanis(C27) Uanis(O5A) = Uanis(O5) 4. Others Fixed Sof: O4(0.8) O5(0.8) O6(0.8) O4A(0.2) O5A(0.2) O6A(0.2) H25A(0.8) H25B(0.8) H25C(0.2) H25D(0.2) C23(0.8) H23A(0.8) H23B(0.8) C24(0.8) H24A(0.8) H24B(0.8) C27(0.8) H27A(0.8) H27B(0.8) H27C(0.8) C28(0.8) H28A(0.8) H28B(0.8) C29(0.8) H29A(0.8) H29B(0.8) C30(0.8) H30A(0.8) H30B(0.8) H30C(0.8) C23A(0.2) H23C(0.2) H23D(0.2) C24A(0.2) H24C(0.2) H24D(0.2) C27A(0.2) H27D(0.2) H27E(0.2) H27F(0.2) C28A(0.2) H28C(0.2) H28D(0.2) C29A(0.2) H29C(0.2) H29D(0.2) C30A(0.2) H30D(0.2) H30E(0.2) H30F(0.2) 5.a Secondary CH2 refined with riding coordinates: C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C25(H25A, H25B), C25(H25C,H25D), C26(H26A,H26B), C23(H23A,H23B), C24(H24A,H24B), C28(H28A,H28B), C29(H29A,H29B), C23A(H23C,H23D), C24A(H24C,H24D), C28A(H28C, H28D), C29A(H29C,H29D) 5.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18) 5.c Idealised Me refined as rotating group: C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C27A(H27D,H27E,H27F), C30A(H30D, H30E,H30F) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.81915(14) 0.20143(8) -0.13150(13) 0.0327(4) Uani 1 1 d . . . . O2 O 0.60257(14) 0.19768(7) -0.09780(13) 0.0319(4) Uani 1 1 d . . . . O3 O 0.69225(14) 0.19903(8) 0.12482(13) 0.0360(4) Uani 1 1 d D . . . O4 O 0.90816(17) 0.19582(9) 0.08770(16) 0.0264(5) Uani 0.8 1 d D P A 1 O5 O 0.7032(2) 0.33253(15) -0.0241(2) 0.0382(7) Uani 0.8 1 d D P A 1 O6 O 0.9297(2) 0.33485(12) 0.1340(2) 0.0511(7) Uani 0.8 1 d D P A 1 O4A O 0.8696(7) 0.1728(4) 0.0842(7) 0.0264(5) Uani 0.2 1 d D P A 2 O5A O 0.6770(10) 0.3299(7) -0.0615(12) 0.0382(7) Uani 0.2 1 d D P A 2 O6A O 0.8911(9) 0.3110(5) 0.0917(10) 0.0511(7) Uani 0.2 1 d D P A 2 C19 C 0.7372(2) 0.15319(14) -0.1904(2) 0.0430(6) Uani 1 1 d . . . . H19A H 0.7477 0.1119 -0.1481 0.052 Uiso 1 1 calc R . . . H19B H 0.7492 0.1446 -0.2639 0.052 Uiso 1 1 calc R . . . C20 C 0.6168(2) 0.18020(14) -0.2035(2) 0.0434(6) Uani 1 1 d . . . . H20A H 0.6046 0.2191 -0.2520 0.052 Uiso 1 1 calc R . . . H20B H 0.5572 0.1472 -0.2391 0.052 Uiso 1 1 calc R . . . C21 C 0.5691(2) 0.14556(11) -0.0364(2) 0.0332(5) Uani 1 1 d . . . . H21A H 0.6231 0.1080 -0.0300 0.040 Uiso 1 1 calc R . . . H21B H 0.4881 0.1309 -0.0735 0.040 Uiso 1 