#------------------------------------------------------------------------------ #$Date: 2026-09-24 07:42:57 +0100 (Thu, 24 Sep 2026) $ #$Revision: 306901 $ #$URL: svn://www.crystallography.net/cod/cif/4/51/95/4519525.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_4519525 loop_ _publ_author_name 'Kapustin, Eugene A.' 'Lee, Seungkyu' 'Alshammari, Ahmad S.' 'Yaghi, Omar M.' _publ_section_title ; Molecular Retrofitting Adapts a Metal--Organic Framework to Extreme Pressure ; _journal_issue 6 _journal_name_full 'ACS Central Science' _journal_page_first 662 _journal_page_last 667 _journal_paper_doi 10.1021/acscentsci.7b00169 _journal_volume 3 _journal_year 2017 _chemical_absolute_configuration ad _chemical_formula_moiety 'C28 H18 Al2 O10' _chemical_formula_sum 'C28 H18 Al2 O10' _chemical_formula_weight 568.38 _chemical_name_common MOF-520_0.15GPa _space_group_crystal_system tetragonal _space_group_IT_number 94 _space_group_name_Hall 'P 4n 2n' _space_group_name_H-M_alt 'P 42 21 2' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 19.070(3) _cell_length_b 19.070(3) _cell_length_c 36.930(7) _cell_measurement_reflns_used 3242 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 13.01 _cell_measurement_theta_min 2.19 _cell_volume 13430(4) _computing_cell_refinement 'SAINT V8.34A Bruker-AXS, Madison WI' _computing_data_collection 'Bruker APEX2 Bruker-AXS, Madison WI' _computing_data_reduction 'SAINT V8.34A Bruker-AXS, Madison WI' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2015)' _computing_structure_solution 'XS (Sheldrick, 2008)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.892 _diffrn_measured_fraction_theta_max 0.892 _diffrn_measurement_device_type 'Perkin Elmer CMOS' _diffrn_measurement_method '\w 80 degrees scan' _diffrn_radiation_monochromator 'silicon 111' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.49594 _diffrn_reflns_av_R_equivalents 0.1067 _diffrn_reflns_av_unetI/netI 0.1517 _diffrn_reflns_Laue_measured_fraction_full 0.892 _diffrn_reflns_Laue_measured_fraction_max 0.892 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 10435 _diffrn_reflns_point_group_measured_fraction_full 0.875 _diffrn_reflns_point_group_measured_fraction_max 0.875 _diffrn_reflns_theta_full 13.025 _diffrn_reflns_theta_max 13.025 _diffrn_reflns_theta_min 0.839 _diffrn_source ; Advanced Light Source, station 12.2.2 ; _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.029 _exptl_absorpt_correction_T_max 0.7437 _exptl_absorpt_correction_T_min 0.4700 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1657 before and 0.0791 after correction. The Ratio of minimum to maximum transmission is 0.6320. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 0.563 _exptl_crystal_description block _exptl_crystal_F_000 2336 _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.153 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.035 _refine_ls_abs_structure_details ; Flack x determined using 563 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.6(7) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 329 _refine_ls_number_reflns 4641 _refine_ls_number_restraints 303 _refine_ls_restrained_S_all 0.922 _refine_ls_R_factor_all 0.1582 _refine_ls_R_factor_gt 0.0628 _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^)+(0.1060P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1628 _refine_ls_wR_factor_ref 0.2101 _reflns_Friedel_coverage 0.686 _reflns_Friedel_fraction_full 0.852 _reflns_Friedel_fraction_max 0.852 _reflns_number_gt 1888 _reflns_number_total 4641 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file oc7b00169_si_002.cif _cod_data_source_block MOF520_0.15GPa _cod_original_cell_volume 13430(5) _cod_database_code 4519525 _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 0.7437 _shelx_estimated_absorpt_t_min 0.4700 _exptl_absorpt_special_details ; Data was collected in a Merril Bassett DAC. DAC opening angle of 40 degrees. The pressure of 0.15 GPa was measured via ruby method. The sample was collected by rotating 80 degrees. The data sets were merged in XPREP to produce the final data set. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, H1 of O1, H2 of O2 At 1.5 times of: H3 of O3 2. Restrained distances O3-H3 0.85 with sigma of 0.01 C1-H3 1.988823 with sigma of 0.02 Al2-H3 2.384167 with sigma of 0.02 3. Rigid body (RIGU) restrains C6, Al1, O1, O10, Al2, H1, C28, O3, O2, O9, H28, C1, Al3, H2, C2, O4, C3, C4, C5, C8, C13, C9, C12, C10, C21, C11, C14, C26, C22, C19, C15, C25, C23, C1AA, C24, C0AA, C27, C20, O8, O7, O5, O6, Al1, O1, Al1, O10, Al2, O1, O1, H1, O10, C28, Al2, O3, Al2, O2, Al2, O9, O9, C28, C28, H28, O3, C1, Al3, O2, O2, H2, O4, C1, C2, C1, Al3, O4, C6, C2, C3, C2, C6, C4, C3, C5, C4, C5, C4, C8, C5, C8, C13, C9, C8, C13, C12, C9, C10, C21, C12, C12, C11, C14, C10, C11, C10, C26, C21, C22, C21, C19, C14, C15, C14, C26, C25, C23, C22, C22, C19, C1AA, C15, C25, C23, C25, C24, C24, C23, C1AA, C0AA, C27, C24, C20, C0AA, O8, C27, O7, C27, O5, C20, O6, C20 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4.a Aromatic/amide H refined with riding coordinates: O2(H2), O1(H1), C23(H23), C22(H22), C26(H26), C25(H25), C6(H6), C44(H44), C4(H4), C3(H3A), C13(H13), C9(H9), C28(H28), C11(H11), C17(H17), C19(H19), C15(H15), C1AA(H1AA) 4.b Fitted hexagon refined as free rotating group: C23(C22,C21,C26,C25,C24), C6(C44,C5,C4,C3,C2), C17(C19,C14,C15,C1AA,C0AA) ; _shelx_res_file ; p2_25kev_0m.res created by SHELXL-2014/7 TITL P2_25keV_0m in P42212 #94 REM reset to P42212 #94 CELL 0.49594 19.07 19.07 36.93 90 90 90 ZERR 222 0.0027 0.0027 0.00739 0 0 0 LATT -1 SYMM 0.5-Y,0.5+X,0.5+Z SYMM -X,-Y,+Z SYMM 0.5+Y,0.5-X,0.5+Z SYMM 0.5+X,0.5-Y,0.5-Z SYMM 0.5-X,0.5+Y,0.5-Z SYMM +Y,+X,-Z SYMM -Y,-X,-Z SFAC C H O Al DISP Al 0.031 0.024 81.761 DISP C 0.001 0.001 6.243 DISP H -0 0 0.608 DISP O 0.004 0.003 13.948 UNIT 222 222 222 222 DFIX 0.85 0.01 O3 H3 DANG 1.988823 0.02 C1 H3 DANG 2.384167 0.02 Al2 H3 RIGU C6 Al1 O1 O10 Al2 H1 C28 O3 O2 O9 H28 C1 Al3 H2 C2 O4 C3 C4 C5 C8 C13 = C9 C12 C10 C21 C11 C14 C26 C22 C19 C15 C25 C23 C1AA C24 C0AA C27 C20 O8 O7 = O5 O6 AL1 O1 AL1 O10 AL2 O1 O1 H1 O10 C28 AL2 O3 AL2 O2 AL2 O9 O9 C28 C28 = H28 O3 C1 AL3 O2 O2 H2 O4 C1 C2 C1 AL3 O4 C6 C2 C3 C2 C6 C4 C3 C5 C4 C5 C4 = C8 C5 C8 C13 C9 C8 C13 C12 C9 C10 C21 C12 C12 C11 C14 C10 C11 C10 C26 C21 = C22 C21 C19 C14 C15 C14 C26 C25 C23 C22 C22 C19 C1AA C15 C25 C23 C25 C24 C24 = C23 C1AA C0AA C27 C24 C20 C0AA O8 C27 O7 C27 O5 C20 O6 C20 L.S. 24 PLAN 120 TEMP 23 BOND ABIN ACTA fmap 2 REM REM REM WGHT 0.106000 FVAR 0.12322 AL1 4 0.663493 0.336507 0.500000 10.50000 0.08543 0.08543 = 0.15907 0.00890 0.00890 0.00122 AL2 4 0.618172 0.391257 0.415996 11.00000 0.09028 0.08993 = 0.17535 0.00417 -0.00263 0.00206 AL3 4 0.500000 0.500000 0.381488 10.50000 0.05653 0.06893 = 0.12050 0.00000 0.00000 0.00081 O2 3 0.562779 0.471566 0.419496 11.00000 0.04367 0.06493 = 0.09681 0.00932 0.01809 -0.00866 AFIX 43 H2 2 0.565616 0.498793 0.440337 11.00000 -1.20000 AFIX 0 O3 3 0.650602 0.406861 0.370423 11.00000 0.08136 0.13343 = 0.18204 0.01950 0.01000 0.00897 H3 2 0.692855 0.397394 0.364751 11.00000 -1.50000 O1 3 0.597016 0.353008 0.467613 11.00000 0.12400 0.11780 = 0.17614 0.00825 0.00291 -0.01371 AFIX 43 H1 2 0.550650 0.344194 0.473953 11.00000 -1.20000 AFIX 0 O4 3 0.552730 0.479319 0.344183 11.00000 0.06267 0.07560 = 0.10457 0.00681 -0.01133 0.00664 C1 1 0.612826 0.438365 0.337683 11.00000 0.04405 0.05627 = 0.15502 0.00827 0.00143 -0.00842 AFIX 66 C23 1 0.789454 0.633380 0.066568 11.00000 0.24771 0.11457 = 0.19748 -0.00273 0.03062 -0.02115 AFIX 43 H23 2 0.796714 0.635778 0.041697 11.00000 -1.20000 AFIX 65 C22 1 0.780543 0.568666 0.083266 11.00000 0.15244 0.10117 = 0.19116 -0.00273 0.02076 -0.00324 AFIX 43 H22 2 0.781841 0.527767 0.069566 11.00000 -1.20000 AFIX 65 C21 1 0.769692 0.565081 0.120439 11.00000 0.09912 0.09109 = 0.17755 -0.00124 0.01560 -0.00028 C26 1 0.767752 0.626210 0.140915 11.00000 0.11722 0.11037 = 0.17390 -0.00365 0.01488 -0.00434 AFIX 43 H26 2 0.760492 0.623811 0.165786 11.00000 -1.20000 AFIX 65 C25 1 0.776663 0.690924 0.124218 11.00000 0.19344 0.11383 = 0.18214 0.00033 0.01430 -0.02169 AFIX 43 H25 2 0.775365 0.731823 0.137918 11.00000 -1.20000 AFIX 65 C24 1 0.787513 0.694510 0.087045 11.00000 0.07142 0.08061 = 0.16046 0.00019 -0.01136 -0.01656 AFIX 0 