#------------------------------------------------------------------------------ #$Date: 2026-09-24 07:48:01 +0100 (Thu, 24 Sep 2026) $ #$Revision: 306902 $ #$URL: svn://www.crystallography.net/cod/cif/4/51/95/4519540.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_4519540 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 'C34 H21 Al2 O10' _chemical_formula_sum 'C34 H21 Al2 O10' _chemical_formula_weight 643.47 _chemical_name_common 'MOF-520-BPDC_3.32 GPa' _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 geom _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 19.0287(13) _cell_length_b 19.0287(13) _cell_length_c 36.5400(17) _cell_measurement_reflns_used 6601 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 15.04 _cell_measurement_theta_min 2.27 _cell_volume 13230.8(14) _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 0.604 _diffrn_measured_fraction_theta_max 0.886 _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 0.0514 _diffrn_reflns_av_unetI/netI 0.0564 _diffrn_reflns_Laue_measured_fraction_full 0.604 _diffrn_reflns_Laue_measured_fraction_max 0.886 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_number 19092 _diffrn_reflns_point_group_measured_fraction_full 0.583 _diffrn_reflns_point_group_measured_fraction_max 0.869 _diffrn_reflns_theta_full 17.311 _diffrn_reflns_theta_max 15.108 _diffrn_reflns_theta_min 0.842 _diffrn_source ; Advanced Light Source, station 12.2.2 ; _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.032 _exptl_absorpt_correction_T_max 0.7439 _exptl_absorpt_correction_T_min 0.6484 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0980 before and 0.0588 after correction. The Ratio of minimum to maximum transmission is 0.8716. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 0.646 _exptl_crystal_description block _exptl_crystal_F_000 2648 _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.294 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.045 _refine_ls_abs_structure_details ; Flack x determined using 2296 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.9(2) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 416 _refine_ls_number_reflns 6997 _refine_ls_number_restraints 387 _refine_ls_restrained_S_all 1.084 _refine_ls_R_factor_all 0.0616 _refine_ls_R_factor_gt 0.0508 _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^)+(0.1000P)^2^+0.4790P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1443 _refine_ls_wR_factor_ref 0.1546 _reflns_Friedel_coverage 0.716 _reflns_Friedel_fraction_full 0.557 _reflns_Friedel_fraction_max 0.847 _reflns_number_gt 5936 _reflns_number_total 6997 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file oc7b00169_si_003.cif _cod_data_source_block MOF520_BPDC_3.32GPa _cod_original_cell_volume 13230.8(19) _cod_database_code 