#------------------------------------------------------------------------------ #$Date: 2018-01-17 04:10:52 +0200 (Wed, 17 Jan 2018) $ #$Revision: 205286 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/11/7121146.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_7121146 loop_ _publ_author_name 'Pollard, Victoria A.' 'Orr, Samantha A.' 'McLellan, Ross' 'Kennedy, Alan R.' 'Hevia, Eva' 'Mulvey, Robert E.' _publ_section_title ; Lithium diamidodihydridoaluminates: bimetallic cooperativity in catalytic hydroboration and metallation applications ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C7CC08214B _journal_year 2018 _chemical_formula_moiety 'C24 H62 Al Li N2 O3 Si4' _chemical_formula_sum 'C24 H62 Al Li N2 O3 Si4' _chemical_formula_weight 573.03 _chemical_name_systematic ; ? ; _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' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary iterative _audit_creation_date 2016-12-15 _audit_creation_method ; Olex2 1.2 (compiled 2016.11.24 svn.r3356 for OlexSys, GUI svn.r5267) ; _audit_update_record ; 2017-10-12 deposited with the CCDC. 2017-11-29 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.154(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.1211(7) _cell_length_b 11.6571(5) _cell_length_c 16.3906(6) _cell_measurement_reflns_used 10447 _cell_measurement_temperature 151.4 _cell_measurement_theta_max 29.4255 _cell_measurement_theta_min 3.0145 _cell_volume 3653.4(2) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'olex2.refine (Bourhis et al., 2015)' _computing_structure_solution 'olex2.solve (Bourhis et al., 2015)' _diffrn_ambient_temperature 151.4 _diffrn_detector_area_resol_mean 16.0727 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -6.00 75.00 1.0000 50.0300 omega____ theta____ kappa____ phi______ frames - 19.3443 -122.0000 62.0000 81 #__ type_ start__ end____ width___ exp.time_ 2 omega -6.00 86.00 1.0000 50.0300 omega____ theta____ kappa____ phi______ frames - 19.3443 37.0000 -90.0000 92 #__ type_ start__ end____ width___ exp.time_ 3 omega -53.00 45.00 1.0000 50.0300 omega____ theta____ kappa____ phi______ frames - 19.3443 -37.0000 90.0000 98 #__ type_ start__ end____ width___ exp.time_ 4 omega 65.00 93.00 1.0000 50.0300 omega____ theta____ kappa____ phi______ frames - 19.3443 -151.0000 -124.0000 28 #__ type_ start__ end____ width___ exp.time_ 5 omega -87.00 -9.00 1.0000 50.0300 omega____ theta____ kappa____ phi______ frames - -20.1256 142.0000 -125.0000 78 #__ type_ start__ end____ width___ exp.time_ 6 omega -11.00 89.00 1.0000 50.0300 omega____ theta____ kappa____ phi______ frames - 19.3443 77.0000 60.0000 100 ; _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0081787000 _diffrn_orient_matrix_UB_12 0.0553266000 _diffrn_orient_matrix_UB_13 -0.0152293000 _diffrn_orient_matrix_UB_21 0.0359904000 _diffrn_orient_matrix_UB_22 0.0148280000 _diffrn_orient_matrix_UB_23 0.0008226000 _diffrn_orient_matrix_UB_31 0.0037633000 _diffrn_orient_matrix_UB_32 -0.0204669000 _diffrn_orient_matrix_UB_33 -0.0405061000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_unetI/netI 0.0425 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 36740 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.000 _diffrn_reflns_theta_min 3.021 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.211 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.86880 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.042 _exptl_crystal_description plate _exptl_crystal_F_000 1264 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.440 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.047 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 376 _refine_ls_number_reflns 8703 _refine_ls_number_restraints 150 _refine_ls_restrained_S_all 1.013 _refine_ls_R_factor_all 0.0801 _refine_ls_R_factor_gt 0.0527 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+1.9900P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1181 _refine_ls_wR_factor_ref 0.1345 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6410 _reflns_number_total 8703 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; REM REM R1 = 0.0527 for 6410 Fo > 4sig(Fo) and 0.0801 for all 8703 data REM 376 parameters refined using 150 restraints REM Highest difference peak 0.440, deepest hole -0.464, 1-sigma level 0.047 TITL CELL 0.71073 19.1211 11.6571 16.3906 90.000 90.154 90.000 ZERR 4.0000 0.0007 0.0005 0.0006 0.000 0.003 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H AL LI N O SI UNIT 96 248 4 4 8 12 16 MERG 2 OMIT -3 56 FMAP 2 GRID PLAN 20 TEMP -123 TWIN 1.00 0.00 0.00 0.00 -1.00 0.00 0.00 0.00 -1.00 2 DFIX 1.53 .01 C15 C16 C15 C14 c13 c14 DFIX 1.53 .01 C15a C16a C15a C14a c13a c14a DFIX 1.53 .01 C23 C24 C23 C22 c22 c21 DFIX 1.53 .01 C23a C24a C23a C22a c22a c21a DFIX 1.53 .01 c17 c18 c18 c19 c19 c20 DFIX 1.53 .01 c17a c18a c18a c19a c19a c20a DFIX 1.43 .01 o1 c13 o1 c16 o1 c13a o1 c16a DFIX 1.43 .01 o2 c17 o2 c20 o2 c17a o2 c20a DFIX 1.43 .01 o3 c21 o3 c24 o3 c21a o3 c24a EADP C13 C13a EADP C14 C14a EADP C15 C15a EADP C16 C16a EADP C17 C17a EADP C18 C18a EADP C19 C19a EADP C20 C20a EADP C21 C21a EADP C22 C22a EADP C23 C23a EADP C24 C24a DELU 0.010 0.010 O2 C17 C18 C19 C20 SIMU 0.020 