1 calc R . . . C22 C 0.5770(2) 0.17344(12) 0.0757(2) 0.0346(5) Uani 1 1 d . . . . H22A H 0.5181 0.2086 0.0684 0.042 Uiso 1 1 calc R . . . H22B H 0.5595 0.1391 0.1240 0.042 Uiso 1 1 calc R . . . C25 C 0.9438(2) 0.14419(12) 0.0245(2) 0.0351(5) Uani 1 1 d D . . . H25A H 0.8905 0.1062 0.0156 0.042 Uiso 0.8 1 calc R P A 1 H25B H 1.0252 0.1299 0.0608 0.042 Uiso 0.8 1 calc R P A 1 H25C H 0.9232 0.0976 0.0117 0.042 Uiso 0.2 1 calc R P A 2 H25D H 1.0263 0.1467 0.0709 0.042 Uiso 0.2 1 calc R P A 2 C26 C 0.9346(2) 0.17599(12) -0.0846(2) 0.0339(5) Uani 1 1 d . . . . H26A H 0.9927 0.2118 -0.0741 0.041 Uiso 1 1 calc R . . . H26B H 0.9527 0.1438 -0.1360 0.041 Uiso 1 1 calc R . . . C23 C 0.7752(2) 0.14796(14) 0.1790(2) 0.0326(7) Uani 0.8 1 d D P A 1 H23A H 0.7638 0.1083 0.1325 0.039 Uiso 0.8 1 calc R P A 1 H23B H 0.7641 0.1366 0.2520 0.039 Uiso 0.8 1 calc R P A 1 C24 C 0.8957(3) 0.17591(15) 0.1932(2) 0.0329(6) Uani 0.8 1 d D P A 1 H24A H 0.9078 0.2138 0.2439 0.039 Uiso 0.8 1 calc R P A 1 H24B H 0.9559 0.1428 0.2265 0.039 Uiso 0.8 1 calc R P A 1 C27 C 0.5822(3) 0.34998(19) -0.0552(4) 0.0572(11) Uani 0.8 1 d D P A 1 H27A H 0.5340 0.3107 -0.0754 0.086 Uiso 0.8 1 calc GR P A 1 H27B H 0.5658 0.3796 -0.1189 0.086 Uiso 0.8 1 calc GR P A 1 H27C H 0.5634 0.3716 0.0072 0.086 Uiso 0.8 1 calc GR P A 1 C28 C 0.7776(2) 0.38873(16) 0.0037(3) 0.0271(8) Uani 0.8 1 d D P A 1 H28A H 0.7627 0.4115 0.0679 0.033 Uiso 0.8 1 calc R P A 1 H28B H 0.7602 0.4193 -0.0598 0.033 Uiso 0.8 1 calc R P A 1 C29 C 0.9033(3) 0.36783(19) 0.0316(3) 0.0365(8) Uani 0.8 1 d D P A 1 H29A H 0.9155 0.3386 -0.0268 0.044 Uiso 0.8 1 calc R P A 1 H29B H 0.9549 0.4063 0.0372 0.044 Uiso 0.8 1 calc R P A 1 C30 C 1.0511(3) 0.3186(2) 0.1659(4) 0.0558(10) Uani 0.8 1 d D P A 1 H30A H 1.0696 0.2939 0.1062 0.084 Uiso 0.8 1 calc GR P A 1 H30B H 1.0693 0.2921 0.2334 0.084 Uiso 0.8 1 calc GR P A 1 H30C H 1.0980 0.3586 0.1800 0.084 Uiso 0.8 1 calc GR P A 1 C23A C 0.7787(9) 0.1750(6) 0.2211(6) 0.0326(7) Uani 0.2 1 d D P A 2 H23C H 0.7438 0.1499 0.2711 0.039 Uiso 0.2 1 calc R P A 2 H23D H 0.8301 0.2099 0.2630 0.039 Uiso 0.2 1 calc R P A 2 C24A C 0.8394(11) 0.1327(6) 0.1573(9) 0.0329(6) Uani 0.2 1 d D P A 2 H24C H 0.9101 0.1123 0.2077 0.039 Uiso 0.2 1 calc R P A 2 