4519540 _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 0.7439 _shelx_estimated_absorpt_t_min 0.6484 _exptl_absorpt_special_details ; Data was collected in a Merril Bassett DAC. DAC opening angle of 40 degrees. The pressure of 3.32 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, All O(H) groups 2. Rigid body (RIGU) restrains Al1, Al2, Al3, O2, H2, O3, O1, H1, O4, C1, C26, H26, C23, H23, C20, C25, H25, C22, H22, C24, C27, C17, C7, H7, C21, C5, C16, H16, C8, C2, C18, H18, C3, H3, C4, H4, C14, C6, H6, C13, H13, C19, H19, C10, C15, H15, C12, C11, H11, C9, H9, O8, O10, O5, O6, O9, O7, C28, C6G, H6G, C1G, C5G, H5G, C2G, H2G, C4G, C3G, H3G, Al1, O1, Al1, O10, Al2, O1, O1, H1, O10, C28, Al2, O2, Al2, O3, Al2, O9, O9, C28, C28, C1G, Al3, O2, O2, H2, O3, C1, C6G, C1G, C2G, C1G, Al3, O4, O4, C1, C2, C1, C6G, H6G, C6G, C5G, C2G, H2G, C3G, C2G, C7, C2, C3, C2, C5G, H5G, C5G, C4G, C4G, C3G, C3G, H3G, C7, H7, C7, C6, C3, H3, C4, C3, C6, C5, C6, H6, C5, C4, C4, H4, C8, C5, C8, C13, C9, C8, C13, H13, C13, C12, C9, C10, C9, H9, C21, C12, C12, C11, C14, C10, C11, C10, C26, C21, C22, C21, C11, H11, C19, C14, C15, C14, C26, H26, C26, C25, C23, C22, C22, H22, C19, C18, C19, H19, C16, C15, C15, H15, C25, H25, C25, C24, C23, H23, C24, C23, C18, C17, C18, H18, C17, C16, C16, H16, C27, C24, C20, C17, 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 3.a Aromatic/amide H refined with riding coordinates: O2(H2), O1(H1), C26(H26), C23(H23), C25(H25), C22(H22), C7(H7), C16(H16), C18(H18), C3(H3), C4(H4), C6(H6), C13(H13), C19(H19), C15(H15), C11(H11), C9(H9), C6G(H6G), C5G(H5G), C2G(H2G), C3G(H3G) ; _shelx_res_file ; TITL P10_25kev_0m in P42212 #94 REM reset to P42212 #94 CELL 0.49594 19.0287 19.0287 36.54 90 90 90 ZERR 8 0.0013 0.0013 0.0017 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 272 168 80 16 RIGU Al1 Al2 Al3 O2 H2 O3 O1 H1 O4 C1 C26 H26 C23 H23 C20 C25 H25 C22 H22 = C24 C27 C17 C7 H7 C21 C5 C16 H16 C8 C2 C18 H18 C3 H3 C4 H4 C14 C6 H6 C13 H13 = C19 H19 C10 C15 H15 C12 C11 H11 C9 H9 O8 O10 O5 O6 O9 O7 C28 C6G H6G C1G C5G = H5G C2G H2G C4G C3G H3G AL1 O1 AL1 O10 AL2 O1 O1 H1 O10 C28 AL2 O2 AL2 O3 = AL2 O9 O9 C28 C28 C1G AL3 O2 O2 H2 O3 C1 C6G C1G C2G C1G AL3 O4 O4 C1 C2 C1 = C6G H6G C6G C5G C2G H2G C3G C2G C7 C2 C3 C2 C5G H5G C5G C4G C4G C3G C3G H3G = C7 H7 C7 C6 C3 H3 C4 C3 C6 C5 C6 H6 C5 C4 C4 H4 C8 C5 C8 C13 C9 C8 C13 H13 = C13 C12 C9 C10 C9 H9 C21 C12 C12 C11 C14 C10 C11 C10 C26 C21 C22 C21 C11 H11 = C19 C14 C15 C14 C26 H26 C26 C25 C23 C22 C22 H22 C19 C18 C19 H19 C16 C15 C15 = H15 C25 H25 C25 C24 C23 H23 C24 C23 C18 C17 C18 H18 C17 C16 C16 H16 C27 C24 = C20 C17 O8 C27 O7 C27 O5 C20 O6 C20 L.S. 24 PLAN 20 TEMP 23 BOND ACTA ABIN fmap 2 REM REM REM WGHT 0.100000 0.479000 FVAR 0.10387 AL1 4 0.664532 0.335468 0.500000 