0.020 1.700 O2 C17 C18 C19 C20 DELU 0.010 0.010 O1 C13 C14 C15 C16 SIMU 0.020 0.020 1.700 O1 C13 C14 C15 C16 DELU 0.010 0.010 O3 C21 C22 C23 C24 SIMU 0.020 0.020 1.700 O3 C21 C22 C23 C24 BOND $H CONF L.S. 16 ACTA WGHT 0.054000 1.990000 BASF 0.04681 FVAR 2.81408 0.68818 0.68046 0.51459 LI1 4 0.743946 0.260152 0.378916 11.00000 0.03998 0.03631 = 0.04151 -0.00053 0.00336 -0.00001 AL1 3 0.746828 0.519460 0.291983 11.00000 0.02612 0.02762 = 0.03633 -0.00351 -0.00141 0.00219 SI1 7 0.904008 0.532615 0.268477 11.00000 0.03109 0.04586 = 0.05248 0.00318 0.01683 0.00217 SI2 7 0.843955 0.691693 0.392628 11.00000 0.02857 0.03013 = 0.03850 0.00116 -0.00261 -0.00577 SI3 7 0.649728 0.705404 0.224022 11.00000 0.05614 0.04370 = 0.05030 -0.00638 -0.02084 0.01631 SI4 7 0.600681 0.556674 0.362203 11.00000 0.03142 0.04572 = 0.10270 0.00114 0.01862 0.00165 O1 6 0.818400 0.235376 0.456321 11.00000 0.04490 0.04896 = 0.05658 0.01524 -0.01135 -0.00921 O3 6 0.665692 0.188025 0.431025 11.00000 0.05355 0.04820 = 0.05851 -0.01091 0.01522 -0.02061 O2 6 0.758512 0.165831 0.283540 11.00000 0.05952 0.04239 = 0.03988 -0.00234 0.00184 0.01402 N1 5 0.832675 0.587355 0.319854 11.00000 0.02432 0.03037 = 0.03351 0.00073 0.00438 -0.00140 N2 5 0.665490 0.607157 0.300277 11.00000 0.02738 0.02936 = 0.04955 -0.00763 -0.00564 0.00394 C4 1 0.909074 0.803840 0.361065 11.00000 0.04731 0.03874 = 0.08958 0.00183 0.00624 -0.01386 AFIX 137 H4A 2 0.954942 0.768021 0.353288 11.00000 -1.50000 H4B 2 0.912454 0.862658 0.403613 11.00000 -1.50000 H4C 2 0.893791 0.839331 0.309833 11.00000 -1.50000 AFIX 0 C5 1 0.763868 0.777779 0.414568 11.00000 0.04202 0.04769 = 0.05943 -0.02220 -0.00098 -0.00125 AFIX 137 H5A 2 0.747468 0.814479 0.364241 11.00000 -1.50000 H5B 2 0.774885 0.836790 0.455202 11.00000 -1.50000 H5C 2 0.727204 0.727265 0.435779 11.00000 -1.50000 AFIX 0 C1 1 0.893079 0.378062 0.239185 11.00000 0.04218 0.05544 = 0.05475 -0.00988 0.01205 0.01251 AFIX 137 H1A 2 0.875913 0.334532 0.286200 11.00000 -1.50000 H1B 2 0.938238 0.346842 0.221819 11.00000 -1.50000 H1C 2 0.859376 0.372077 0.194236 11.00000 -1.50000 AFIX 0 C6 1 0.871717 0.630993 0.493285 11.00000 0.07811 0.04532 = 0.04606 -0.00186 -0.01896 -0.00385 AFIX 137 H6A 2 0.835691 0.578263 0.513227 11.00000 -1.50000 H6B 2 0.878102 0.693482 0.532602 11.00000 -1.50000 H6C 2 0.915901 0.589435 0.486756 11.00000 -1.50000 AFIX 0 C2 1 0.921728 0.613630 0.172192 11.00000 0.10764 0.08215 = 0.08658 0.02517 0.06797 0.01876 AFIX 137 H2A 2 0.881047 0.608087 0.135910 11.00000 -1.50000 H2B 2 0.962728 0.580872 0.145036 11.00000 -1.50000 H2C 2 0.930692 0.694369 0.185192 11.00000 -1.50000 AFIX 0 C7 1 0.620092 0.849114 0.261022 11.00000 0.06252 0.04322 = 0.09161 -0.00556 -0.02447 0.01759 AFIX 137 H7A 2 0.577008 0.840280 0.292656 11.00000 -1.50000 H7B 2 0.611224 0.899361 0.214187 11.00000 -1.50000 H7C 2 0.656512 0.883012 0.295611 11.00000 -1.50000 AFIX 0 C3 1 0.987308 0.531874 0.329842 11.00000 0.02473 0.07419 = 0.12204 -0.01825 0.00150 0.00389 AFIX 137 H3A 2 1.000993 0.610950 0.342422 11.00000 -1.50000 H3B 2 1.024426 0.494719 0.298309 11.00000 -1.50000 H3C 2 0.979894 0.489568 0.380757 11.00000 -1.50000 AFIX 0 C11 1 0.567286 0.414086 0.326618 11.00000 0.04408 0.06599 = 0.16971 0.00739 -0.02333 -0.02237 AFIX 137 H11A 2 0.547111 0.422111 0.271888 11.00000 -1.50000 H11B 2 0.531310 0.386569 0.364328 11.00000 -1.50000 H11C 2 0.605963 0.358979 0.325020 11.00000 -1.50000 AFIX 0 C8 1 0.731176 0.733130 0.164064 11.00000 0.11226 0.08963 = 0.06044 0.03878 0.01715 0.03887 AFIX 137 H8A 2 0.769275 0.753888 0.201353 11.00000 -1.50000 H8B 2 0.722905 0.796200 0.125701 11.00000 -1.50000 H8C 2 0.743990 0.663819 0.133749 11.00000 -1.50000 AFIX 0 C12 1 0.521872 0.653640 0.366666 11.00000 0.06624 0.09672 = 0.25254 0.04376 0.08251 0.03465 AFIX 137 H12A 2 0.535135 0.727006 0.391465 11.00000 -1.50000 H12B 2 0.485325 0.617291 0.399549 11.00000 -1.50000 H12C 2 0.504190 0.667026 0.311304 11.00000 -1.50000 AFIX 0 C10 1 0.630980 0.541308 0.470001 11.00000 0.12072 0.06457 = 0.07838 -0.00089 0.05433 -0.02180 AFIX 137 H10A 2 0.674506 0.496951 0.471345 11.00000 -1.50000 H10B 2 0.595109 0.501433 0.501818 11.00000 -1.50000 H10C 2 0.639234 0.617471 0.493437 11.00000 -1.50000 AFIX 0 C9 1 0.580634 0.655829 0.150846 11.00000 0.14567 0.08640 = 0.11767 -0.03494 -0.09423 0.03463 AFIX 137 H9A 2 0.595346 0.583627 0.125525 11.00000 -1.50000 H9B 2 0.573731 0.714087 0.108477 11.00000 -1.50000 H9C 2 0.536681 0.643839 0.180255 11.00000 -1.50000 PART 1 AFIX 0 C13 1 0.834390 0.125565 0.492023 21.00000 0.06145 0.05328 = 0.04755 0.01266 -0.00650 0.00205 AFIX 23 H13A 2 0.816351 0.061761 0.458111 21.00000 -1.20000 H13B 2 0.815201 0.118923 0.547863 21.00000 -1.20000 AFIX 0 C14 1 0.914216 0.128118 0.492843 21.00000 0.06329 0.05667 = 0.06462 0.00825 -0.00241 0.01817 AFIX 23 H14A 2 0.931813 0.116153 0.549062 21.00000 -1.20000 H14B 2 0.932885 0.066189 0.457773 21.00000 -1.20000 AFIX 0 C15 1 0.937723 0.243234 0.461424 21.00000 0.04622 0.06664 = 0.07330 0.00716 -0.00578 -0.00112 AFIX 23 H15A 2 0.951107 0.238861 0.403202 21.00000 -1.20000 H15B 2 0.977766 0.272986 0.493461 21.00000 -1.20000 AFIX 0 C16 1 0.873037 0.317575 0.473018 21.00000 0.05167 0.04208 = 0.04147 -0.01620 0.00115 -0.00130 AFIX 23 H16A 