C20 1 0.982731 0.153669 0.120309 11.00000 0.11435 0.09269 = 0.18135 0.00489 0.01180 0.00137 C27 1 0.816173 0.766550 0.059338 11.00000 0.05997 0.05298 = 0.15128 -0.00050 -0.00331 0.01314 AFIX 66 C6 1 0.617465 0.483305 0.278320 11.00000 0.13127 0.15496 = 0.19841 0.04512 0.01143 0.01993 AFIX 43 H6 2 0.580513 0.513498 0.283516 11.00000 -1.20000 AFIX 65 C44 1 0.646057 0.481771 0.243707 11.00000 0.27976 0.39441 = 0.37933 0.04913 0.07820 0.06971 AFIX 43 H44 2 0.628236 0.510937 0.225745 11.00000 -1.20000 AFIX 65 C5 1 0.701285 0.436644 0.235941 11.00000 0.06709 0.07623 = 0.15940 -0.01031 -0.00761 -0.00253 C4 1 0.727922 0.393051 0.262788 11.00000 0.06886 0.08781 = 0.16446 -0.00708 0.02225 0.01491 AFIX 43 H4 2 0.764873 0.362858 0.257592 11.00000 -1.20000 AFIX 65 C3 1 0.699330 0.394584 0.297401 11.00000 0.12203 0.13625 = 0.17860 0.00875 0.02199 0.02494 AFIX 43 H3A 2 0.717152 0.365417 0.315363 11.00000 -1.20000 AFIX 65 C2 1 0.644102 0.439711 0.305167 11.00000 0.04954 0.05663 = 0.15261 -0.00667 0.00692 -0.02530 AFIX 0 C13 1 0.729230 0.490474 0.172064 11.00000 0.08384 0.09107 = 0.16823 -0.00481 0.00302 0.00499 AFIX 43 H13 2 0.695686 0.524966 0.176174 11.00000 -1.20000 AFIX 0 C10 1 0.808926 0.388189 0.148900 11.00000 0.07102 0.07487 = 0.13201 -0.00243 -0.01069 -0.02391 C12 1 0.762127 0.495261 0.139371 11.00000 0.11927 0.10252 = 0.17600 -0.00354 0.01221 -0.00531 C9 1 0.768983 0.378446 0.182665 11.00000 0.09793 0.08071 = 0.15009 0.02072 -0.00650 -0.00139 AFIX 43 H9 2 0.763329 0.333975 0.192580 11.00000 -1.20000 AFIX 0 O8 3 0.828646 0.808816 0.084740 11.00000 0.06243 0.06069 = 0.13031 0.01190 0.00403 -0.00532 O10 3 0.731241 0.399089 0.481274 11.00000 0.08564 0.07214 = 0.16292 -0.01343 0.01130 0.00273 O5 3 1.032839 0.170505 0.093489 11.00000 0.08180 0.07910 = 0.13834 0.01003 -0.01909 -0.00251 O6 3 0.955899 0.091215 0.120262 11.00000 0.06663 0.06655 = 0.11098 0.01091 0.00509 0.01281 O7 3 0.799889 0.766800 0.037589 11.00000 0.11459 0.11042 = 0.16473 0.00626 -0.01273 -0.01412 O9 3 0.698320 0.444772 0.427151 11.00000 0.08567 0.09596 = 0.17746 -0.00298 0.00936 -0.00548 C28 1 0.735367 0.444239 0.453167 11.00000 0.03983 0.05269 = 0.16186 -0.01289 0.01716 0.01164 AFIX 43 H28 2 0.770404 0.478101 0.454202 11.00000 -1.20000 AFIX 0 C8 1 0.737342 0.441908 0.200928 11.00000 0.13938 0.10904 = 0.17915 0.00524 0.02066 0.00448 C11 1 0.801993 0.433192 0.127707 11.00000 0.11263 0.09441 = 0.14439 0.00467 0.01502 0.00013 AFIX 43 H11 2 0.820814 0.429910 0.104538 11.00000 -1.20000 AFIX 66 C17 1 0.955237 0.279701 0.109206 11.00000 0.26433 0.13866 = 0.25745 0.02798 0.01304 -0.03488 AFIX 43 H17 2 0.996144 0.286176 0.095910 11.00000 -1.20000 AFIX 65 C19 1 0.912169 0.336584 0.116904 11.00000 0.14364 0.13550 = 0.22447 0.00300 0.04700 -0.02598 AFIX 43 H19 2 0.924260 0.381117 0.108759 11.00000 -1.20000 AFIX 65 C14 1 0.851029 0.326906 0.136777 11.00000 0.10610 0.10229 = 0.16255 0.00995 0.01309 -0.00669 C15 1 0.832957 0.260345 0.148952 11.00000 0.10705 0.10266 = 0.12891 0.00919 0.00721 -0.01112 AFIX 43 H15 2 0.792050 0.253870 0.162248 11.00000 -1.20000 AFIX 65 C1AA 1 0.876024 0.203461 0.141254 11.00000 0.11153 0.10651 = 0.17654 0.01237 0.00372 -0.01079 AFIX 43 H1AA 2 0.863933 0.158928 0.149399 11.00000 -1.20000 AFIX 65 C0AA 1 0.937165 0.213138 0.121381 11.00000 0.12996 0.09567 = 0.21452 -0.00070 0.01894 -0.00515 AFIX 0 HKLF 4 REM P2_25keV_0m in P42212 #94 REM R1 = 0.0628 for 1888 Fo > 4sig(Fo) and 0.1582 for all 4641 data REM 329 parameters refined using 303 restraints END WGHT 0.1052 0.0000 REM Highest difference peak 0.153, deepest hole -0.351, 1-sigma level 0.035 Q1 1 0.6436 0.5145 0.3810 11.00000 0.05 0.15 Q2 1 0.5003 0.4817 0.3698 11.00000 0.05 0.15 Q3 1 0.6898 0.3221 0.5176 11.00000 0.05 0.14 Q4 1 0.6902 0.4006 0.5001 11.00000 0.05 0.13 Q5 1 0.9426 0.1265 0.1469 11.00000 0.05 0.13 Q6 1 0.7579 0.4258 0.4332 11.00000 0.05 0.12 Q7 1 0.6238 0.4779 0.4709 11.00000 0.05 0.12 Q8 1 0.6025 0.3175 0.3666 11.00000 0.05 0.12 Q9 1 0.8371 0.7583 0.0487 11.00000 0.05 0.12 Q10 1 0.6901 0.3997 0.2333 11.00000 0.05 0.11 Q11 1 0.6215 0.3157 0.5002 11.00000 0.05 0.11 Q12 1 0.7592 0.3653 0.4991 11.00000 0.05 0.11 Q13 1 0.8331 0.7125 0.0056 