10.50000 0.02082 0.02082 = 0.01450 -0.00388 -0.00388 0.00465 AL2 4 0.618020 0.387409 0.416976 11.00000 0.01906 0.01755 = 0.01378 0.00291 0.00088 0.00265 AL3 4 0.500000 0.500000 0.385476 10.50000 0.01475 0.02027 = 0.01358 0.00000 0.00000 0.00197 O2 3 0.567123 0.471859 0.417635 11.00000 0.01635 0.01124 = 0.00976 -0.00125 -0.00326 0.01189 AFIX 43 H2 2 0.577437 0.502823 0.436580 11.00000 -1.20000 AFIX 0 O3 3 0.641362 0.395738 0.365928 11.00000 0.02451 0.03743 = 0.02165 0.00232 0.00430 0.00825 O1 3 0.602074 0.365712 0.465150 11.00000 0.01270 0.02344 = 0.00959 0.00489 -0.00575 0.00648 AFIX 43 H1 2 0.555868 0.370740 0.473019 11.00000 -1.20000 AFIX 0 O4 3 0.557245 0.472618 0.345426 11.00000 0.03894 0.05546 = 0.01278 -0.00166 0.00156 0.02161 C1 1 0.612180 0.436625 0.340521 11.00000 0.03078 0.03606 = 0.01324 0.00627 0.00855 0.00455 C26 1 0.763595 0.628371 0.139630 11.00000 0.08347 0.02999 = 0.01761 0.00619 0.00025 -0.00796 AFIX 43 H26 2 0.759961 0.627912 0.165010 11.00000 -1.20000 AFIX 0 C23 1 0.770012 0.632813 0.064758 11.00000 0.08151 0.02745 = 0.02269 0.00085 0.00698 -0.00812 AFIX 43 H23 2 0.768005 0.634054 0.039336 11.00000 -1.20000 AFIX 0 C20 1 0.978805 0.151833 0.110713 11.00000 0.02688 0.01501 = 0.00474 -0.00511 0.00138 -0.00438 C25 1 0.774692 0.690755 0.123168 11.00000 0.06058 0.02913 = 0.02314 0.00086 0.00524 -0.00795 AFIX 43 H25 2 0.778077 0.731933 0.136763 11.00000 -1.20000 AFIX 0 C22 1 0.761534 0.567817 0.084860 11.00000 0.09200 0.02509 = 0.03636 0.00171 0.02126 -0.00594 AFIX 43 H22 2 0.759068 0.526355 0.071447 11.00000 -1.20000 AFIX 0 C24 1 0.781016 0.691770 0.084760 11.00000 0.04842 0.03136 = 0.02158 -0.00009 0.01320 -0.00216 C27 1 0.804595 0.756821 0.066020 11.00000 0.02689 0.02176 = 0.02426 0.00671 0.00383 0.00101 C17 1 0.932796 0.207932 0.118683 11.00000 0.03197 0.02183 = 0.02393 -0.00514 0.00813 -0.00419 C7 1 0.605929 0.470001 0.276664 11.00000 0.06113 0.06753 = 0.01323 0.01095 0.02248 0.03505 AFIX 43 H7 2 0.565150 0.494735 0.282223 11.00000 -1.20000 AFIX 0 C21 1 0.757039 0.563042 0.120864 11.00000 0.04980 0.02961 = 0.03245 0.00185 0.01058 -0.00563 C5 1 0.692813 0.432768 0.231480 11.00000 0.06042 0.04362 = 0.02405 0.01811 0.01983 0.02131 C16 1 0.864585 0.200557 0.137513 11.00000 0.03613 0.02170 = 0.05938 -0.00414 0.02568 -0.01156 AFIX 43 H16 2 0.851009 0.155543 0.144462 11.00000 -1.20000 AFIX 0 C8 1 0.728050 0.433694 0.197100 11.00000 0.07454 0.02853 = 0.03262 0.01275 0.02948 0.02283 C2 1 0.640551 0.429684 0.302893 11.00000 0.03636 0.02305 = 0.02354 0.00085 0.01064 0.00386 C18 1 0.948646 0.280467 0.110221 11.00000 0.03725 0.02292 = 0.04133 -0.00283 0.01537 -0.00531 AFIX 43 H18 2 0.990209 0.291128 0.098035 11.00000 -1.20000 AFIX 0 C3 1 0.697528 0.387978 0.296246 11.00000 0.10042 0.10229 = 0.03033 0.03425 0.04273 0.06583 