2 0.869993 0.347764 0.529352 21.00000 -1.20000 H16B 2 0.871930 0.382247 0.433887 21.00000 -1.20000 AFIX 0 C17 1 0.723983 0.186349 0.206100 31.00000 0.06646 0.04555 = 0.05034 -0.00150 -0.01142 0.00807 AFIX 23 H17A 2 0.739052 0.260867 0.183115 31.00000 -1.20000 H17B 2 0.672629 0.188198 0.213517 31.00000 -1.20000 AFIX 0 C18 1 0.743996 0.090079 0.149665 31.00000 0.05403 0.07896 = 0.05099 -0.01640 -0.01007 0.00316 AFIX 23 H18A 2 0.744980 0.114947 0.091927 31.00000 -1.20000 H18B 2 0.712661 0.022989 0.155503 31.00000 -1.20000 AFIX 0 C19 1 0.818075 0.065694 0.183254 31.00000 0.05750 0.06861 = 0.05199 -0.01653 0.00282 0.01371 AFIX 23 H19A 2 0.834481 -0.011585 0.167146 31.00000 -1.20000 H19B 2 0.852064 0.123756 0.164105 31.00000 -1.20000 AFIX 0 C20 1 0.807286 0.073581 0.274207 31.00000 0.06459 0.03926 = 0.05022 -0.00330 0.00123 0.01254 AFIX 23 H20A 2 0.787892 0.001103 0.296040 31.00000 -1.20000 H20B 2 0.851822 0.090747 0.302627 31.00000 -1.20000 AFIX 0 C21 1 0.641641 0.079895 0.399350 41.00000 0.05557 0.06311 = 0.09843 -0.02709 0.02151 -0.02880 AFIX 23 H21A 2 0.680711 0.024194 0.398276 41.00000 -1.20000 H21B 2 0.624133 0.089943 0.342903 41.00000 -1.20000 AFIX 0 C22 1 0.584251 0.035967 0.452762 41.00000 0.07781 0.06616 = 0.07781 -0.00892 0.01085 -0.04187 AFIX 23 H22A 2 0.541222 0.021388 0.420675 41.00000 -1.20000 H22B 2 0.598431 -0.035831 0.480504 41.00000 -1.20000 AFIX 0 C23 1 0.573198 0.129384 0.512481 41.00000 0.06278 0.05752 = 0.06194 0.00478 0.01484 -0.01105 AFIX 23 H23A 2 0.562727 0.097594 0.567109 41.00000 -1.20000 H23B 2 0.533872 0.179131 0.495276 41.00000 -1.20000 AFIX 0 C24 1 0.641945 0.197369 0.514148 41.00000 0.08701 0.05435 = 0.06471 -0.01069 0.03015 -0.01490 AFIX 23 H24A 2 0.633857 0.278404 0.529540 41.00000 -1.20000 H24B 2 0.675972 0.162854 0.552595 41.00000 -1.20000 PART 2 AFIX 0 C13A 1 0.833783 0.131963 0.500117 -21.00000 0.06145 0.05328 = 0.04755 0.01266 -0.00650 0.00205 AFIX 23 H13C 2 0.805021 0.069119 0.477122 -21.00000 -1.20000 H13D 2 0.819707 0.142372 0.557725 -21.00000 -1.20000 AFIX 0 C14A 1 0.910599 0.095532 0.498057 -21.00000 0.06329 0.05667 = 0.06462 0.00825 -0.00241 0.01817 AFIX 23 H14C 2 0.924013 0.044690 0.543880 -21.00000 -1.20000 H14D 2 0.924831 0.061648 0.445263 -21.00000 -1.20000 AFIX 0 C15A 1 0.934930 0.218646 0.509116 -21.00000 0.04622 0.06664 = 0.07330 0.00716 -0.00578 -0.00112 AFIX 23 H15C 2 0.983987 0.227709 0.491065 -21.00000 -1.20000 H15D 2 0.931419 0.242242 0.566983 -21.00000 -1.20000 AFIX 0 C16A 1 0.885823 0.289192 0.455970 -21.00000 0.05167 0.04208 = 0.04147 -0.01620 0.00115 -0.00130 AFIX 23 H16C 2 0.882210 0.368280 0.477560 -21.00000 -1.20000 H16D 2 0.904015 0.293165 0.399549 -21.00000 -1.20000 AFIX 0 C17A 1 0.716333 0.171095 0.210754 -31.00000 0.06646 0.04555 = 0.05034 -0.00150 -0.01142 0.00807 AFIX 23 H17C 2 0.705476 0.251306 0.195439 -31.00000 -1.20000 H17D 2 0.672187 0.127671 0.217105 -31.00000 -1.20000 AFIX 0 C18A 1 0.764658 0.114470 0.148808 -31.00000 0.05403 0.07896 = 0.05099 -0.01640 -0.01007 0.00316 AFIX 23 H18C 2 0.798875 0.170403 0.127181 -31.00000 -1.20000 H18D 2 0.737512 0.082088 0.102735 -31.00000 -1.20000 AFIX 0 C19A 1 0.801659 0.019379 0.196664 -31.00000 0.05750 0.06861 = 0.05199 -0.01653 0.00282 0.01371 AFIX 23 H19C 2 0.770685 -0.046938 0.207432 -31.00000 -1.20000 H19D 2 0.845051 -0.006833 0.169630 -31.00000 -1.20000 AFIX 0 C20A 1 0.816335 0.089190 0.272995 -31.00000 0.06459 0.03926 = 0.05022 -0.00330 0.00123 0.01254 AFIX 23 H20C 2 0.820960 0.038051 0.320929 -31.00000 -1.20000 H20D 2 0.860347 0.133021 0.266780 -31.00000 -1.20000 AFIX 0 C21A 1 0.623295 0.095641 0.399556 -41.00000 0.05557 0.06311 = 0.09843 -0.02709 0.02151 -0.02880 AFIX 23 H21C 2 0.649535 0.047477 0.360424 -41.00000 -1.20000 H21D 2 0.580115 0.124505 0.373165 -41.00000 -1.20000 AFIX 0 C23A 1 0.613827 0.113594 0.548017 -41.00000 0.06278 0.05752 = 0.06194 0.00478 0.01484 -0.01105 AFIX 23 H23C 2 0.651055 0.089552 0.586471 -41.00000 -1.20000 H23D 2 0.569074 0.120642 0.577834 -41.00000 -1.20000 AFIX 0 C22A 1 0.607579 0.031636 0.477375 -41.00000 0.07781 0.06616 = 0.07781 -0.00892 0.01085 -0.04187 AFIX 23 H22C 2 0.559694 -0.000516 0.475062 -41.00000 -1.20000 H22D 2 0.640978 -0.032540 0.484328 -41.00000 -1.20000 AFIX 0 C24A 1 0.632797 0.225137 0.504842 -41.00000 0.08701 0.05435 = 0.06471 -0.01069 0.03015 -0.01490 AFIX 23 H24C 2 0.590462 0.271145 0.492945 -41.00000 -1.20000 H24D 2 0.665309 0.271555 0.538406 -41.00000 -1.20000 PART 0 AFIX 0 H 2 0.736510 0.411833 0.352102 11.00000 0.04712 HA 2 0.750706 0.469547 0.204732 11.00000 0.04907 HKLF 4 REM REM R1 = 0.0527 for 6410 Fo > 4sig(Fo) and 0.0801 for all 8703 data REM 376 parameters refined using 150 restraints END WGHT 0.0539 1.9915 REM Highest difference peak 0.440, deepest hole -0.465, 1-sigma level 0.047 Q1 1 0.6208 0.6716 0.2514 11.00000 0.05 0.44 Q2 1 0.6069 0.5361 0.4082 11.00000 0.05 0.44 Q3 1 0.5751 0.0803 0.4834 11.00000 0.05 0.33 Q4 1 0.6667 0.0526 0.4554 11.00000 0.05 0.29 Q5 1 0.9033 0.2600 0.4312 11.00000 0.05 0.28 Q6 1 0.8271 0.6439 0.3465 11.00000 0.05 0.27 Q7 1 0.6424 0.5728 0.3281 11.00000 0.05 0.27 Q8 1 0.6340 0.0266 0.5034 11.00000 0.05 0.27 Q9 1 0.8647 0.6563 0.4474 11.00000 0.05 0.26 Q10 1 0.8627 0.5569 0.3031 11.00000 0.05 0.26 Q11 1 