11.00000 0.05 0.11 Q14 1 0.6986 0.4027 0.4562 11.00000 0.05 0.11 Q15 1 1.0265 0.2250 0.0657 11.00000 0.05 0.11 Q16 1 0.6558 0.5280 0.4121 11.00000 0.05 0.11 Q17 1 1.0377 0.2090 0.0724 11.00000 0.05 0.11 Q18 1 0.6460 0.4025 0.2998 11.00000 0.05 0.11 Q19 1 0.5120 0.4815 0.3980 11.00000 0.05 0.10 Q20 1 0.7030 0.5200 0.3115 11.00000 0.05 0.10 Q21 1 0.8361 0.3163 0.1976 11.00000 0.05 0.10 Q22 1 0.8139 0.3833 0.1597 11.00000 0.05 0.10 Q23 1 0.9785 0.2695 0.2405 11.00000 0.05 0.10 Q24 1 0.7790 0.2723 0.1133 11.00000 0.05 0.10 Q25 1 0.7301 0.6969 0.0505 11.00000 0.05 0.10 Q26 1 0.9069 0.0967 0.1004 11.00000 0.05 0.10 Q27 1 0.7185 0.4272 0.4548 11.00000 0.05 0.10 Q28 1 0.6411 0.3324 0.5123 11.00000 0.05 0.10 Q29 1 0.7268 0.6990 0.0915 11.00000 0.05 0.10 Q30 1 0.7531 0.3811 0.4969 11.00000 0.05 0.10 Q31 1 1.0016 0.1853 0.1228 11.00000 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17 7.7075 13.4626 13 5 18 -2.7971 -7.5063 13 5 19 6.0259 1.1966 13 6 0 -1.1244 0.0000 13 6 2 4.3058 5.1066 13 6 3 7.3777 -4.3032 13 6 4 -4.8836 3.9200 13 6 5 18.3310 -4.3631 13 6 6 -4.1638 12.0837 13 6 8 3.6122 -8.2267 13 6 9 -3.7907 14.3444 13 6 10 -7.3980 -9.5347 13 6 11 1.7223 -5.8762 13 6 12 -10.1999 -0.5490 13 6 13 19.5517 -1.1534 13 6 14 12.2178 7.8273 13 6 15 4.1245 8.6778 13 6 16 1.1982 -3.1195 13 6 17 20.8969 13.2241 13 6 18 5.6300 7.6784 13 7 0 -13.7213 0.0000 13 7 1 4.2019 -2.7823 13 7 2 -2.5542 4.8894 13 7 3 6.1239 1.9229 13 7 4 -3.8384 -7.2101 13 7 5 3.3322 1.7599 13 7 6 1.1322 10.5102 13 7 7 0.4992 -11.5477 13 7 8 7.3709 14.3870 13 7 9 6.8391 -2.5174 13 7 10 -4.3510 1.5893 13 7 11 4.7283 -8.8108 13 7 12 -9.0786 -4.9368 13 7 13 6.4930 4.6480 13 7 14 -5.1735 1.8321 13 7 15 -5.0843 -10.7755 13 7 16 -12.8297 -14.7691 13 7 17 8.7557 -1.9102 13 8 0 0.8977 0.0000 13 8 1 4.3336 -8.2429 13 8 2 -2.7822 3.9998 13 8 3 7.9242 -9.3282 13 8 4 1.3548 17.5075 13 8 5 2.7657 3.0483 13 8 6 7.1771 1.7424 13 8 7 4.5414 -3.2328 13 8 8 10.0931 -0.0962 13 8 9 -14.2346 -9.9994 13 8 10 -4.2346 -2.2219 13 8 11 6.4525 8.6638 13 8 12 -4.1026 -4.5809 13 8 13 -8.4483 5.3625 13 8 14 -0.0753 -1.8818 13 8 15 2.1824 -8.2859 13 9 0 -8.2380 0.0000 13 9 1 -5.6361 1.8439 13 9 2 4.2885 -4.1963 13 9 3 -0.0748 -3.9862 13 9 4 -0.4811 3.3604 13 9 5 -6.9897 -2.1075 13 9 6 3.4551 -8.0886 13 9 7 -6.8916 -7.1024 13 9 8 -0.6429 6.3326 13 9 9 16.3284 -3.5493 13 9 10 7.9634 -1.9582 13 9 11 0.1469 -7.2964 13 9 12 10.9223 4.7777 13 9 13 -0.0781 -4.0755 13 10 0 -4.7026 -0.0000 13 10 1 0.2436 9.5070 13 10 2 3.4923 1.2403 13 10 3 -1.1036 6.0320 13 10 4 -3.5420 0.6479 13 10 5 -2.9888 -1.7085 13 10 6 0.4551 1.2735 13 10 7 8.5657 4.9252 13 10 8 0.7620 2.0453 13 10 9 5.9253 0.6946 13 10 10 11.6670 0.0524 13 11 0 6.1932 -0.0000 13 11 1 10.1745 0.8195 13 11 2 1.1141 5.6512 13 11 3 -1.6498 -4.7420 13 11 6 -0.5989 -2.5504 14 0 0 -14.1126 -0.0000 14 0 1 0.0000 3.8344 14 0 2 -14.9835 0.0000 14 0 3 0.0000 3.4966 14 0 4 -6.6371 -0.0000 14 0 5 0.0000 3.4055 14 0 6 -20.0972 -0.0000 14 0 7 0.0000 10.0386 14 0 8 4.1690 0.0000 14 0 9 0.0000 2.8981 14 0 10 -5.3227 0.0000 14 0 13 -0.0000 -7.6024 14 0 14 -8.8728 -0.0000 14 0 15 0.0000 14.6288 14 0 16 17.0858 0.0000 14 0 17 0.0000 13.6864 14 0 18 7.6281 0.0000 14 0 19 0.0000 1.1867 14 1 0 1.8319 -0.0000 14 1 2 25.7321 -17.4331 14 1 3 16.0842 11.3544 14 1 4 3.5832 -10.6158 14 1 5 -7.1455 1.9931 14 1 6 14.1078 29.1598 14 1 9 -3.6379 15.7186 14 1 10 -12.0900 -1.6423 14 1 11 -7.8910 -4.3936 14 1 12 -0.2212 24.7583 14 1 13 -14.5257 -32.2106 14 1 14 -1.5685 -15.4182 14 1 15 6.8694 -5.9937 14 1 16 7.3805 22.8709 14 1 17 5.1654 -15.6462 14 1 18 -2.3285 7.0624 14 1 19 -12.0743 1.5509 14 2 0 -2.5797 0.0000 14 2 1 6.8039 -3.3563 14 2 2 2.5766 -16.7552 14 2 3 21.9224 2.4831 14 2 4 7.1110 2.8702 14 2 11 8.8365 34.5175 14 2 12 23.8370 15.1568 14 2 13 -3.1679 -12.9271 14 2 14 12.1425 -2.4165 14 2 15 -8.0729 -9.6190 14 2 16 2.3994 12.7877 14 2 17 -3.1973 -9.0210 14 2 18 -10.7991 9.6434 14 2 19 3.4426 -7.2630 14 3 0 -0.8219 0.0000 14 3 2 -5.3133 -10.9485 14 3 3 8.3405 -0.6840 14 3 4 2.1284 -7.1289 14 3 6 6.9237 9.5771 14 3 11 9.0829 -5.3296 14 3 12 -8.9691 12.1984 14 3 13 0.2642 -5.1495 14 3 14 9.9130 -2.1826 14 3 15 -18.4463 -17.8572 14 3 16 3.7622 14.8511 14 3 17 2.0552 -8.4865 14 3 18 -9.7980 6.0191 14 4 3 -1.9429 7.9629 14 4 5 -2.4743 4.1770 14 4 7 -11.9363 -6.7384 14 4 8 -8.3350 -21.0049 14 4 9 -5.2664 -0.7807 14 4 11 1.2854 -16.1111 14 4 12 -2.5642 -9.6281 14 4 13 1.9346 16.1192 14 4 14 0.0295 -28.0262 14 4 15 8.8985 7.6504 14 4 16 5.0140 20.5598 14 4 17 3.1135 9.7887 14 4 18 3.9668 6.5141 14 5 0 4.1489 -0.0000 14 5 1 -5.7047 5.3019 14 5 2 3.1335 -6.3345 14 5 3 2.3260 -4.6174 14 5 6 -6.7635 -0.6123 14 5 7 6.9104 10.2508 14 5 8 0.0297 16.5125 14 5 9 0.8258 -10.7465 14 5 10 9.1871 14.7120 14 5 11 2.1160 9.9229 14 5 12 0.8219 -7.9315 14 5 13 13.6088 -4.2017 14 5 14 17.6967 -9.2962 14 5 15 -10.6709 16.8949 14 5 16 2.1013 -7.8962 14 5 17 -8.4823 2.1859 14 6 0 -4.1634 0.0000 14 6 1 -9.2370 1.8018 14 6 2 1.4785 4.9393 14 6 3 1.2442 2.5228 14 6 4 6.1126 -4.3010 14 6 5 5.4362 17.3017 14 6 6 2.7379 -0.3515 14 6 7 4.6816 -0.3951 14 6 8 8.4267 -9.7202 14 6 9 -8.1662 7.6905 14 6 10 11.6744 6.2637 14 6 11 -5.3665 -2.2053 14 6 12 -13.2452 -3.9035 14 6 13 -8.5755 -1.3183 14 6 14 -1.1382 -1.6523 14 6 15 -7.3312 -0.9260 14 6 16 1.7841 -3.2987 14 7 0 4.2700 -0.0000 14 7 1 -0.2037 -3.8665 14 7 2 -1.0249 -1.4445 14 7 3 -2.9784 -3.7980 14 7 4 7.2603 -10.5001 14 7 5 -3.8875 -0.4297 14 7 7 -10.2353 0.8729 14 7 9 3.1100 -0.7609 14 7 10 -7.2603 -6.1391 14 7 11 -2.8235 4.4542 14 7 12 8.1221 -10.5694 14 7 13 1.5316 -12.8172 14 7 14 0.9375 2.0558 14 8 0 -5.2731 0.0000 14 8 1 3.0619 7.7101 14 8 2 3.5136 -2.9429 14 8 3 -0.1331 3.0741 14 8 4 -5.5253 2.7218 14 8 5 1.9383 0.7325 14 8 6 5.9928 2.8652 14 8 7 -8.4297 -3.3978 14 8 8 -7.9699 1.9511 14 8 9 -7.7263 -0.8917 14 8 10 -8.3750 -3.5379 14 8 11 -7.5878 7.0202 14 8 12 -7.0829 4.5850 14 9 0 -5.4211 0.0000 14 9 1 -0.6517 -3.4280 14 9 2 8.5216 -8.0885 14 9 3 4.6395 6.2543 14 9 4 4.5195 -10.3357 14 9 5 1.8823 -2.0398 14 9 6 1.6333 1.3486 14 9 8 -4.0902 15.2849 14 9 9 3.3614 -2.3209 14 10 0 4.7015 -0.0000 14 10 1 -9.4813 -0.4257 14 10 2 -2.0229 -3.2608 14 10 3 0.0918 2.4510 14 10 4 1.0689 5.7235 15 0 1 -22.8857 0.0000 15 0 2 0.0000 28.3538 15 0 3 -6.0535 0.0000 15 0 4 -0.0000 -6.3905 15 0 5 -16.8708 0.0000 15 0 6 0.0000 6.5445 15 0 7 -13.1740 0.0000 15 0 8 -0.0000 -15.1191 15 0 9 -11.4662 -0.0000 15 0 10 -0.0000 -31.2615 15 0 11 -17.1609 0.0000 15 0 12 -0.0000 -5.6458 15 0 14 0.0000 15.0904 15 0 15 3.5949 0.0000 15 0 16 0.0000 23.0367 15 1 0 4.3673 -0.0000 15 1 1 -4.2192 -34.6217 15 1 2 -1.2250 -13.7995 15 1 3 -28.2541 -2.6098 15 1 4 -0.0591 -28.7385 15 1 5 -6.8158 17.6211 15 1 6 -4.0975 8.0115 15 1 7 -26.1219 -17.8910 15 1 8 -14.9755 -2.8218 15 1 12 -32.6114 0.4327 15 1 13 6.1955 12.0490 15 1 14 -4.8077 0.4506 15 1 16 -0.8131 8.7699 15 2 3 10.4563 18.4945 15 2 4 2.1527 -2.4277 15 2 5 2.6889 2.4772 15 2 12 9.7471 20.3312 15 2 13 10.6937 -1.1039 15 2 14 12.9590 -13.5750 15 2 15 -4.5585 17.8243 15 2 16 31.0466 -3.3261 15 3 1 -7.2913 -16.5748 15 3 3 -8.6563 -4.6141 15 3 4 0.0275 -11.2466 15 3 12 -1.8845 12.7757 15 3 13 -8.4144 23.8056 15 3 14 -11.6871 -7.1833 15 3 15 6.8471 6.7773 15 4 0 -16.1120 0.0000 15 4 1 -4.0227 -2.5425 15 4 3 -12.8095 -0.2608 15 4 4 -0.7991 6.6938 15 4 5 -0.6516 -1.2982 15 4 6 -12.9673 -3.3284 15 4 7 -5.7686 -8.4318 15 4 8 -10.6878 -2.2450 15 4 9 5.3819 21.3375 15 4 12 18.0381 -9.7849 15 4 13 5.2442 -4.6927 15 4 14 -8.3024 6.3877 15 5 0 -1.0675 0.0000 15 5 1 -8.3977 5.9980 15 5 2 7.2681 4.8085 15 5 3 -1.9273 -2.5769 15 5 4 0.0838 -5.8564 15 5 5 0.4815 -2.6252 15 5 6 4.2346 -8.1166 15 5 7 -3.2201 -4.7607 15 5 8 -6.5066 -13.6723 15 5 10 -2.0180 -8.9842 15 5 11 -7.7118 7.1336 15 5 12 -4.8241 15.0827 15 5 13 -1.4779 -6.5974 15 6 0 0.1617 0.0000 15 6 1 1.5446 1.6810 15 6 2 -3.2915 6.5192 15 6 4 -3.8159 -8.8394 15 6 5 8.9141 5.6346 15 6 6 4.7934 4.3557 15 6 7 2.3617 9.5195 15 6 8 7.9694 13.7389 15 6 9 -5.1888 2.6552 15 6 10 1.5602 -4.0681 15 6 12 -2.3155 -0.2359 15 7 0 -8.4722 0.0000 15 7 1 2.0560 2.2125 15 7 2 0.6740 1.0886 15 7 3 -2.3371 -1.2154 15 7 4 12.2536 7.1557 15 7 5 -0.4582 7.5655 15 7 6 -1.4043 -3.4990 15 7 7 -6.6868 0.2410 15 7 8 4.7230 8.3227 15 7 9 3.7548 0.2948 15 8 0 3.2541 -0.0000 15 8 1 2.1429 1.2740 15 8 2 1.5626 -6.9090 15 8 3 3.4178 -4.7865 15 8 4 1.2899 0.8308 15 8 5 4.2602 2.4647 15 8 6 -1.1533 -6.1497 16 0 0 42.3313 0.0000 16 0 1 -0.0000 -18.1744 16 0 2 -4.2090 0.0000 16 0 3 -0.0000 -13.2605 16 0 4 -24.8989 -0.0000 16 0 5 0.0000 2.1758 16 0 6 -5.8932 0.0000 16 0 7 -0.0000 -29.3516 16 0 8 -17.0111 0.0000 16 0 9 0.0000 17.7317 16 0 10 -11.1920 -0.0000 16 0 11 0.0000 7.1343 16 0 12 -10.2313 0.0000 16 1 0 30.2317 -0.0000 16 1 1 18.6695 -10.0570 16 1 2 20.0572 14.7123 16 1 3 -8.5081 27.0509 16 1 4 -11.7077 9.0618 16 1 5 13.7763 6.8448 16 1 6 -19.2862 7.3455 16 1 7 1.8903 -10.6412 16 1 8 3.5026 21.9598 16 1 9 -4.5859 -3.0058 16 1 10 -15.7345 11.3283 16 2 1 33.4996 50.7960 16 2 5 1.2238 4.0801 16 2 6 14.8353 5.5005 16 3 0 5.5404 -0.0000 16 3 1 4.6108 6.0918 16 3 3 -11.9444 0.8040 16 4 1 12.3347 -0.7169 16 4 2 5.2263 -6.7771 16 4 3 -0.9686 8.5385 16 4 4 7.9461 -3.1986 16 4 6 5.1037 -8.1524 16 4 7 0.2719 -1.0085 16 5 0 0.1912 -0.0000 16 5 2 -0.7149 -2.9507 16 5 3 -3.9821 -4.5364 16 5 4 -0.5240 2.7647 16 5 5 12.8952 10.0809 16 5 6 -6.4292 -3.9908 16 5 7 5.8575 9.5966 16 5 8 0.2828 3.8830 16 6 0 5.3287 -0.0000 16 6 1 -3.5957 0.9277 16 6 2 5.5346 1.1501 16 6 3 -1.7803 1.8312 16 6 4 -4.7628 -7.3635 16 6 5 -2.2033 2.0673 17 0 1 7.2607 0.0000 17 0 2 0.0000 34.3502 17 0 3 21.9872 0.0000 17 0 4 -0.0000 -13.6407 17 0 5 -3.1028 0.0000 17 0 6 -0.0000 -29.8576 17 1 0 -32.5581 -0.0000 17 1 1 -17.8101 -34.4993 17 1 2 17.2067 -4.5593 17 1 3 -29.8640 -22.5320 17 1 4 -18.7755 -15.0888 17 1 5 13.3955 17.5737 17 1 6 7.1616 15.3863 17 2 0 -0.4206 0.0000 17 2 1 -13.3506 9.1608 17 2 2 -0.0252 9.5004 17 2 5 5.1753 -1.7376 17 3 0 -0.3350 -0.0000 17 3 1 -7.5963 8.7856 17 3 2 8.5459 9.2153 17 3 3 5.9868 -7.3618 0 0 0 0.0 0.0 ; _shelx_fab_checksum 48350 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-y+1/2, x+1/2, z+1/2' '-x, -y, z' 'y+1/2, -x+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'y, x, -z' '-y, -x, -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 Al1 Al 0.6635(3) 0.3365(3) 0.5000 0.110(3) Uani 1 2 d S TU P . . Al2 Al 0.6182(3) 0.3913(3) 0.41600(19) 0.119(2) Uani 1 1 d D U . . . Al3 Al 0.5000 0.5000 0.3815(2) 0.082(2) Uani 1 2 d S TU P . . O2 O 0.5628(3) 0.4716(3) 0.4195(2) 0.068(3) Uani 1 1 d . U . . . H2 H 0.5656 0.4988 0.4403 0.082 Uiso 1 1 calc R U . . . O3 O 0.6506(5) 0.4069(6) 0.3704(4) 0.132(4) Uani 1 1 d D U . . . H3 H 0.693(3) 0.397(8) 0.3648(15) 0.198 Uiso 1 1 d DR . . . . O1 O 0.5970(6) 0.3530(5) 0.4676(3) 0.139(4) Uani 1 1 d . U . . . H1 H 0.5506 0.3442 0.4740 0.167 Uiso 1 1 calc R U . . . O4 O 0.5527(4) 0.4793(4) 0.3442(3) 0.081(3) Uani 1 1 d . U . . . C1 C 0.6128(7) 0.4384(7) 0.3377(5) 0.085(4) Uani 1 1 d D U . . . C23 C 0.7895(6) 0.6334(7) 0.0666(3) 0.187(9) Uani 1 1 d . U . . . H23 H 0.7967 0.6358 0.0417 0.224 Uiso 1 1 calc R . . . . C22 C 0.7805(6) 0.5687(5) 0.0833(4) 0.148(7) Uani 1 1 d G U . . . H22 H 0.7818 0.5278 0.0696 0.178 Uiso 1 1 calc R . . . . C21 C 0.7697(5) 0.5651(4) 0.1204(4) 0.123(6) Uani 1 1 d G U . . . C26 C 0.7678(5) 0.6262(7) 0.1409(3) 0.134(6) Uani 1 1 d G U . . . H26 H 0.7605 0.6238 0.1658 0.161 Uiso 1 1 calc R . . . . C25 C 0.7767(5) 0.6909(5) 0.1242(4) 0.163(8) Uani 1 1 d G U . . . H25 H 0.7754 0.7318 0.1379 0.196 Uiso 1 1 calc R . . . . C24 C 0.7875(5) 0.6945(4) 0.0870(4) 0.104(5) Uani 1 1 d G U . . . C20 C 0.9827(10) 0.1537(9) 0.1203(6) 0.129(7) Uani 1 1 d . U . . . C27 C 0.8162(11) 0.7665(12) 0.0593(6) 0.088(6) Uani 1 1 d . U . . . C6 C 0.6175(5) 0.4833(6) 0.2783(4) 0.162(8) Uani 1 1 d . U . . . H6 H 0.5805 0.5135 0.2835 0.194 Uiso 1 1 calc R . . . . C44 C 0.6461(7) 0.4818(6) 0.2437(4) 0.35(2) Uani 1 1 d G . . . . H44 H 0.6282 0.5109 0.2257 0.421 Uiso 1 1 calc R . . . . C5 C 0.7013(6) 0.4366(7) 0.2359(3) 0.101(5) Uani 1 1 d G U . . . C4 C 0.7279(4) 0.3931(5) 0.2628(4) 0.107(5) Uani 1 1 d G U . . . H4 H 0.7649 0.3629 0.2576 0.128 Uiso 1 1 calc R . . . . C3 C 0.6993(6) 0.3946(5) 0.2974(3) 0.146(7) Uani 1 1 d G U . . . H3A H 0.7172 0.3654 0.3154 0.175 Uiso 1 1 calc R . . . . C2 C 0.6441(6) 0.4397(6) 0.3052(3) 0.086(4) Uani 1 1 d G U . . . C13 C 0.7292(8) 0.4905(9) 0.1721(5) 0.114(6) Uani 1 1 d . U . . . H13 H 0.6957 0.5250 0.1762 0.137 Uiso 1 1 calc R . . . . C10 C 