AFIX 43 H3 2 0.716072 0.358716 0.314199 11.00000 -1.20000 AFIX 0 C4 1 0.725774 0.391258 0.262233 11.00000 0.05996 0.06436 = 0.03195 0.02198 0.02320 0.03297 AFIX 43 H4 2 0.767221 0.366905 0.257643 11.00000 -1.20000 AFIX 0 C14 1 0.840772 0.319916 0.137586 11.00000 0.04069 0.03481 = 0.03996 -0.00012 0.02483 -0.00102 C6 1 0.635792 0.471593 0.241023 11.00000 0.08121 0.08533 = 0.03984 0.02076 0.02510 0.05037 AFIX 43 H6 2 0.615390 0.500492 0.223461 11.00000 -1.20000 AFIX 0 C13 1 0.722848 0.493227 0.174578 11.00000 0.04721 0.02286 = 0.03439 0.00154 0.01841 0.00482 AFIX 43 H13 2 0.697101 0.531538 0.182942 11.00000 -1.20000 AFIX 0 C19 1 0.905093 0.332454 0.119470 11.00000 0.04262 0.03116 = 0.03324 0.00550 0.02340 0.00103 AFIX 43 H19 2 0.917506 0.378453 0.113799 11.00000 -1.20000 AFIX 0 C10 1 0.796736 0.381052 0.149147 11.00000 0.04465 0.03746 = 0.03044 0.00126 0.02129 0.00111 C15 1 0.824532 0.248719 0.144710 11.00000 0.04407 0.02778 = 0.04640 0.00021 0.03544 -0.00180 AFIX 43 H15 2 0.781422 0.238108 0.155350 11.00000 -1.20000 AFIX 0 C12 1 0.753941 0.497478 0.140862 11.00000 0.05663 0.03397 = 0.03034 -0.00085 0.01459 -0.00545 C11 1 0.793848 0.441845 0.129098 11.00000 0.05492 0.03846 = 0.02834 0.00112 0.02581 -0.00587 AFIX 43 H11 2 0.819096 0.445411 0.107385 11.00000 -1.20000 AFIX 0 C9 1 0.763297 0.372688 0.183026 11.00000 0.06603 0.03175 = 0.03434 0.00786 0.03377 0.00980 AFIX 43 H9 2 0.763891 0.330230 0.195627 11.00000 -1.20000 AFIX 0 O8 3 0.826500 0.805545 0.088175 11.00000 0.04153 0.02855 = 0.02328 0.00057 0.00323 -0.01704 O10 3 0.734877 0.394961 0.481636 11.00000 0.01746 0.04633 = 0.02833 0.00579 0.00086 0.00235 O5 3 1.039498 0.165408 0.097671 11.00000 0.02239 0.02344 = 0.02940 0.00666 0.01437 0.00360 O6 3 0.957785 0.090598 0.116945 11.00000 0.02071 0.01496 = 0.03759 -0.00318 0.01224 0.00379 O9 3 0.705481 0.437094 0.425868 11.00000 0.01131 0.02592 = 0.03069 0.00764 -0.00006 -0.00781 O7 3 0.800724 0.760242 0.032529 11.00000 0.04808 0.02432 = 0.01723 0.00264 0.00149 -0.02229 C28 1 0.747461 0.426300 0.451619 11.00000 0.01723 0.02722 = 0.02970 -0.01065 0.00054 0.01085 C6G 1 0.849647 0.480598 0.417670 11.00000 0.03468 0.06272 = 0.04738 -0.00435 0.00009 0.00009 AFIX 43 H6G 2 0.821512 0.489869 0.397427 11.00000 -1.20000 AFIX 0 C1G 1 0.821046 0.451863 0.448161 11.00000 0.02181 0.04730 = 0.03560 -0.01244 -0.00222 0.00492 C5G 1 0.918063 0.495596 0.416649 11.00000 0.03715 0.12959 = 0.05186 -0.00309 -0.00497 -0.01460 AFIX 43 H5G 2 0.938006 0.509733 0.394610 11.00000 -1.20000 AFIX 0 C2G 1 0.863952 0.441436 0.478823 11.00000 0.01973 0.10688 = 0.05128 0.00182 -0.00972 -0.00060 AFIX 43 H2G 2 0.843072 0.429064 0.500914 11.00000 -1.20000 AFIX 0 C4G 1 0.959482 0.490871 0.446769 11.00000 0.03471 0.12534 = 0.04717 -0.00814 -0.00727 -0.01129 C3G 1 0.936255 