0.6998 0.5864 0.3004 11.00000 0.05 0.25 Q12 1 0.9323 0.1805 0.5143 11.00000 0.05 0.24 Q13 1 0.8825 0.4402 0.2622 11.00000 0.05 0.24 Q14 1 0.7982 0.1254 0.1467 11.00000 0.05 0.24 Q15 1 0.6698 0.6631 0.2796 11.00000 0.05 0.23 Q16 1 0.8786 0.7565 0.3859 11.00000 0.05 0.23 Q17 1 0.8275 0.1059 0.2284 11.00000 0.05 0.23 Q18 1 0.6962 0.6997 0.1881 11.00000 0.05 0.22 Q19 1 0.5880 0.4902 0.3386 11.00000 0.05 0.22 Q20 1 0.7384 0.4982 0.3479 11.00000 0.05 0.22 ; _cod_data_source_file c7cc08214b2.cif _cod_data_source_block RMSO22 _cod_database_code 7121146 _shelxl_version_number 2013-2 _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. ; _reflns_odcompleteness_completeness 99.79 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 27.01 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.95319 0.04681 2. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 3. Restrained distances C15-C16 = C15-C14 = C13-C14 1.53 with sigma of 0.01 C15A-C16A = C15A-C14A = C13A-C14A 1.53 with sigma of 0.01 C23-C24 = C23-C22 = C22-C21 1.53 with sigma of 0.01 C23A-C24A = C23A-C22A = C22A-C21A 1.53 with sigma of 0.01 C17-C18 = C18-C19 = C19-C20 1.53 with sigma of 0.01 C17A-C18A = C18A-C19A = C19A-C20A 1.53 with sigma of 0.01 O1-C13 = O1-C16 = O1-C13A = O1-C16A 1.43 with sigma of 0.01 O2-C17 = O2-C20 = O2-C17A = O2-C20A 1.43 with sigma of 0.01 O3-C21 = O3-C24 = O3-C21A = O3-C24A 1.43 with sigma of 0.01 4. Rigid bond restraints O2, C17, C18, C19, C20 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 O1, C13, C14, C15, C16 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 O3, C21, C22, C23, C24 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 5. Uiso/Uaniso restraints and constraints O2 \\sim C17 \\sim C18 \\sim C19 \\sim C20: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.02 O1 \\sim C13 \\sim C14 \\sim C15 \\sim C16: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.02 O3 \\sim C21 \\sim C22 \\sim C23 \\sim C24: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.02 Uanis(C13) = Uanis(C13A) Uanis(C14) = Uanis(C14A) Uanis(C15) = Uanis(C15A) Uanis(C16) = Uanis(C16A) Uanis(C17) = Uanis(C17A) Uanis(C18) = Uanis(C18A) Uanis(C19) = Uanis(C19A) Uanis(C20) = Uanis(C20A) Uanis(C21) = Uanis(C21A) Uanis(C22) = Uanis(C22A) Uanis(C23) = Uanis(C23A) Uanis(C24) = Uanis(C24A) 6. Others Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C14A)=Sof(H14C)=Sof(H14D)=Sof(C15A)= Sof(H15C)=Sof(H15D)=Sof(C16A)=Sof(H16C)=Sof(H16D)=1-FVAR(1) Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C15)=Sof(H15A)= Sof(H15B)=Sof(C16)=Sof(H16A)=Sof(H16B)=FVAR(1) Sof(C17A)=Sof(H17C)=Sof(H17D)=Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(C19A)= Sof(H19C)=Sof(H19D)=Sof(C20A)=Sof(H20C)=Sof(H20D)=1-FVAR(2) Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19A)= Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=FVAR(2) Sof(C21A)=Sof(H21C)=Sof(H21D)=Sof(C23A)=Sof(H23C)=Sof(H23D)=Sof(C22A)= Sof(H22C)=Sof(H22D)=Sof(C24A)=Sof(H24C)=Sof(H24D)=1-FVAR(3) Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)= Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=FVAR(3) 7.a Secondary CH2 refined with riding coordinates: C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A, H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C13A(H13C,H13D), C14A(H14C, H14D), C15A(H15C,H15D), C16A(H16C,H16D), C17A(H17C,H17D), C18A(H18C,H18D), C19A(H19C,H19D), C20A(H20C,H20D), C21A(H21C,H21D), C23A(H23C,H23D), C22A(H22C, H22D), C24A(H24C,H24D) 7.b Idealised Me refined as rotating group: C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C2(H2A, H2B,H2C), C7(H7A,H7B,H7C), C3(H3A,H3B,H3C), C11(H11A,H11B,H11C), C8(H8A,H8B, H8C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C) ; _olex2_submission_original_sample_id RMSO22 _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_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.7439(2) 0.2602(3) 0.3789(2) 0.0393(9) Uani 1 1 d . . . . . Al1 Al 0.74683(3) 0.51946(6) 0.29198(4) 0.03003(15) Uani 1 1 d . . . . . Si1 Si 0.90401(3) 0.53262(6) 0.26848(4) 0.04311(18) Uani 1 1 d . . . . . Si2 Si 0.84395(3) 0.69169(5) 0.39263(4) 0.03241(15) Uani 1 1 d . . . . . Si3 Si 0.64973(4) 0.70540(7) 0.22402(5) 0.0501(2) Uani 1 1 d . . . . . Si4 Si 0.60068(4) 0.55667(7) 0.36220(6) 0.0599(2) Uani 1 1 d . . . . . O1 O 0.81840(9) 0.23538(15) 0.45632(11) 0.0502(4) Uani 1 1 d D U . . . O3 O 0.66569(10) 0.18803(16) 0.43102(11) 0.0534(5) Uani 1 1 d D U . . . O2 O 0.75851(10) 0.16583(15) 0.28354(10) 0.0473(4) Uani 1 1 d D U . . . N1 N 0.83268(9) 0.58735(15) 0.31985(10) 0.0294(4) Uani 1 1 d . . . . . N2 N 0.66549(9) 0.60716(16) 0.30028(12) 0.0354(4) Uani 1 1 d . . . . . C4 C 0.90907(15) 0.8038(2) 0.3611(2) 0.0585(7) Uani 1 1 d . . . . . H4A H 0.9549 0.7680 0.3533 0.088 Uiso 1 1 calc GR . . . . H4B H 0.9125 0.8627 0.4036 0.088 Uiso 1 1 calc GR . . . . H4C H 0.8938 0.8393 0.3098 0.088 Uiso 1 1 calc GR . . . . C5 C 0.76387(13) 0.7778(2) 0.41457(17) 0.0497(6) Uani 1 1 d . . . . . H5A H 0.7475 0.8145 0.3642 0.075 Uiso 1 1 calc GR . . . . H5B H 0.7749 0.8368 0.4552 0.075 Uiso 1 1 calc GR . . . . H5C H 0.7272 0.7273 0.4358 0.075 Uiso 1 1 calc GR . . . . C1 C 0.89308(14) 0.3781(2) 0.23919(17) 0.0508(7) Uani 1 1 d . . . . . H1A H 0.8759 0.3345 0.2862 