H24D H 0.7861 0.0979 0.1178 0.039 Uiso 0.2 1 calc R P A 2 C27A C 0.5545(11) 0.3389(9) -0.1092(17) 0.0572(11) Uani 0.2 1 d D P A 2 H27D H 0.5263 0.3089 -0.1716 0.086 Uiso 0.2 1 calc GR P A 2 H27E H 0.5394 0.3839 -0.1357 0.086 Uiso 0.2 1 calc GR P A 2 H27F H 0.5131 0.3303 -0.0533 0.086 Uiso 0.2 1 calc GR P A 2 C28A C 0.7357(12) 0.3846(8) -0.0007(15) 0.0271(8) Uani 0.2 1 d D P A 2 H28C H 0.7065 0.3923 0.0647 0.033 Uiso 0.2 1 calc R P A 2 H28D H 0.7194 0.4240 -0.0480 0.033 Uiso 0.2 1 calc R P A 2 C29A C 0.8650(14) 0.3719(7) 0.0363(16) 0.0365(8) Uani 0.2 1 d D P A 2 H29C H 0.8961 0.3722 -0.0291 0.044 Uiso 0.2 1 calc R P A 2 H29D H 0.9045 0.4072 0.0868 0.044 Uiso 0.2 1 calc R P A 2 C30A C 1.0093(10) 0.2942(9) 0.1491(16) 0.0558(10) Uani 0.2 1 d D P A 2 H30D H 1.0547 0.2888 0.0956 0.084 Uiso 0.2 1 calc GR P A 2 H30E H 1.0100 0.2533 0.1896 0.084 Uiso 0.2 1 calc GR P A 2 H30F H 1.0442 0.3289 0.2015 0.084 Uiso 0.2 1 calc GR P A 2 Li1 Li 0.7567(3) 0.24164(17) 0.0006(3) 0.0263(8) Uani 1 1 d . . . . Al1 Al 1.27258(5) 0.04675(3) 0.13021(5) 0.02339(18) Uani 1 1 d . . . . C1 C 1.28244(18) 0.14205(11) 0.09360(19) 0.0281(5) Uani 1 1 d . . . . C2 C 1.3138(2) 0.19019(12) 0.1763(2) 0.0338(5) Uani 1 1 d . . . . H2 H 1.3310 0.1770 0.2516 0.041 Uiso 1 1 calc R . . . C3 C 1.3210(2) 0.25613(12) 0.1537(2) 0.0397(6) Uani 1 1 d . . . . H3 H 1.3425 0.2867 0.2127 0.048 Uiso 1 1 calc R . . . C4 C 1.2963(2) 0.27690(13) 0.0445(2) 0.0425(6) Uani 1 1 d . . . . H4 H 1.3012 0.3218 0.0281 0.051 Uiso 1 1 calc R . . . C5 C 1.2647(2) 0.23170(14) -0.0404(2) 0.0430(6) Uani 1 1 d . . . . H5 H 1.2473 0.2455 -0.1155 0.052 Uiso 1 1 calc R . . . C6 C 1.2585(2) 0.16562(13) -0.0155(2) 0.0353(6) Uani 1 1 d . . . . H6 H 1.2370 0.1353 -0.0750 0.042 Uiso 1 1 calc R . . . C7 C 1.43113(18) 0.01202(10) 0.21410(17) 0.0226(4) Uani 1 1 d . . . . C8 C 1.46176(19) -0.01268(10) 0.32300(18) 0.0274(5) Uani 1 1 d . . . . H8 H 1.4048 -0.0119 0.3631 0.033 Uiso 1 1 calc R . . . C9 C 1.5726(2) -0.03834(11) 0.3743(2) 0.0342(5) Uani 1 1 d . . . . H9 H 1.5903 -0.0540 0.4484 0.041 Uiso 1 1 calc R . . . C10 C 1.6568(2) -0.04093(11) 0.3175(2) 0.0361(6) Uani 1 1 d . . . . H10 H 1.7321 -0.0589 0.3518 0.043 Uiso 1 1 calc R . . . C11 C 1.6306(2) -0.01720(11) 0.2103(2) 