0.448850 0.477484 11.00000 0.02973 0.18494 = 0.06422 0.02027 -0.01149 -0.00953 AFIX 43 H3G 2 0.966665 0.428956 0.494503 11.00000 -1.20000 AFIX 0 HKLF 4 REM P10_25kev_0m in P42212 #94 REM R1 = 0.0508 for 5936 Fo > 4sig(Fo) and 0.0616 for all 6997 data REM 416 parameters refined using 387 restraints END WGHT 0.1003 0.4874 REM Highest difference peak 0.294, deepest hole -0.337, 1-sigma level 0.045 Q1 1 1.0255 0.1680 0.0882 11.00000 0.05 0.22 Q2 1 0.7220 0.4289 0.4162 11.00000 0.05 0.20 Q3 1 0.7397 0.5759 0.0385 11.00000 0.05 0.19 Q4 1 0.8693 0.4671 0.4822 11.00000 0.05 0.19 Q5 1 0.6257 0.4669 0.4092 11.00000 0.05 0.17 Q6 1 0.5683 0.4968 0.4167 11.00000 0.05 0.17 Q7 1 0.9393 0.4648 0.4746 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-6.6316 16 8 6 -1.3673 4.2551 16 8 7 -4.4608 5.4569 16 8 8 -0.8305 1.5646 16 8 9 0.4084 9.2979 16 8 10 10.3616 1.9971 16 8 11 -3.7639 -1.3652 16 8 12 -1.2535 -2.0369 16 8 13 4.6299 0.0004 16 8 14 1.4600 -5.0285 16 8 15 5.4167 2.2002 16 8 16 0.1066 -1.8089 16 8 17 -2.1170 1.9475 16 9 0 -5.9523 -0.0000 16 9 1 -49.0053 2.7103 16 9 2 0.1979 29.0355 16 9 14 -0.9872 2.3783 16 9 15 0.1612 12.2524 17 0 1 -1.4673 0.0000 17 0 2 0.0000 18.1336 17 0 3 5.4007 0.0000 17 0 4 0.0000 3.2457 17 0 5 -6.2055 0.0000 17 0 6 -0.0000 -8.7558 17 0 7 -5.2927 -0.0000 17 0 8 -0.0000 -1.6039 17 0 9 -2.3416 -0.0000 17 0 10 -0.0000 -4.1244 17 0 11 0.7838 0.0000 17 0 12 0.0000 9.1621 17 0 13 1.0877 0.0000 17 0 14 -0.0000 -6.2222 17 0 15 3.2110 -0.0000 17 0 16 0.0000 9.7400 17 0 17 1.1196 -0.0000 17 0 18 -0.0000 -4.8013 17 0 19 -1.2075 -0.0000 17 0 20 -0.0000 -4.7194 17 1 0 -5.5018 -0.0000 17 1 1 6.7035 -0.4228 17 1 2 10.0384 -5.2082 17 1 3 -3.8350 -2.3817 17 1 4 -6.4855 -7.5449 17 1 5 -5.1686 -2.8260 17 1 6 -3.3671 -7.5888 17 1 7 -4.6333 1.4530 17 1 8 3.7746 0.2987 17 1 9 -0.9059 0.2894 17 1 10 2.2738 2.6532 17 1 11 1.6627 -1.3580 17 1 12 -0.8733 4.6319 17 1 13 -3.5380 -2.4157 17 1 14 3.5368 -1.2652 17 1 15 0.9212 0.4937 17 1 16 1.9412 6.8531 17 1 17 2.4849 -3.6646 17 1 18 -2.2055 2.9104 17 1 19 1.0692 1.0824 17 1 20 2.2308 3.5408 17 2 0 10.0308 0.0000 17 2 1 14.5045 7.2959 17 2 2 3.4260 0.4287 17 2 3 1.6041 11.9741 17 2 4 2.4781 -1.4909 17 2 5 5.7757 1.4765 17 2 6 -4.2511 -2.5654 17 2 7 3.6083 -3.9529 17 2 8 -9.8814 -2.1710 17 2 9 0.2828 -2.3528 17 2 10 3.4153 -7.5395 17 2 11 1.1698 -9.1009 17 2 12 -5.6305 4.7240 17 2 13 5.4031 0.6399 17 2 14 5.1622 -1.3995 17 2 15 0.3512 -2.4805 17 2 16 9.2740 -3.5938 17 2 17 1.2149 2.7463 17 2 18 1.7410 2.7311 17 2 19 -0.4161 -6.6601 17 3 0 0.3446 -0.0000 17 3 1 1.9544 -0.7679 17 3 2 -1.7036 -3.5553 17 3 3 6.0289 6.1525 17 3 4 5.8103 2.9905 17 3 5 3.6206 -12.0093 17 3 6 1.3661 6.5943 17 3 7 -4.5329 2.5781 17 3 8 13.6680 -4.6365 17 3 9 -7.0851 5.0416 17 3 10 7.2663 1.2280 17 3 11 -4.4429 -5.2023 