0.076 Uiso 1 1 calc GR . . . . H1B H 0.9382 0.3468 0.2218 0.076 Uiso 1 1 calc GR . . . . H1C H 0.8594 0.3721 0.1942 0.076 Uiso 1 1 calc GR . . . . C6 C 0.87172(17) 0.6310(2) 0.49329(16) 0.0565(7) Uani 1 1 d . . . . . H6A H 0.8357 0.5783 0.5132 0.085 Uiso 1 1 calc GR . . . . H6B H 0.8781 0.6935 0.5326 0.085 Uiso 1 1 calc GR . . . . H6C H 0.9159 0.5894 0.4868 0.085 Uiso 1 1 calc GR . . . . C2 C 0.9217(2) 0.6136(3) 0.1722(2) 0.0920(14) Uani 1 1 d . . . . . H2A H 0.8810 0.6081 0.1359 0.138 Uiso 1 1 calc GR . . . . H2B H 0.9627 0.5809 0.1450 0.138 Uiso 1 1 calc GR . . . . H2C H 0.9307 0.6944 0.1852 0.138 Uiso 1 1 calc GR . . . . C7 C 0.62009(17) 0.8491(2) 0.2610(2) 0.0658(9) Uani 1 1 d . . . . . H7A H 0.5770 0.8403 0.2927 0.099 Uiso 1 1 calc GR . . . . H7B H 0.6112 0.8994 0.2142 0.099 Uiso 1 1 calc GR . . . . H7C H 0.6565 0.8830 0.2956 0.099 Uiso 1 1 calc GR . . . . C3 C 0.98731(14) 0.5319(3) 0.3298(2) 0.0737(10) Uani 1 1 d . . . . . H3A H 1.0010 0.6109 0.3424 0.110 Uiso 1 1 calc GR . . . . H3B H 1.0244 0.4947 0.2983 0.110 Uiso 1 1 calc GR . . . . H3C H 0.9799 0.4896 0.3808 0.110 Uiso 1 1 calc GR . . . . C11 C 0.56729(18) 0.4141(3) 0.3266(3) 0.0933(13) Uani 1 1 d . . . . . H11A H 0.5471 0.4221 0.2719 0.140 Uiso 1 1 calc GR . . . . H11B H 0.5313 0.3866 0.3643 0.140 Uiso 1 1 calc GR . . . . H11C H 0.6060 0.3590 0.3250 0.140 Uiso 1 1 calc GR . . . . C8 C 0.7312(2) 0.7331(4) 0.1641(2) 0.0874(12) Uani 1 1 d . . . . . H8A H 0.7693 0.7539 0.2014 0.131 Uiso 1 1 calc GR . . . . H8B H 0.7229 0.7962 0.1257 0.131 Uiso 1 1 calc GR . . . . H8C H 0.7440 0.6638 0.1337 0.131 Uiso 1 1 calc GR . . . . C12 C 0.5219(2) 0.6536(4) 0.3667(4) 0.138(2) Uani 1 1 d . . . . . H12A H 0.5351 0.7270 0.3915 0.208 Uiso 1 1 calc GR . . . . H12B H 0.4853 0.6173 0.3995 0.208 Uiso 1 1 calc GR . . . . H12C H 0.5042 0.6670 0.3113 0.208 Uiso 1 1 calc GR . . . . C10 C 0.6310(2) 0.5413(3) 0.4700(2) 0.0878(13) Uani 1 1 d . . . . . H10A H 0.6745 0.4970 0.4713 0.132 Uiso 1 1 calc GR . . . . H10B H 0.5951 0.5014 0.5018 0.132 Uiso 1 1 calc GR . . . . H10C H 0.6392 0.6175 0.4934 0.132 Uiso 1 1 calc GR . . . . C9 C 0.5806(3) 0.6558(4) 0.1508(3) 0.1167(19) Uani 1 1 d . . . . . H9A H 0.5953 0.5836 0.1255 0.175 Uiso 1 1 calc GR . . . . H9B H 0.5737 0.7141 0.1085 0.175 Uiso 1 1 calc GR . . . . H9C H 0.5367 0.6438 0.1803 0.175 Uiso 1 1 calc GR . . . . C13 C 0.8344(7) 0.1256(11) 0.4920(13) 0.0541(19) Uani 0.688(6) 1 d D U P A 1 H13A H 0.8164 0.0618 0.4581 0.065 Uiso 0.688(6) 1 calc R . P A 1 H13B H 0.8152 0.1189 0.5479 0.065 Uiso 0.688(6) 1 calc R . P A 1 C14 C 0.9142(6) 0.1281(5) 0.4928(8) 0.0615(14) Uani 0.688(6) 1 d D U P A 1 H14A H 0.9318 0.1162 0.5491 0.074 Uiso 0.688(6) 1 calc R . P A 1 H14B H 0.9329 0.0662 0.4578 0.074 Uiso 0.688(6) 1 calc R . P A 1 C15 C 0.9377(2) 0.2432(4) 0.4614(4) 0.0621(12) Uani 0.688(6) 1 d D U P A 1 H15A H 0.9511 0.2389 0.4032 0.074 Uiso 0.688(6) 1 calc R . P A 1 H15B H 0.9778 0.2730 0.4935 0.074 Uiso 0.688(6) 1 calc R . P A 1 C16 C 0.8730(2) 0.3176(4) 0.4730(3) 0.0451(10) Uani 0.688(6) 1 d D U P A 1 H16A H 0.8700 0.3478 0.5294 0.054 Uiso 0.688(6) 1 calc R . P A 1 H16B H 0.8719 0.3822 0.4339 0.054 Uiso 0.688(6) 1 calc R . P A 1 C17 C 0.7240(6) 0.1863(11) 0.2061(5) 0.0541(18) Uani 0.680(11) 1 d D U P B 1 H17A H 0.7391 0.2609 0.1831 0.065 Uiso 0.680(11) 1 calc R . P B 1 H17B H 0.6726 0.1882 0.2135 0.065 Uiso 0.680(11) 1 calc R . P B 1 C18 C 0.7440(4) 0.0901(7) 0.1497(5) 0.0613(17) Uani 0.680(11) 1 d D U P B 1 H18A H 0.7450 0.1149 0.0919 0.074 Uiso 0.680(11) 1 calc R . P B 1 H18B H 0.7127 0.0230 0.1555 0.074 Uiso 0.680(11) 1 calc R . P B 1 C19 C 0.8181(3) 0.0657(8) 0.1833(4) 0.0594(16) Uani 0.680(11) 1 d D U P B 1 H19A H 0.8345 -0.0116 0.1671 0.071 Uiso 0.680(11) 1 calc R . P B 1 H19B H 0.8521 0.1238 0.1641 0.071 Uiso 0.680(11) 1 calc R . P B 1 C20 C 0.8073(5) 0.0736(8) 0.2742(5) 0.0514(16) Uani 0.680(11) 1 d D U P B 1 H20A H 0.7879 0.0011 0.2960 0.062 Uiso 0.680(11) 1 calc R . P B 1 H20B H 0.8518 0.0907 0.3026 0.062 Uiso 0.680(11) 1 calc R . P B 1 C21 C 0.6416(6) 0.0799(10) 0.3993(9) 0.072(2) Uani 0.515(5) 1 d D U P C 1 H21A H 0.6807 0.0242 0.3983 0.087 Uiso 0.515(5) 1 calc R . P C 1 H21B H 0.6241 0.0899 0.3429 0.087 Uiso 0.515(5) 1 calc R . P C 1 C22 C 0.5843(5) 0.0360(9) 0.4528(6) 0.074(2) Uani 0.515(5) 1 d D U P C 1 H22A H 0.5412 0.0214 0.4207 0.089 Uiso 0.515(5) 1 calc R . P C 1 H22B H 0.5984 -0.0358 0.4805 0.089 Uiso 0.515(5) 1 calc R . P C 1 C23 C 0.5732(4) 0.1294(5) 0.5125(4) 0.0607(12) Uani 0.515(5) 1 d D U P C 1 H23A H 0.5627 0.0976 0.5671 0.073 Uiso 0.515(5) 1 calc R . P C 1 H23B H 0.5339 0.1791 0.4953 0.073 Uiso 0.515(5) 1 calc R . P C 1 C24 C 0.6419(7) 0.1974(10) 0.5141(6) 0.069(2) Uani 0.515(5) 1 d D U P C 1 H24A H 0.6339 0.2784 0.5295 0.082 Uiso 0.515(5) 1 calc R . P C 1 H24B H 0.6760 0.1629 0.5526 0.082 Uiso 0.515(5) 1 calc R . P C 1 C13A C 0.8338(17) 0.132(3) 0.500(3) 0.0541(19) Uani 0.312(6) 1 d D . P A 2 H13C H 0.8050 0.0691 0.4771 0.065 Uiso 0.312(6) 1 calc R . P A 2 H13D H 0.8197 0.1424 0.5577 0.065 Uiso 0.312(6) 1 calc R . P A 2 C14A C 0.9106(15) 0.0955(13) 0.498(2) 0.0615(14) Uani 0.312(6) 1 d D . P A 2 H14C H 0.9240 0.0447 0.5439 0.074 Uiso 0.312(6) 1 calc R . P A 2 H14D H 0.9248 0.0616 0.4453 0.074 Uiso 0.312(6) 1 