0.0346(5) Uani 1 1 d . . . . H11 H 1.6879 -0.0186 0.1706 0.042 Uiso 1 1 calc R . . . C12 C 1.52019(19) 0.00875(10) 0.16084(18) 0.0269(5) Uani 1 1 d . . . . H12 H 1.5042 0.0251 0.0873 0.032 Uiso 1 1 calc R . . . C13 C 1.15966(18) 0.03500(10) 0.22142(17) 0.0243(4) Uani 1 1 d . . . . C14 C 1.17836(19) 0.06128(11) 0.32837(18) 0.0287(5) Uani 1 1 d . . . . H14 H 1.2493 0.0843 0.3604 0.034 Uiso 1 1 calc R . . . C15 C 1.0974(2) 0.05501(11) 0.38923(19) 0.0309(5) Uani 1 1 d . . . . H15 H 1.1134 0.0739 0.4610 0.037 Uiso 1 1 calc R . . . C16 C 0.9940(2) 0.02145(11) 0.3456(2) 0.0317(5) Uani 1 1 d . . . . H16 H 0.9389 0.0168 0.3871 0.038 Uiso 1 1 calc R . . . C17 C 0.9715(2) -0.00537(11) 0.2407(2) 0.0328(5) Uani 1 1 d . . . . H17 H 0.9004 -0.0284 0.2097 0.039 Uiso 1 1 calc R . . . C18 C 1.05325(19) 0.00141(10) 0.18060(18) 0.0268(5) Uani 1 1 d . . . . H18 H 1.0362 -0.0175 0.1088 0.032 Uiso 1 1 calc R . . . H1 H 1.224(2) 0.0095(12) 0.0093(19) 0.032 Uiso 1 1 d R . . . 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 O1 0.0318(9) 0.0378(9) 0.0291(8) -0.0005(7) 0.0096(7) 0.0057(7) O2 0.0305(8) 0.0323(8) 0.0312(9) -0.0057(7) 0.0057(7) 0.0011(7) O3 0.0290(9) 0.0479(10) 0.0320(9) -0.0009(8) 0.0101(7) -0.0105(8) O4 0.0183(11) 0.0335(12) 0.0285(9) 0.0049(9) 0.0083(9) 0.0007(8) O5 0.0284(15) 0.0238(9) 0.056(2) -0.0073(14) 0.0013(12) 0.0016(11) O6 0.0531(18) 0.0460(16) 0.066(2) 0.0144(13) 0.0361(14) 0.0102(12) O4A 0.0183(11) 0.0335(12) 0.0285(9) 0.0049(9) 0.0083(9) 0.0007(8) O5A 0.0284(15) 0.0238(9) 0.056(2) -0.0073(14) 0.0013(12) 0.0016(11) O6A 0.0531(18) 0.0460(16) 0.066(2) 0.0144(13) 0.0361(14) 0.0102(12) C19 0.0412(15) 0.0546(16) 0.0326(13) -0.0199(12) 0.0097(11) 0.0008(12) C20 0.0402(15) 0.0541(16) 0.0303(13) -0.0080(12) 0.0009(11) 0.0034(12) C21 0.0243(11) 0.0296(12) 0.0454(14) -0.0086(10) 0.0092(10) -0.0045(9) C22 0.0254(12) 0.0373(13) 0.0449(14) -0.0058(11) 0.0161(10) -0.0055(10) C25 0.0224(11) 0.0413(13) 0.0426(14) 0.0032(11) 0.0109(10) 0.0104(10) C26 0.0292(12) 0.0344(12) 0.0431(14) -0.0013(11) 0.0186(10) 0.0037(10) C23 0.0374(16) 0.0406(18) 0.0178(15) 0.0090(12) 0.0046(13) -0.0043(15) C24 0.0315(16) 0.0384(16) 0.0257(14) 0.0046(12) 0.0031(12) -0.0008(12) C27 0.033(2) 0.036(2) 0.088(4) -0.012(2) -0.007(2) 