17 3 12 6.7668 9.1814 17 3 13 3.7128 -6.4614 17 3 14 0.1094 -0.9885 17 3 15 1.4252 -0.5451 17 3 16 1.0125 -6.0124 17 3 17 -2.4386 -0.5568 17 3 18 -1.2481 -2.3112 17 3 19 -1.0512 -1.1331 17 4 0 15.2345 -0.0000 17 4 1 4.1799 1.8290 17 4 2 11.4078 -2.0160 17 4 3 9.1947 5.6048 17 4 4 5.4669 -1.8542 17 4 5 4.7962 2.3515 17 4 6 2.1931 -3.7721 17 4 7 8.7204 -12.2629 17 4 8 0.7394 2.2607 17 4 9 -0.8189 8.2686 17 4 10 0.7252 -3.0766 17 4 11 -3.6011 -2.3691 17 4 12 -4.1123 -0.9011 17 4 13 1.3961 -4.8107 17 4 14 -0.6607 1.6005 17 4 15 -3.1121 2.1144 17 4 16 -1.4488 -6.8129 17 4 17 3.7160 0.3977 17 4 18 -1.2718 3.3876 17 5 0 10.3300 -0.0000 17 5 1 -10.1880 -5.1397 17 5 2 1.4705 -5.3756 17 5 3 8.9544 -1.7981 17 5 4 7.6782 2.8553 17 5 5 -0.1576 -2.7718 17 5 6 5.7329 1.5762 17 5 7 -4.0477 -2.4983 17 5 8 -9.9032 7.4827 17 5 9 -2.9653 -1.0893 17 5 10 -0.0722 1.2428 17 5 11 4.1578 -2.7157 17 5 12 -4.0537 2.3503 17 5 13 0.5777 0.7915 17 5 14 1.0745 0.8839 17 5 15 -1.5705 10.4506 17 5 16 -0.3117 0.6005 17 5 17 1.6866 2.5735 17 6 0 -3.6464 0.0000 17 6 1 2.8181 8.3510 17 6 2 -6.8222 3.4287 17 6 3 -9.1410 1.9116 17 6 4 -0.9459 -3.1327 17 6 5 -1.6923 6.7417 17 6 6 -2.3545 12.3902 17 6 7 -8.1357 0.5326 17 6 8 -8.0637 -0.0962 17 6 9 -0.5377 6.0944 17 6 10 3.6500 -4.5202 17 6 11 1.9076 3.4937 17 6 12 -4.7096 5.0743 17 6 13 -4.4209 4.3378 17 6 14 -4.3519 -2.3103 17 6 15 -0.0746 3.1439 17 6 16 0.1308 -1.9414 17 7 0 -0.1787 0.0000 17 7 1 -0.6393 2.5671 17 7 2 -1.4298 1.8605 17 7 3 -10.4297 -3.7620 17 7 4 -0.6206 -8.4941 17 7 5 4.6997 -0.8661 17 7 6 1.2311 -2.3770 17 7 7 5.4819 -5.9133 17 7 8 1.3779 -4.9535 17 7 9 7.0894 -4.2355 17 7 10 1.5703 7.4936 17 7 11 0.6427 -0.5749 17 7 12 1.2511 3.0235 17 7 13 6.5621 3.0585 17 7 14 -0.3392 -8.0712 17 7 15 -1.1756 0.4894 17 8 0 3.6006 -0.0000 17 8 1 5.9480 1.7705 17 8 2 4.6921 -6.7296 17 8 3 -5.6896 7.3005 17 8 4 -2.2749 1.9179 17 8 5 -2.5980 5.6148 17 8 6 -2.6447 4.2625 17 8 7 5.9621 -0.1540 17 8 8 -2.4229 6.6504 17 8 9 -8.5916 4.6770 17 8 10 -1.1875 3.9149 17 8 11 6.2130 -1.5104 17 8 12 7.9667 4.1379 17 8 13 0.8956 -1.5278 17 9 0 -44.2415 0.0000 17 9 1 -12.4767 10.7584 17 9 2 -15.3858 4.1751 17 9 3 -5.5842 -2.4659 17 9 4 3.8387 -3.9517 18 0 0 -4.2522 0.0000 18 0 1 0.0000 7.1036 18 0 2 -10.7985 0.0000 18 0 3 -0.0000 -0.1168 18 0 4 -7.3966 0.0000 18 0 5 0.0000 0.8538 18 0 6 3.1518 -0.0000 18 0 7 -0.0000 -9.3054 18 0 8 4.7036 -0.0000 18 0 9 -0.0000 -2.7200 18 0 10 -0.3117 0.0000 18 0 11 -0.0000 -7.9095 18 0 12 4.5503 0.0000 18 0 13 -0.0000 -6.4822 18 0 14 -0.0837 -0.0000 18 0 15 0.0000 1.6370 18 0 16 7.1590 0.0000 18 1 0 -3.7106 0.0000 18 1 1 -2.1989 -2.4446 18 1 2 -10.4294 -0.7492 18 1 3 -3.6406 -4.4203 18 1 4 6.0163 -3.7178 18 1 5 2.0625 -0.7143 18 1 6 1.3456 0.9925 18 1 7 -1.4976 6.8013 18 1 8 -12.2550 -0.4273 18 1 