calc R . P A 2 C15A C 0.9349(5) 0.2186(10) 0.5091(8) 0.0621(12) Uani 0.312(6) 1 d D . P A 2 H15C H 0.9840 0.2277 0.4911 0.074 Uiso 0.312(6) 1 calc R . P A 2 H15D H 0.9314 0.2422 0.5670 0.074 Uiso 0.312(6) 1 calc R . P A 2 C16A C 0.8858(5) 0.2892(9) 0.4560(7) 0.0451(10) Uani 0.312(6) 1 d D . P A 2 H16C H 0.8822 0.3683 0.4776 0.054 Uiso 0.312(6) 1 calc R . P A 2 H16D H 0.9040 0.2932 0.3995 0.054 Uiso 0.312(6) 1 calc R . P A 2 C17A C 0.7163(12) 0.171(3) 0.2108(9) 0.0541(18) Uani 0.320(11) 1 d D . P B 2 H17C H 0.7055 0.2513 0.1954 0.065 Uiso 0.320(11) 1 calc R . P B 2 H17D H 0.6722 0.1277 0.2171 0.065 Uiso 0.320(11) 1 calc R . P B 2 C18A C 0.7647(9) 0.1145(14) 0.1488(12) 0.0613(17) Uani 0.320(11) 1 d D . P B 2 H18C H 0.7989 0.1704 0.1272 0.074 Uiso 0.320(11) 1 calc R . P B 2 H18D H 0.7375 0.0821 0.1027 0.074 Uiso 0.320(11) 1 calc R . P B 2 C19A C 0.8017(9) 0.0194(13) 0.1967(9) 0.0594(16) Uani 0.320(11) 1 d D . P B 2 H19C H 0.7707 -0.0469 0.2074 0.071 Uiso 0.320(11) 1 calc R . P B 2 H19D H 0.8451 -0.0068 0.1696 0.071 Uiso 0.320(11) 1 calc R . P B 2 C20A C 0.8163(10) 0.089(2) 0.2730(13) 0.0514(16) Uani 0.320(11) 1 d D . P B 2 H20C H 0.8210 0.0381 0.3209 0.062 Uiso 0.320(11) 1 calc R . P B 2 H20D H 0.8603 0.1330 0.2668 0.062 Uiso 0.320(11) 1 calc R . P B 2 C21A C 0.6233(7) 0.0956(10) 0.3996(8) 0.072(2) Uani 0.485(5) 1 d D . P C 2 H21C H 0.6495 0.0475 0.3604 0.087 Uiso 0.485(5) 1 calc R . P C 2 H21D H 0.5801 0.1245 0.3732 0.087 Uiso 0.485(5) 1 calc R . P C 2 C23A C 0.6138(4) 0.1136(5) 0.5480(4) 0.0607(12) Uani 0.485(5) 1 d D . P C 2 H23C H 0.6511 0.0896 0.5865 0.073 Uiso 0.485(5) 1 calc R . P C 2 H23D H 0.5691 0.1206 0.5778 0.073 Uiso 0.485(5) 1 calc R . P C 2 C22A C 0.6076(6) 0.0316(10) 0.4774(6) 0.074(2) Uani 0.485(5) 1 d D . P C 2 H22C H 0.5597 -0.0005 0.4751 0.089 Uiso 0.485(5) 1 calc R . P C 2 H22D H 0.6410 -0.0325 0.4843 0.089 Uiso 0.485(5) 1 calc R . P C 2 C24A C 0.6328(8) 0.2251(9) 0.5048(6) 0.069(2) Uani 0.485(5) 1 d D . P C 2 H24C H 0.5905 0.2711 0.4929 0.082 Uiso 0.485(5) 1 calc R . P C 2 H24D H 0.6653 0.2716 0.5384 0.082 Uiso 0.485(5) 1 calc R . P C 2 H H 0.7365(13) 0.412(2) 0.3521(15) 0.047(7) Uiso 1 1 d . . . . . HA H 0.7507(13) 0.470(2) 0.2047(15) 0.049(7) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.040(2) 0.036(2) 0.042(2) -0.0005(16) 0.0034(16) 0.0000(17) Al1 0.0261(3) 0.0276(3) 0.0363(3) -0.0035(3) -0.0014(2) 0.0022(3) Si1 0.0311(3) 0.0459(4) 0.0525(4) 0.0032(3) 0.0168(3) 0.0022(3) Si2 0.0286(3) 0.0301(3) 0.0385(3) 0.0012(2) -0.0026(2) -0.0058(2) Si3 0.0561(5) 0.0437(4) 0.0503(4) -0.0064(3) -0.0208(3) 0.0163(3) Si4 0.0314(4) 0.0457(5) 0.1027(7) 0.0011(4) 0.0186(4) 0.0016(3) O1 0.0449(10) 0.0490(11) 0.0566(11) 0.0152(8) -0.0113(8) -0.0092(8) O3 0.0536(11) 0.0482(11) 0.0585(11) -0.0109(8) 0.0152(8) -0.0206(9) O2 0.0595(11) 0.0424(10) 0.0399(9) -0.0023(7) 0.0018(8) 0.0140(8) N1 0.0243(9) 0.0304(10) 0.0335(9) 0.0007(7) 0.0044(7) -0.0014(7) N2 0.0274(9) 0.0294(10) 0.0496(11) -0.0076(8) -0.0056(8) 0.0039(8) C4 0.0473(16) 0.0387(15) 0.090(2) 0.0018(14) 0.0062(14) -0.0139(12) C5 0.0420(14) 0.0477(16) 0.0594(16) -0.0222(12) -0.0010(11) -0.0012(12) C1 0.0422(14) 0.0554(17) 0.0548(15) -0.0099(12) 0.0121(11) 0.0125(12) C6 0.078(2) 0.0453(16) 0.0461(15) -0.0019(12) -0.0190(13) -0.0039(14) C2 0.108(3) 0.082(3) 0.087(2) 0.025(2) 0.068(2) 0.019(2) C7 0.0625(19) 0.0432(17) 0.092(2) -0.0056(15) -0.0245(16) 0.0176(14) C3 0.0247(13) 0.074(2) 0.122(3) -0.018(2) 0.0015(15) 0.0039(14) C11 0.0441(18) 0.066(2) 0.170(4) 0.007(2) -0.023(2) -0.0224(17) C8 0.112(3) 0.090(3) 0.060(2) 0.0388(18) 0.0172(19) 0.039(2) C12 0.066(3) 0.097(3) 0.253(7) 0.044(4) 0.083(3) 0.035(2) C10 0.121(3) 0.065(2) 0.078(2) -0.0009(18) 0.054(2) -0.022(2) C9 0.146(4) 0.086(3) 0.118(3) -0.035(2) -0.094(3) 0.035(3) C13 0.0615(18) 0.053(2) 0.048(4) 0.013(2) -0.0065(19) 0.0020(16) C14 0.063(2) 0.057(4) 0.065(3) 0.008(4) -0.0024(18) 0.018(4) C15 0.046(2) 0.067(3) 0.073(3) 0.007(3) -0.006(2) -0.0011(19) C16 0.052(2) 0.042(3) 0.041(2) -0.0162(17) 0.0011(16) -0.0013(17) C17 0.066(3) 0.046(4) 0.0503(17) -0.0015(17) -0.0114(18) 0.008(2) C18 0.054(4) 0.079(4) 0.0510(18) -0.016(3) -0.010(3) 0.003(3) C19 0.058(3) 0.069(5) 0.052(3) -0.017(3) 0.003(2) 0.014(3) C20 0.065(3) 0.039(3) 0.0502(15) -0.0033(18) 0.0012(17) 0.013(2) C21 0.056(6) 0.063(3) 0.098(3) -0.027(2) 0.022(3) -0.029(4) C22 0.078(6) 0.066(3) 0.078(5) -0.009(3) 0.011(4) -0.042(4) C23 0.063(3) 0.058(3) 0.062(3) 0.005(2) 0.015(2) -0.011(3) C24 0.087(4) 0.054(5) 0.065(3) -0.011(3) 0.030(3) -0.015(3) C13A 0.0615(18) 0.053(2) 0.048(4) 0.013(2) -0.0065(19) 0.0020(16) C14A 0.063(2) 0.057(4) 0.065(3) 0.008(4) -0.0024(18) 0.018(4) C15A 0.046(2) 0.067(3) 0.073(3) 0.007(3) -0.006(2) -0.0011(19) C16A 0.052(2) 0.042(3) 0.041(2) -0.0162(17) 0.0011(16) -0.0013(17) C17A 0.066(3) 0.046(4) 0.0503(17) -0.0015(17) -0.0114(18) 0.008(2) C18A 0.054(4) 0.079(4) 0.0510(18) -0.016(3) -0.010(3) 0.003(3) C19A 0.058(3) 0.069(5) 0.052(3) -0.017(3) 0.003(2) 0.014(3) C20A 0.065(3) 0.039(3) 0.0502(15) -0.0033(18) 0.0012(17) 0.013(2) C21A 0.056(6) 0.063(3) 0.098(3) -0.027(2) 0.022(3) -0.029(4) C23A 0.063(3) 0.058(3) 0.062(3) 0.005(2) 0.015(2) -0.011(3) C22A 0.078(6) 0.066(3) 0.078(5) -0.009(3) 0.011(4) -0.042(4) C24A 0.087(4) 0.054(5) 