0.0112(16) C28 0.033(2) 0.0180(12) 0.0338(14) 0.0000(10) 0.0142(19) -0.0072(16) C29 0.037(2) 0.0437(15) 0.0377(15) -0.0065(12) 0.0248(17) -0.0175(16) C30 0.040(2) 0.056(3) 0.080(3) -0.002(2) 0.029(2) -0.0037(17) C23A 0.0374(16) 0.0406(18) 0.0178(15) 0.0090(12) 0.0046(13) -0.0043(15) C24A 0.0315(16) 0.0384(16) 0.0257(14) 0.0046(12) 0.0031(12) -0.0008(12) C27A 0.033(2) 0.036(2) 0.088(4) -0.012(2) -0.007(2) 0.0112(16) C28A 0.033(2) 0.0180(12) 0.0338(14) 0.0000(10) 0.0142(19) -0.0072(16) C29A 0.037(2) 0.0437(15) 0.0377(15) -0.0065(12) 0.0248(17) -0.0175(16) C30A 0.040(2) 0.056(3) 0.080(3) -0.002(2) 0.029(2) -0.0037(17) Li1 0.0245(18) 0.0246(18) 0.0290(19) 0.0004(15) 0.0066(15) 0.0065(15) Al1 0.0186(3) 0.0292(3) 0.0218(3) 0.0022(3) 0.0048(2) -0.0001(3) C1 0.0149(10) 0.0363(12) 0.0337(12) 0.0062(10) 0.0077(9) 0.0019(9) C2 0.0281(12) 0.0393(13) 0.0355(13) 0.0048(11) 0.0115(10) 0.0033(10) C3 0.0326(13) 0.0373(13) 0.0538(16) -0.0011(12) 0.0196(11) 0.0022(11) C4 0.0328(13) 0.0359(13) 0.0634(18) 0.0136(13) 0.0213(12) 0.0042(11) C5 0.0312(13) 0.0568(17) 0.0407(14) 0.0209(13) 0.0097(11) -0.0019(12) C6 0.0267(12) 0.0469(14) 0.0318(13) 0.0071(11) 0.0072(10) -0.0040(11) C7 0.0224(10) 0.0199(10) 0.0249(11) -0.0035(8) 0.0057(8) -0.0042(8) C8 0.0283(11) 0.0277(11) 0.0265(11) -0.0013(9) 0.0082(9) -0.0019(9) C9 0.0375(13) 0.0295(12) 0.0275(12) 0.0024(10) -0.0043(10) 0.0007(10) C10 0.0211(11) 0.0307(12) 0.0490(15) -0.0044(11) -0.0023(10) 0.0018(9) C11 0.0240(12) 0.0326(12) 0.0495(15) -0.0072(11) 0.0139(10) -0.0035(10) C12 0.0282(11) 0.0262(11) 0.0264(11) -0.0022(9) 0.0081(9) -0.0029(9) C13 0.0225(10) 0.0262(10) 0.0239(11) 0.0052(9) 0.0058(8) 0.0045(9) C14 0.0231(11) 0.0340(12) 0.0262(11) 0.0029(9) 0.0023(9) 0.0015(9) C15 0.0317(12) 0.0381(12) 0.0228(11) 0.0010(10) 0.0074(9) 0.0073(10) C16 0.0283(12) 0.0353(12) 0.0360(13) 0.0092(10) 0.0166(10) 0.0059(10) C17 0.0266(12) 0.0323(12) 0.0405(13) 0.0010(10) 0.0114(10) -0.0028(10) C18 0.0262(11) 0.0271(11) 0.0265(11) 0.0005(9) 0.0067(9) 0.0017(9) 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' Al Al 0.0645 0.0514 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C19 O1 Li1 109.22(16) C26 O1 C19 113.06(18) C26 O1 Li1 108.58(16) C20 O2 C21 115.67(18) C20 