0.8089(8) 0.3882(8) 0.1489(6) 0.093(5) Uani 1 1 d . U . . . C12 C 0.7621(9) 0.4953(10) 0.1394(6) 0.133(6) Uani 1 1 d . U . . . C9 C 0.7690(8) 0.3784(7) 0.1827(5) 0.110(5) Uani 1 1 d . U . . . H9 H 0.7633 0.3340 0.1926 0.131 Uiso 1 1 calc R . . . . O8 O 0.8286(4) 0.8088(4) 0.0847(3) 0.084(3) Uani 1 1 d . U . . . O10 O 0.7312(5) 0.3991(5) 0.4813(3) 0.107(4) Uani 1 1 d . U . . . O5 O 1.0328(5) 0.1705(5) 0.0935(3) 0.100(4) Uani 1 1 d . U . . . O6 O 0.9559(4) 0.0912(4) 0.1203(3) 0.081(3) Uani 1 1 d . U . . . O7 O 0.7999(8) 0.7668(9) 0.0376(4) 0.130(6) Uani 1 1 d . U . . . O9 O 0.6983(6) 0.4448(5) 0.4272(4) 0.120(4) Uani 1 1 d . U . . . C28 C 0.7354(7) 0.4442(8) 0.4532(6) 0.085(5) Uani 1 1 d . U . . . H28 H 0.7704 0.4781 0.4542 0.102 Uiso 1 1 calc R U . . . C8 C 0.7373(9) 0.4419(10) 0.2009(7) 0.143(6) Uani 1 1 d . U . . . C11 C 0.8020(8) 0.4332(9) 0.1277(5) 0.117(6) Uani 1 1 d . U . . . H11 H 0.8208 0.4299 0.1045 0.141 Uiso 1 1 calc R . . . . C17 C 0.9552(5) 0.2797(8) 0.1092(3) 0.220(12) Uani 1 1 d . . . . . H17 H 0.9961 0.2862 0.0959 0.264 Uiso 1 1 calc R . . . . C19 C 0.9122(7) 0.3366(6) 0.1169(3) 0.168(9) Uani 1 1 d G U . . . H19 H 0.9243 0.3811 0.1088 0.201 Uiso 1 1 calc R . . . . C14 C 0.8510(6) 0.3269(5) 0.1368(3) 0.124(6) Uani 1 1 d G U . . . C15 C 0.8330(4) 0.2603(6) 0.1490(3) 0.113(6) Uani 1 1 d G U . . . H15 H 0.7920 0.2539 0.1622 0.135 Uiso 1 1 calc R . . . . C1AA C 0.8760(6) 0.2035(5) 0.1413(4) 0.132(7) Uani 1 1 d G U . . . H1AA H 0.8639 0.1589 0.1494 0.158 Uiso 1 1 calc R . . . . C0AA C 0.9372(6) 0.2131(6) 0.1214(4) 0.147(7) Uani 1 1 d G U . . . 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 Al1 0.085(3) 0.085(3) 0.159(9) 0.009(3) 0.009(3) 0.001(4) Al2 0.090(4) 0.090(4) 0.175(6) 0.004(4) -0.003(4) 0.002(3) Al3 0.057(4) 0.069(4) 0.121(7) 0.000 0.000 0.001(3) O2 0.044(5) 0.065(5) 0.097(8) 0.009(4) 0.018(4) -0.009(4) O3 0.081(7) 0.133(9) 0.182(9) 0.019(7) 0.010(6) 0.009(7) O1 0.124(8) 0.118(8) 0.176(11) 0.008(7) 0.003(7) -0.014(7) O4 0.063(6) 0.076(6) 0.105(8) 0.007(5) -0.011(5) 0.007(5) C1 0.044(8) 0.056(8) 0.155(10) 0.008(7) 0.001(6) -0.008(6) C23 0.25(2) 0.115(10) 0.197(16) -0.003(9) 0.031(13) -0.021(11) C22 0.152(16) 0.101(10) 0.191(15) -0.003(8) 0.021(11) -0.003(10) C21 0.099(12) 0.091(8) 0.178(14) -0.001(8) 0.016(11) 0.000(8) C26 0.117(13) 0.110(9) 0.174(14) -0.004(8) 0.015(10) -0.004(10) C25 0.193(19) 0.114(11) 0.182(15) 0.000(9) 0.014(12) -0.022(11) C24 0.071(10) 0.081(8) 0.160(13) 0.000(7) -0.011(9) -0.017(7) C20 0.114(11) 0.093(9) 0.181(17) 0.005(9) 0.012(10) 0.001(7) C27 0.060(12) 0.053(9) 0.151(13) 0.000(8) -0.003(9) 0.013(8) C6 0.131(15) 0.155(16) 0.198(17) 0.045(13) 0.011(12) 0.020(12) C44 0.28(4) 0.39(5) 0.38(6) 0.05(4) 0.08(4) 0.07(4) C5 0.067(10) 0.076(11) 0.159(12) -0.010(8) -0.008(8) -0.003(8) C4 0.069(10) 0.088(11) 0.164(13) -0.007(9) 0.022(8) 0.015(8) C3 0.122(12) 0.136(13) 0.179(14) 0.009(10) 0.022(9) 0.025(10) C2 0.050(8) 0.057(9) 0.153(11) -0.007(7) 0.007(7) -0.025(6) C13 0.084(11) 0.091(10) 0.168(13) -0.005(8) 0.003(9) 0.005(8) C10 0.071(9) 0.075(8) 0.132(13) -0.002(7) -0.011(8) -0.024(7) C12 0.119(14) 0.103(9) 0.176(14) -0.004(8) 0.012(10) -0.005(8) C9 0.098(11) 0.081(9) 0.150(13) 0.021(8) -0.007(8) -0.001(8) O8 0.062(6) 0.061(6) 0.130(11) 0.012(6) 0.004(6) -0.005(5) O10 0.086(7) 0.072(7) 0.163(11) -0.013(6) 0.011(6) 0.003(5) O5 0.082(7) 0.079(7) 0.138(12) 0.010(6) -0.019(6) -0.003(5) O6 0.067(6) 0.067(6) 0.111(10) 0.011(5) 0.005(5) 0.013(5) O7 0.115(11) 0.110(9) 0.165(13) 0.006(8) -0.013(9) -0.014(8) O9 0.086(7) 0.096(7) 0.177(11) -0.003(7) 0.009(6) -0.005(6) C28 0.040(9) 0.053(9) 0.162(12) -0.013(8) 0.017(7) 0.012(7) C8 0.139(15) 0.109(11) 0.179(12) 0.005(9) 0.021(9) 0.004(10) C11 0.113(12) 0.094(9) 0.144(14) 0.005(8) 0.015(10) 0.000(9) C17 0.26(3) 0.14(2) 0.26(4) 0.03(2) 0.01(2) -0.03(2) C19 0.144(14) 0.136(15) 0.22(2) 0.003(14) 0.047(14) -0.026(11) C14 0.106(11) 0.102(9) 0.163(17) 0.010(8) 0.013(10) -0.007(8) C15 0.107(11) 0.103(9) 0.129(16) 0.009(9) 0.007(9) -0.011(8) C1AA 0.112(12) 0.107(10) 0.177(19) 0.012(10) 0.004(10) -0.011(8) C0AA 0.130(12) 0.096(10) 0.21(2) -0.001(10) 0.019(12) -0.005(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0010 0.0010 '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' O O 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0310 0.0240 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O1 Al1 O1 101.6(8) 8_666 . O1 Al1 O10 97.5(5) . . O1 Al1 O10 85.2(5) . 