0.065(3) -0.011(3) 0.030(3) -0.015(3) 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' N N 0.0061 0.0033 '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' Si Si 0.0817 0.0704 '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 O1 Li1 O2 109.9(2) O1 Li1 H 111.1(8) O3 Li1 O1 102.5(2) O3 Li1 O2 103.0(2) O3 Li1 H 118.1(8) O2 Li1 H 111.6(8) N1 Al1 H 106.8(9) N1 Al1 HA 109.9(9) N2 Al1 N1 118.65(8) N2 Al1 H 106.2(9) N2 Al1 HA 108.4(9) H Al1 HA 106.2(13) N1 Si1 C1 113.08(10) N1 Si1 C2 111.71(13) N1 Si1 C3 114.18(12) C1 Si1 C3 103.06(14) C2 Si1 C1 106.81(16) C2 Si1 C3 107.35(19) N1 Si2 C4 112.57(12) N1 Si2 C5 114.40(10) N1 Si2 C6 112.31(11) C5 Si2 C4 102.92(13) C5 Si2 C6 105.33(14) C6 Si2 C4 108.62(14) N2 Si3 C7 114.41(13) N2 Si3 C8 110.60(12) N2 Si3 C9 112.42(17) C7 Si3 C8 105.60(18) C7 Si3 C9 105.67(16) C8 Si3 C9 107.7(2) N2 Si4 C11 111.58(16) N2 Si4 C12 113.43(16) N2 Si4 C10 111.82(14) C11 Si4 C12 105.8(2) C10 Si4 C11 108.32(18) C10 Si4 C12 105.5(2) C13 O1 Li1 123.8(8) C13 O1 C16 111.1(8) C16 O1 Li1 124.0(3) C13A O1 Li1 127.3(19) C13A O1 C16A 100.8(16) C16A O1 Li1 126.5(5) C21 O3 Li1 118.2(5) C21 O3 C24 107.8(7) C24 O3 Li1 129.5(5) C21A O3 Li1 127.3(6) C24A O3 Li1 126.0(5) C24A O3 C21A 106.3(7) C17 O2 Li1 123.3(4) C20 O2 Li1 127.5(4) C20 O2 C17 109.0(6) C17A O2 Li1 124.4(10) C20A O2 Li1 124.4(7) C20A O2 C17A 110.9(12) Si1 N1 Al1 114.63(10) Si2 N1 Al1 125.16(10) Si2 N1 Si1 120.17(10) Si3 N2 Al1 117.12(11) Si4 N2 Al1 117.42(11) Si4 N2 Si3 122.32(11) Si2 C4 H4A 109.5 Si2 C4 H4B 109.5 Si2 C4 H4C 109.5 H4A C4 H4B 109.5 H4A C4 H4C 109.5 H4B C4 H4C 109.5 Si2 C5 H5A 109.5 Si2 C5 H5B 109.5 Si2 C5 H5C 109.5 H5A C5 H5B 109.5 H5A C5 H5C 109.5 H5B C5 H5C 109.5 Si1 C1 H1A 109.5 Si1 C1 H1B 109.5 Si1 C1 H1C 109.5 H1A C1 H1B 109.5 H1A C1 H1C 109.5 H1B C1 H1C 109.5 Si2 C6 H6A 109.5 Si2 C6 H6B 109.5 Si2 C6 H6C 109.5 H6A C6 H6B 109.5 H6A C6 H6C 109.5 H6B C6 H6C 109.5 Si1 C2 H2A 109.5 Si1 C2 H2B 109.5 Si1 C2 H2C 109.5 H2A C2 H2B 109.5 H2A C2 H2C 109.5 H2B C2 H2C 109.5 Si3 C7 H7A 109.5 Si3 C7 H7B 109.5 Si3 C7 H7C 109.5 H7A C7 H7B 109.5 H7A C7 H7C 109.5 H7B C7 H7C 109.5 Si1 C3 H3A 109.5 Si1 C3 H3B 109.5 Si1 C3 H3C 109.5 H3A C3 H3B 109.5 H3A C3 H3C 109.5 H3B C3 H3C 109.5 Si4 C11 H11A 109.5 Si4 C11 H11B 109.5 Si4 C11 H11C 109.5 H11A C11 H11B 109.5 H11A C11 H11C 109.5 H11B C11 H11C 109.5 Si3 C8 H8A 109.5 Si3 C8 H8B 109.5 Si3 C8 H8C 109.5 H8A C8 H8B 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 Si4 C12 H12A 109.5 Si4 C12 H12B 109.5 Si4 C12 H12C 109.5 H12A C12 H12B 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 Si4 C10 H10A 109.5 Si4 C10 H10B 109.5 Si4 C10 H10C 109.5 H10A C10 H10B 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 Si3 C9 H9A 109.5 Si3 C9 H9B 109.5 Si3 C9 H9C 109.5 H9A C9 H9B 109.5 H9A C9 H9C 109.5 H9B C9 H9C 109.5 O1 C13 H13A 111.5 O1 C13 H13B 111.5 O1 C13 C14 101.4(8) H13A C13 H13B 109.3 C14 C13 H13A 111.5 C14 C13 H13B 111.5 C13 C14 H14A 110.0 C13 C14 H14B 110.0 H14A C14 H14B 108.4 C15 C14 C13 108.3(7) C15 C14 H14A 110.0 C15 C14 H14B 110.0 C14 C15 H15A 111.2 C14 C15 H15B 111.2 C14 C15 C16 102.8(5) H15A C15 H15B 109.1 C16 C15 H15A 111.2 C16 C15 H15B 111.2 O1 C16 C15 100.7(3) O1 C16 H16A 111.6 O1 C16 H16B 111.6 C15 C16 H16A 111.6 C15 C16 H16B 111.6 H16A C16 H16B 109.4 O2 C17 H17A 110.2 O2 C17 H17B 110.2 O2 C17 C18 107.4(7) H17A C17 H17B 108.5 C18 C17 H17A 110.2 C18 C17 H17B 110.2 C17 C18 H18A 112.0 C17 C18 H18B 112.0 C17 C18 C19 98.8(7) H18A C18 H18B 109.7 C19 C18 H18A 112.0 C19 C18 H18B 112.0 C18 C19 H19A 111.3 C18 C19 H19B 111.3 H19A C19 H19B 109.2 C20 C19 C18 102.3(6) C20 C19 H19A 111.3 C20 C19 H19B 111.3 O2 C20 C19 104.0(6) O2 C20 H20A 111.0 O2 C20 H20B 111.0 C19 C20 H20A 111.0 C19 C20 H20B 111.0 H20A C20 H20B 109.0 O3 C21 H21A 109.9 O3 C21 H21B 109.9 O3 C21 C22 108.8(8) H21A C21 H21B 108.3 C22 C21 H21A 109.9 C22 C21 H21B 109.9 C21 C22 H22A 111.0 C21 C22 H22B 111.0 H22A C22 H22B 109.0 C23 C22 C21 104.0(7) C23 C22 H22A 111.0 C23 C22 H22B 111.0 C22 C23 H23A 110.6 C22 C23 H23B 110.6 C22 C23 C24 105.5(6) H23A C23 H23B 108.8 C24 C23 H23A 110.6 C24 C23 H23B 110.6 O3 C24 C23 102.5(7) O3 C24 H24A 111.3 O3 C24 H24B 111.3 C23 C24 H24A 111.3 C23 C24 H24B 111.3 H24A C24 H24B 109.2 O1 C13A H13C 108.6 O1 C13A H13D 108.6 O1 C13A C14A 115(2) H13C C13A H13D 107.6 C14A C13A H13C 108.6 C14A C13A H13D 108.6 C13A C14A H14C 113.3 C13A C14A H14D 113.3 H14C C14A H14D 110.7 C15A C14A C13A 92(2) C15A C14A H14C 113.3 C15A C14A H14D 113.3 C14A C15A H15C 110.8 C14A C15A H15D 110.8 C14A C15A C16A 104.7(13) H15C C15A H15D 108.9 C16A C15A H15C 110.8 C16A C15A H15D 110.8 O1 C16A C15A 108.4(8) O1 C16A H16C 110.0 O1 C16A H16D 110.0 C15A C16A H16C 110.0 C15A C16A H16D 110.0 H16C C16A H16D 108.4 O2 C17A H17C 111.5 O2 C17A H17D 111.5 O2 C17A C18A 101.2(14) H17C C17A H17D 109.3 C18A C17A H17C 111.5 C18A C17A H17D 111.5 C17A C18A H18C 110.8 C17A C18A H18D 110.8 C17A C18A C19A 104.6(16) H18C C18A H18D 108.9 C19A C18A H18C 110.8 C19A C18A H18D 110.8 C18A C19A H19C 112.4 C18A C19A H19D 112.4 H19C C19A H19D 110.0 C20A C19A C18A 96.8(14) C20A C19A H19C 112.4 C20A C19A H19D 112.4 O2 C20A C19A 107.0(11) O2 C20A H20C 110.3 O2 C20A H20D 110.3 C19A C20A H20C 110.3 C19A C20A H20D 110.3 H20C C20A H20D 108.6 O3 C21A H21C 111.7 O3 C21A H21D 111.7 O3 C21A C22A 100.4(9) H21C C21A H21D 109.5 C22A C21A H21C 111.7 C22A C21A H21D 111.7 H23C C23A H23D 109.3 C22A C23A H23C 111.4 C22A C23A H23D 111.4 C22A C23A C24A 101.7(7) C24A C23A H23C 111.4 C24A C23A H23D 111.4 C21A C22A H22C 109.9 C21A C22A H22D 109.9 C23A C22A C21A 108.7(9) C23A C22A H22C 109.9 C23A C22A H22D 109.9 H22C C22A H22D 108.3 O3 C24A C23A 103.9(7) O3 C24A H24C 111.0 O3 C24A H24D 111.0 C23A C24A H24C 111.0 C23A C24A H24D 111.0 H24C C24A H24D 109.