O2 Li1 110.09(17) C21 O2 Li1 109.25(16) C22 O3 C23 111.86(18) C22 O3 C23A 127.3(6) C22 O3 Li1 109.51(16) C23 O3 Li1 107.67(18) C23A O3 Li1 116.3(5) C25 O4 Li1 112.86(17) C24 O4 C25 114.7(2) C24 O4 Li1 108.71(19) C27 O5 C28 111.6(3) C27 O5 Li1 122.5(3) C28 O5 Li1 125.1(2) C29 O6 C30 108.5(3) C25 O4A Li1 115.4(5) C24A O4A C25 115.1(7) C24A O4A Li1 120.8(6) C27A O5A C28A 114.3(12) C27A O5A Li1 124.9(12) C28A O5A Li1 112.4(10) C29A O6A C30A 120.5(13) C29A O6A Li1 106.7(10) C30A O6A Li1 124.8(10) O1 C19 C20 106.7(2) O2 C20 C19 110.5(2) O2 C21 C22 105.43(18) O3 C22 C21 110.13(18) O4 C25 C26 102.98(19) O4A C25 C26 113.8(4) O1 C26 C25 110.60(18) O3 C23 C24 105.9(2) O4 C24 C23 110.0(2) O5 C28 C29 109.3(3) O6 C29 C28 107.7(2) O3 C23A C24A 94.9(7) O4A C24A C23A 105.6(9) O5A C28A C29A 109.5(14) O6A C29A C28A 111.6(14) O1 Li1 O6A 106.9(3) O2 Li1 O1 79.28(13) O2 Li1 O3 79.66(14) O2 Li1 O6A 165.0(3) O3 Li1 O1 133.07(18) O3 Li1 O6A 104.1(3) O4 Li1 O1 78.23(13) O4 Li1 O2 127.15(19) O4 Li1 O3 82.03(14) O5 Li1 O1 113.9(2) O5 Li1 O2 97.20(16) O5 Li1 O3 109.99(19) O5 Li1 O4 135.6(2) O4A Li1 O1 79.2(2) O4A Li1 O2 110.2(3) O4A Li1 O3 69.7(2) O4A Li1 O5A 164.1(4) O4A Li1 O6A 84.6(4) O5A Li1 O1 105.1(5) O5A Li1 O2 85.7(3) O5A Li1 O3 114.5(5) O5A Li1 O6A 79.6(4) C7 Al1 C1 110.91(9) C13 Al1 C1 109.69(9) C13 Al1 C7 109.55(9) C2 C1 Al1 122.20(17) C6 C1 Al1 123.14(18) C6 C1 C2 114.7(2) C3 C2 C1 123.6(2) C4 C3 C2 119.5(3) C5 C4 C3 119.5(2) C4 C5 C6 119.8(2) C5 C6 C1 122.9(2) C8 C7 Al1 125.78(16) C12 C7 Al1 119.11(16) C12 C7 C8 115.06(19) C9 C8 C7 122.5(2) C10 C9 C8 120.0(2) C11 C10 C9 119.5(2) C10 C11 C12 119.7(2) C11 C12 C7 123.2(2) C14 C13 Al1 123.24(16) C18 C13 Al1 121.80(16) C18 C13 C14 114.93(19) C15 C14 C13 122.8(2) C16 C15 C14 120.1(2) C15 C16 C17 119.3(2) C16 C17 C18 119.9(2) C17 C18 C13 122.9(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C19 1.439(3) O1 C26 1.429(3) O1 Li1 2.163(4) O2 C20 1.430(3) O2 C21 1.439(3) O2 Li1 2.101(4) O3 C22 1.433(3) O3 C23 1.468(3) O3 C23A 1.435(4) O3 Li1 2.111(4) O4 C25 1.456(3) O4 C24 1.434(3) O4 Li1 2.050(4) O5 C27 1.424(3) O5 C28 1.435(3) O5 Li1 1.967(5) O6 C29 1.408(3) O6 C30 1.422(4) O4A C25 1.433(4) O4A C24A 1.355(14) O4A Li1 2.025(9) O5A C27A 1.420(5) O5A C28A 