8_666 O1 Al1 O10 85.2(5) 8_666 . O1 Al1 O10 97.5(5) 8_666 8_666 O1 Al1 O7 84.3(5) 8_666 2_645 O1 Al1 O7 84.3(5) . 6_645 O1 Al1 O7 169.9(6) 8_666 6_645 O1 Al1 O7 169.9(6) . 2_645 O10 Al1 O10 175.8(7) . 8_666 O10 Al1 O7 85.9(6) . 6_645 O10 Al1 O7 85.9(6) 8_666 2_645 O10 Al1 O7 91.1(6) 8_666 6_645 O10 Al1 O7 91.1(6) . 2_645 O7 Al1 O7 91.0(8) 2_645 6_645 O2 Al2 O1 96.6(5) . . O2 Al2 O8 176.4(6) . 6_645 O2 Al2 O5 92.0(4) . 5_455 O2 Al2 O9 90.0(4) . . O3 Al2 O2 97.0(5) . . O3 Al2 O1 166.4(5) . . O3 Al2 O8 86.5(6) . 6_645 O3 Al2 O5 101.9(6) . 5_455 O3 Al2 O9 80.7(6) . . O8 Al2 O1 79.9(5) 6_645 . O8 Al2 O5 86.8(4) 6_645 5_455 O8 Al2 O9 91.1(5) 6_645 . O5 Al2 O1 78.5(5) 5_455 . O9 Al2 O1 98.4(6) . . O9 Al2 O5 176.5(6) . 5_455 O2 Al3 O2 86.2(6) . 3_665 O2 Al3 O6 90.4(4) . 6_655 O2 Al3 O6 92.4(4) 3_665 6_655 O2 Al3 O6 90.4(4) 3_665 5_455 O2 Al3 O6 92.4(4) . 5_455 O4 Al3 O2 174.6(5) . 3_665 O4 Al3 O2 98.8(4) 3_665 3_665 O4 Al3 O2 98.8(4) . . O4 Al3 O2 174.6(5) 3_665 . O4 Al3 O4 76.2(7) . 3_665 O4 Al3 O6 85.8(4) . 6_655 O4 Al3 O6 85.8(4) 3_665 5_455 O4 Al3 O6 91.2(4) 3_665 6_655 O4 Al3 O6 91.2(4) . 5_455 O6 Al3 O6 176.2(7) 5_455 6_655 Al2 O2 Al3 122.3(5) . . C1 O3 Al2 129.5(9) . . Al1 O1 Al2 122.8(6) . . C1 O4 Al3 136.6(10) . . O4 C1 O3 117.8(14) . . C2 C1 O3 120.4(13) . . C2 C1 O4 120.3(14) . . C22 C23 C24 120.0 . . C23 C22 C21 120.0 . . C22 C21 C26 120.0 . . C22 C21 C12 121.0(14) . . C26 C21 C12 119.0(14) . . C21 C26 C25 120.0 . . C24 C25 C26 120.0 . . C23 C24 C27 108.9(12) . . C25 C24 C23 120.0 . . C25 C24 C27 130.2(12) . . O5 C20 C0AA 104.5(14) . . O6 C20 O5 118.3(16) . . O6 C20 C0AA 119.3(16) . . O8 C27 C24 97.0(16) . . O7 C27 C24 115(3) . . O7 C27 O8 139(3) . . C44 C6 C2 120.0 . . C5 C44 C6 120.0 . . C44 C5 C4 120.0 . . C44 C5 C8 119.6(14) . . C4 C5 C8 119.9(14) . . C5 C4 C3 120.0 . . C4 C3 C2 120.0 . . C1 C2 C6 119.2(13) . . C1 C2 C3 120.7(13) . . C3 C2 C6 120.0 . . C12 C13 C8 131(2) . . C9 C10 C14 115.8(15) . . C11 C10 C9 127(2) . . C11 C10 C14 116(2) . . C13 C12 C21 120.8(18) . . C13 C12 C11 116.3(18) . . C11 C12 C21 121.6(18) . . C10 C9 C8 118.9(15) . . C27 O8 Al2 129.0(15) . 6_655 C28 O10 Al1 136.3(10) . . C20 O5 Al2 121.9(10) . 5 C20 O6 Al3 130.9(10) . 5 C27 O7 Al1 121(3) . 4_564 C28 O9 Al2 130.7(14) . . O9 C28 O10 126.2(17) . . C5 C8 C9 121.7(17) . . C13 C8 C5 130.9(19) . . C13 C8 C9 103(2) . . C10 C11 C12 117(2) . . C19 C17 C0AA 120.0 . . C17 C19 C14 120.0 . . C19 C14 C10 120.5(11) . . C15 C14 C10 119.1(12) . . C15 C14 C19 120.0 . . C14 C15 C1AA 120.0 . . C0AA C1AA C15 120.0 . . C17 C0AA C20 124.4(13) . . C1AA C0AA C20 114.8(13) . . C1AA C0AA C17 120.0 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Al1 O1 1.771(11) 8_666 Al1 O1 1.771(11) . Al1 O10 1.890(10) . Al1 O10 1.890(10) 8_666 Al1 O7 2.045(18) 2_645 Al1 O7 2.045(18) 6_645 Al2 O2 1.865(8) . Al2 O3 1.818(13) . Al2 O1 2.080(12) . Al2 O8 1.871(9) 6_645 Al2 O5 2.039(10) 5_455 Al2 O9 1.883(12) . Al3 O2 1.923(10) 3_665 Al3 O2 1.923(10) . Al3 O4 1.751(11) . Al3 O4 1.751(11) 3_665 Al3 O6 1.933(8) 6_655 Al3 O6 1.933(8) 5_455 O3 C1 1.530(18) . O4 C1 1.407(14) . C1 C2 1.341(18) . C23 C22 1.3900 . C23 C24 1.3900 . C22 C21 1.3900 . C21 C26 1.3900 . C21 C12 1.511(19) . C26 C25 1.3900 . C25 C24 1.3900 . C24 C27 1.80(2) . C20 O5 1.413(19) . C20 O6 1.296(17) . C20 C0AA 1.429(17) . C27 O8 1.26(2) . C27 O7 0.86(3) . C6 C44 1.3900 . C6 C2 1.3900 . C44 C5 1.3900 . C5 C4 1.3900 . C5 C8 1.47(2) . C4 C3 1.3900 . C3 C2 1.3900 . C13 C12 1.36(2) . C13 C8 1.42(2) . C10 C9 1.47(2) . C10 C11 1.169(18) . C10 C14 1.487(17) . C12 C11 1.47(2) . C9 C8 1.51(2) . O8 Al2 1.871(9) 6_655 O10 C28 1.351(18) . O5 Al2 2.039(10) 5 O6 Al3 1.933(8) 5 O7 Al1 2.045(18) 4_564 O9 C28 1.193(18) . C17 C19 1.3900 . C17 C0AA 1.3900 . C19 C14 1.3900 . C14 C15 1.3900 . C15 C1AA 1.3900 . C1AA C0AA 1.3900 . 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 -0.761 -0.155 -0.040 9653.7 15064.2