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Li1 O1 1.926(4) Li1 O3 1.919(4) Li1 O2 1.932(4) Li1 H 1.83(3) Al1 N1 1.8776(18) Al1 N2 1.8664(19) Al1 H 1.61(3) Al1 HA 1.55(2) Si1 N1 1.7271(17) Si1 C1 1.876(3) Si1 C2 1.871(3) Si1 C3 1.882(3) Si2 N1 1.7168(18) Si2 C4 1.879(3) Si2 C5 1.867(3) Si2 C6 1.871(3) Si3 N2 1.721(2) Si3 C7 1.870(3) Si3 C8 1.872(4) Si3 C9 1.873(3) Si4 N2 1.708(2) Si4 C11 1.873(4) Si4 C12 1.885(4) Si4 C10 1.867(4) O1 C13 1.440(6) O1 C16 1.443(4) O1 C13A 1.433(9) O1 C16A 1.434(8) O3 C21 1.438(8) O3 C24 1.441(8) O3 C21A 1.442(8) O3 C24A 1.432(8) O2 C17 1.449(6) O2 C20 1.432(5) O2 C17A 1.440(9) O2 C20A 1.432(9) C4 H4A 0.9800 C4 H4B 0.9800 C4 H4C 0.9800 C5 H5A 0.9800 C5 H5B 0.9800 C5 H5C 0.9800 C1 H1A 0.9800 C1 H1B 0.9800 C1 H1C 0.9800 C6 H6A 0.9800 C6 H6B 0.9800 C6 H6C 0.9800 C2 H2A 0.9800 C2 H2B 0.9800 C2 H2C 0.9800 C7 H7A 0.9800 C7 H7B 0.9800 C7 H7C 0.9800 C3 H3A 0.9800 C3 H3B 0.9800 C3 H3C 0.9800 C11 H11A 0.9800 C11 H11B 0.9800 C11 H11C 0.9800 C8 H8A 0.9800 C8 H8B 0.9800 C8 H8C 0.9800 C12 H12A 0.9800 C12 H12B 0.9800 C12 H12C 0.9800 C10 H10A 0.9800 C10 H10B 0.9800 C10 H10C 0.9800 C9 H9A 0.9800 C9 H9B 0.9800 C9 H9C 0.9800 C13 H13A 0.9900 C13 H13B 0.9900 C13 C14 1.527(7) C14 H14A 0.9900 C14 H14B 0.9900 C14 C15 1.506(6) C15 H15A 0.9900 C15 H15B 0.9900 C15 C16 1.523(5) C16 H16A 0.9900 C16 H16B 0.9900 C17 H17A 0.9900 C17 H17B 0.9900 C17 C18 1.504(7) C18 H18A 0.9900 C18 H18B 0.9900 C18 C19 1.545(6) C19 H19A 0.9900 C19 H19B 0.9900 C19 C20 1.508(8) C20 H20A 0.9900 C20 H20B 0.9900 C21 H21A 0.9900 C21 H21B 0.9900 C21 C22 1.496(8) C22 H22A 0.9900 C22 H22B 0.9900 C22 C23 1.480(8) C23 H23A 0.9900 C23 H23B 0.9900 C23 C24 1.535(9) C24 H24A 0.9900 C24 H24B 0.9900 C13A H13C 0.9900 C13A H13D 0.9900 C13A C14A 1.529(10) C14A H14C 0.9900 C14A H14D 0.9900 C14A C15A 1.519(9) C15A H15C 0.9900 C15A H15D 0.9900 C15A C16A 1.521(9) C16A H16C 0.9900 C16A H16D 0.9900 C17A H17C 0.9900 C17A H17D 0.9900 C17A C18A 1.525(10) C18A H18C 0.9900 C18A H18D 0.9900 C18A C19A 1.530(9) C19A H19C 0.9900 C19A H19D 0.9900 C19A C20A 1.518(10) C20A H20C 0.9900 C20A H20D 0.9900 C21A H21C 0.9900 C21A H21D 0.9900 C21A C22A 1.509(9) C23A H23C 0.9900 C23A H23D 0.9900 C23A C22A 1.506(8) C23A C24A 1.525(9) C22A H22C 0.9900 C22A H22D 0.9900 C24A H24C 0.9900 C24A H24D 0.9900 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 Li1 O1 C13 C14 140.7(9) Li1 O1 C16 C15 -127.7(4) Li1 O1 C13A C14A 132(3) Li1 O1 C16A C15A -161.9(7) Li1 O3 C21 C22 175.8(7) Li1 O3 C24 C23 174.0(4) Li1 O3 C21A C22A 145.0(6) Li1 O3 C24A C23A -142.9(6) Li1 O2 C17 C18 -175.4(5) Li1 O2 C20 C19 -156.8(5) Li1 O2 C17A C18A 160.7(10) Li1 O2 C20A C19A 171.4(11) O1 C13 C14 C15 3.1(17) O1 C13A C14A C15A 41(4) O3 C21 C22 C23 4.4(13) O3 C21A C22A C23A 24.2(12) O2 C17 C18 C19 -31.6(11) O2 C17A C18A C19A 37(2) N1 Al1 N2 Si3 77.34(13) N1 Al1 N2 Si4 -122.18(11) N2 Al1 N1 Si1 -150.95(10) N2 Al1 N1 Si2 31.52(16) C4 Si2 N1 Al1 -140.78(14) C4 Si2 N1 Si1 41.83(16) C5 Si2 N1 Al1 -23.75(17) C5 Si2 N1 Si1 158.86(13) C1 Si1 N1 Al1 -29.60(15) C1 Si1 N1 Si2 148.05(13) C6 Si2 N1 Al1 96.25(16) C6 Si2 N1 Si1 -81.14(16) C2 Si1 N1 Al1 90.92(18) C2 Si1 N1 Si2 -91.4(2) C7 Si3 N2 Al1 -135.61(14) C7 Si3 N2 Si4 64.94(18) C3 Si1 N1 Al1 -147.03(14) C3 Si1 N1 Si2 30.63(18) C11 Si4 N2 Al1 -61.44(18) C11 Si4 N2 Si3 97.96(18) C8 Si3 N2 Al1 -16.5(2) C8 Si3 N2 Si4 -175.99(18) C12 Si4 N2 Al1 179.2(2) C12 Si4 N2 Si3 -21.4(3) C10 Si4 N2 Al1 60.06(17) C10 Si4 N2 Si3 -140.55(16) C9 Si3 N2 Al1 103.8(2) C9 Si3 N2 Si4 -55.6(2) C13 O1 C16 C15 40.8(10) C13 O1 C13A C14A 75(17) C13 O1 C16A C15A -12.8(13) C13 C14 C15 C16 20.1(13) C14 C15 C16 O1 -35.1(7) C16 O1 C13 C14 -27.8(16) C16 O1 C13A C14A -42(4) C16 O1 C16A C15A 108(2) C17 O2 C20 C19 18.2(10) C17 O2 C17A C18A 74(7) C17 O2 C20A C19A -24(2) C17 C18 C19 C20 41.7(11) C18 C19 C20 O2 -37.8(11) C20 O2 C17 C18 9.3(11) C20 O2 C17A C18A -24(2) C20 O2 C20A C19A 60(6) C21 O3 C24 C23 -30.8(12) C21 O3 C21A C22A 86(4) C21 O3 C24A C23A 30.0(14) C21 C22 C23 C24 -23.0(11) C22 C23 C24 O3 33.5(10) C24 O3 C21 C22 17.4(14) C24 O3 C21A C22A -25.8(12) C24 O3 C24A C23A -35(3) C13A O1 C13 C14 -92(18) C13A O1 C16 C15 47(2) C13A O1 C16A C15A -7(2) C13A C14A C15A C16A -40(2) C14A C15A C16A O1 33.2(17) C16A O1 C13 C14 -9.5(15) C16A O1 C16 C15 -23.5(16) C16A O1 C13A C14A -23(4) C17A O2 C17 C18 -76(8) C17A O2 C20 C19 28.3(16) C17A O2 C20A C19A -14(3) C17A C18A C19A C20A -43(2) C18A C19A C20A O2 35(2) C20A O2 C17 C18 19.9(16) C20A O2 C20 C19 -81(7) C20A O2 C17A C18A -14(3) C21A O3 C21 C22 -55(4) C21A O3 C24 C23 -15.4(11) C21A O3 C24A C23A 43.8(13) C22A C23A C24A O3 -25.8(12) C24A O3 C21 C22 2.3(15) C24A O3 C24 C23 90(4) C24A O3 C21A C22A -41.8(12) C24A C23A C22A C21A 0.6(12) loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.95319 2 0.04681