1.424(5) O5A Li1 2.091(15) O6A C29A 1.422(5) O6A C30A 1.427(5) O6A Li1 2.203(12) C19 C20 1.497(4) C21 C22 1.499(3) C25 C26 1.494(3) C23 C24 1.504(4) C28 C29 1.495(4) C23A C24A 1.498(6) C28A C29A 1.496(6) Al1 C1 2.021(2) Al1 C7 2.011(2) Al1 C13 2.008(2) C1 C2 1.406(3) C1 C6 1.405(3) C2 C3 1.390(3) C3 C4 1.388(4) C4 C5 1.384(4) C5 C6 1.399(4) C7 C8 1.408(3) C7 C12 1.403(3) C8 C9 1.395(3) C9 C10 1.384(4) C10 C11 1.383(4) C11 C12 1.389(3) C13 C14 1.406(3) C13 C18 1.403(3) C14 C15 1.392(3) C15 C16 1.379(3) C16 C17 1.383(3) C17 C18 1.394(3) loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion O1 C19 C20 O2 -55.3(3) O2 C21 C22 O3 -55.9(2) O3 C23 C24 O4 -56.8(3) O3 C23A C24A O4A 55.7(10) O4 C25 C26 O1 -55.9(2) O5 C28 C29 O6 -70.5(4) O4A C25 C26 O1 -30.9(5) O5A C28A C29A O6A -51(2) C19 O1 C26 C25 -83.2(2) C20 O2 C21 C22 172.06(19) C21 O2 C20 C19 -84.1(3) C22 O3 C23 C24 162.1(2) C22 O3 C23A C24A 93.6(8) C25 O4 C24 C23 -85.1(3) C25 O4A C24A C23A 171.6(7) C26 O1 C19 C20 162.8(2) C23 O3 C22 C21 -82.8(3) C23 O3 C23A C24A 25.7(7) C24 O4 C25 O4A 54.7(9) C24 O4 C25 C26 173.0(2) C27 O5 C28 C29 -178.0(3) C30 O6 C29 C28 -176.0(3) C23A O3 C22 C21 -113.1(6) C23A O3 C23 C24 -70.4(11) C24A O4A C25 O4 -135.2(15) C24A O4A C25 C26 155.0(8) C27A O5A C28A C29A -174.6(17) C30A O6A C29A C28A -169.9(16) Li1 O1 C19 C20 41.8(2) Li1 O1 C26 C25 38.2(2) Li1 O2 C20 C19 40.3(3) Li1 O2 C21 C22 47.2(2) Li1 O3 C22 C21 36.5(2) Li1 O3 C23 C24 41.7(3) Li1 O3 C23A C24A -54.2(9) Li1 O4 C25 O4A -70.5(9) Li1 O4 C25 C26 47.8(2) Li1 O4 C24 C23 42.3(3) Li1 O5 C28 C29 11.8(4) Li1 O4A C25 O4 76.7(9) Li1 O4A C25 C26 7.0(7) Li1 O4A C24A C23A -42.2(11) Li1 O5A C28A C29A 35.4(18) Li1 O6A C29A C28A 39.8(17) Al1 C1 C2 C3 -179.77(18) Al1 C1 C6 C5 179.59(18) Al1 C7 C8 C9 177.44(16) Al1 C7 C12 C11 -176.99(17) Al1 C13 C14 C15 177.44(17) Al1 C13 C18 C17 -177.62(17) C1 C2 C3 C4 0.0(4) C2 C1 C6 C5 -0.2(3) C2 C3 C4 C5 0.2(4) C3 C4 C5 C6 -0.4(4) C4 C5 C6 C1 0.4(4) C6 C1 C2 C3 0.1(3) C7 C8 C9 C10 -0.8(3) C8 C7 C12 C11 0.5(3) C8 C9 C10 C11 0.8(3) C9 C10 C11 C12 -0.2(3) C10 C11 C12 C7 -0.5(3) C12 C7 C8 C9 0.2(3) C13 C14 C15 C16 0.5(3) C14 C13 C18 C17 0.3(3) C14 C15 C16 C17 -0.5(3) C15 C16 C17 C18 0.3(3) C16 C17 C18 C13 -0.2(3) C18 C13 C14 C15 -0.4(3)