9 4.1610 -5.9825 18 1 10 1.6718 0.5379 18 1 11 -2.6483 0.8816 18 1 12 -3.7139 -3.0470 18 1 13 7.7636 0.9985 18 1 14 -8.2043 0.6102 18 1 15 -1.9045 2.9174 18 1 16 1.6239 1.1742 18 2 0 -7.6766 -0.0000 18 2 1 2.5222 -1.1961 18 2 2 1.1487 -1.9095 18 2 3 5.0639 -0.8735 18 2 4 1.2885 2.7276 18 2 5 -13.6456 6.5660 18 2 6 4.3551 -4.3558 18 2 7 8.0779 -0.6014 18 2 8 2.5078 0.7630 18 2 9 -7.9080 2.8137 18 2 10 3.3794 -3.3979 18 2 11 1.9554 3.4048 18 2 12 6.1379 0.5933 18 2 13 2.6505 2.3668 18 2 14 -1.1693 4.6196 18 2 15 -4.2945 3.6280 18 2 16 -0.8036 2.0375 18 3 0 8.8269 -0.0000 18 3 1 12.1888 -6.5853 18 3 2 5.4812 -4.3192 18 3 3 10.3617 -3.4769 18 3 4 6.5275 -9.5481 18 3 5 0.1318 1.2867 18 3 6 -8.0676 -0.2469 18 3 7 4.0235 -1.3839 18 3 8 5.1122 1.3010 18 3 9 1.5435 -2.4523 18 3 10 -4.3730 1.1227 18 3 11 -0.5131 -0.1756 18 3 12 3.4498 3.3344 18 3 13 5.2641 -1.1094 18 3 14 1.5405 -2.8073 18 3 15 1.6307 -2.7446 18 4 0 2.2368 -0.0000 18 4 1 6.2879 0.7086 18 4 2 1.8490 6.0146 18 4 3 1.2344 2.7795 18 4 4 4.4650 10.2122 18 4 5 2.6006 -1.3443 18 4 6 -0.4594 6.2399 18 4 7 3.5253 -4.1145 18 4 8 0.4266 -4.1220 18 4 9 1.6762 2.0219 18 4 10 -6.9086 -2.4510 18 4 11 4.5145 -0.7723 18 4 12 2.2068 0.2717 18 4 13 -2.2134 1.7335 18 4 14 0.3165 1.9553 18 5 0 7.6953 -0.0000 18 5 1 8.4599 4.2921 18 5 2 5.7067 -4.7698 18 5 3 6.7862 -0.8175 18 5 4 -6.9221 1.8225 18 5 5 3.6861 -4.4185 18 5 6 1.4590 -2.7731 18 5 7 -3.8636 -0.8036 18 5 8 3.7136 -9.9172 18 5 9 -3.0997 0.1160 18 5 10 -0.8084 -1.4938 18 5 11 1.8616 -1.4204 18 5 12 -4.3036 -0.7315 18 5 13 -3.3101 1.5749 18 6 0 -1.7849 -0.0000 18 6 1 7.9116 -4.0694 18 6 2 -0.6428 4.3583 18 6 3 -3.2768 -2.6066 18 6 4 -6.1347 1.2536 18 6 5 2.3540 -0.4397 18 6 6 -1.0865 1.5143 18 6 7 -2.9937 -0.4349 18 6 8 -3.0276 -0.2555 18 6 9 2.3814 -0.8750 18 6 10 3.4733 2.4363 18 6 11 -3.8116 0.6455 18 6 12 -1.9435 -6.4239 18 7 0 -6.0379 -0.0000 18 7 1 2.2808 -8.1886 18 7 2 -6.4667 -4.7874 18 7 3 9.2668 -8.0599 18 7 4 -1.2614 2.9268 18 7 5 -2.8807 -2.3946 18 7 6 3.4623 9.1070 18 7 7 1.0183 -3.7249 18 7 8 -2.1806 -2.9532 18 7 9 -0.4998 -6.1228 18 8 0 -2.6174 -0.0000 18 8 1 4.6401 9.0804 18 8 2 -1.0770 -4.6780 18 8 3 7.0669 1.6351 18 8 4 -4.2436 5.6196 18 8 5 -3.8306 5.2529 18 8 6 3.6312 -6.2453 19 0 1 -6.4823 0.0000 19 0 2 -0.0000 -14.0764 19 0 3 5.3378 0.0000 19 0 4 -0.0000 -0.1231 19 0 5 1.8014 -0.0000 19 0 6 0.0000 8.1394 19 0 7 -1.8392 0.0000 19 0 8 0.0000 1.7285 19 0 9 3.8045 -0.0000 19 0 10 -0.0000 -5.3534 19 0 11 4.9558 0.0000 19 0 12 0.0000 2.2900 19 1 0 -1.2137 -0.0000 19 1 1 -3.3060 -0.8899 19 1 2 -6.9470 2.8235 19 1 3 -0.7088 1.4628 19 1 4 0.0626 4.5591 19 1 5 -2.7091 -2.9739 19 1 6 6.0979 -0.4744 19 1 7 -8.7787 2.0127 19 1 8 4.3669 -7.5378 19 1 9 2.2153 -2.8962 19 1 10 3.1266 -4.4632 19 1 11 1.7290 6.0640 19 2 0 0.4788 -0.0000 19 2 1 -6.7147 1.8081 19 2 2 -9.3612 -2.0205 19 2 3 4.5185 2.0551 19 2 4 1.6995 -0.4646 19 2 5 -2.3961 0.5880 19 2 6 -3.9984 -1.2412 19 2 7 -1.7815 -3.2773 19 2 8 2.7020 -0.1549 19 2 9 0.8053 2.7599 19 2 10 1.4596 -1.0067 19 2 11 2.7285 -3.7260 19 3 0 1.8249 -0.0000 19 3 1 -0.1038 -3.1636 19 3 2 1.9127 0.5617 19 3 3 -4.4432 3.9168 19 3 4 -3.7124 1.9844 19 3 5 3.3820 0.2866 19 3 6 2.9012 2.0884 19 3 7 2.4629 3.0983 19 3 8 -2.6840 2.3563 19 3 9 0.7862 -5.5773 19 3 10 0.5738 3.8864 19 4 0 0.7274 -0.0000 19 4 1 6.3365 1.0104 19 4 2 2.0901 2.2342 19 4 3 5.5964 1.0983 19 4 4 2.4370 -0.1901 19 4 5 0.8327 -8.2094 19 4 6 0.4390 3.4525 19 4 7 4.1927 -3.0432 19 4 8 4.2150 -1.8914 19 4 9 -0.3779 1.7784 19 5 0 5.0711 0.0000 19 5 1 1.6162 5.2047 19 5 2 -10.3619 -4.4320 19 5 3 5.9649 0.4179 19 5 4 9.8703 -5.1059 19 5 5 4.9482 1.3632 19 5 6 -4.1263 6.2501 19 5 7 0.7798 -3.0601 19 6 0 -6.0295 -0.0000 19 6 1 4.0902 3.1990 19 6 2 2.6633 5.8504 19 6 3 -6.0961 -1.0410 20 0 0 -1.8342 -0.0000 0 0 0 0.0 0.0 ; _shelx_fab_checksum 26902 _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 0.66453(8) 0.33547(8) 0.5000 0.0187(5) Uani 1 2 d S TU P . . Al2 Al 0.61802(8) 0.38741(8) 0.41698(3) 0.0168(4) Uani 1 1 d . U . . . Al3 Al 0.5000 0.5000 0.38548(4) 0.0162(5) Uani 1 2 d S TU P . . O2 O 0.56712(17) 0.47186(16) 0.41764(7) 0.0125(8) Uani 1 1 d . U . . . H2 H 0.5774 0.5028 0.4366 0.015 Uiso 1 1 calc R U . . . O3 O 0.64136(19) 0.3957(2) 0.36593(8) 0.0279(10) Uani 1 1 d . U . . . O1 O 0.60207(17) 0.36571(17) 0.46515(7) 0.0152(8) Uani 1 1 d . U . . . H1 H 0.5559 0.3707 0.4730 0.018 Uiso 1 1 calc R U . . . O4 O 0.5572(2) 0.4726(2) 0.34543(8) 0.0357(11) Uani 1 1 d . U . . . C1 C 0.6122(3) 0.4366(3) 0.34052(12) 0.0267(14) Uani 1 1 d . U . . . C26 C 0.7636(4) 0.6284(3) 0.13963(13) 0.0437(18) Uani 1 1 d . U . . . H26 H 0.7600 0.6279 0.1650 0.052 Uiso 1 1 calc R U . . . C23 C 0.7700(4) 0.6328(3) 0.06476(14) 0.0439(18) Uani 1 1 d . U . . . H23 H 0.7680 0.6341 0.0393 0.053 Uiso 1 1 calc R U . . . C20 C 0.9788(3) 0.1518(3) 0.11071(10) 0.0155(12) Uani 1 1 d . U . . . C25 C 0.7747(4) 0.6908(3) 0.12317(13) 0.0376(16) Uani 1 1 d . U . . . H25 H 0.7781 0.7319 0.1368 0.045 Uiso 1 1 calc R U . . . C22 C 0.7615(4) 0.5678(3) 0.08486(14) 0.051(2) Uani 1 1 d . U . . . H22 H 0.7591 0.5264 0.0714 0.061 Uiso 1 1 calc R U . . . C24 C 0.7810(3) 0.6918(3) 0.08476(13) 0.0338(15) Uani 1 1 d . U . . . C27 C 0.8046(3) 0.7568(3) 0.06602(12) 0.0243(13) Uani 1 1 d . U . . . C17 C 0.9328(3) 0.2079(3) 0.11868(12) 0.0259(13) Uani 1 1 d . U . . . C7 C 0.6059(4) 0.4700(4) 0.27666(12) 0.0473(19) Uani 1 1 d . U . . . H7 H 0.5652 0.4947 0.2822 0.057 Uiso 1 1 calc R U . . . C21 C 0.7570(4) 0.5630(3) 0.12086(13) 0.0373(15) Uani 1 1 d . U . . . C5 C 0.6928(4) 0.4328(3) 0.23148(13) 0.0427(17) Uani 1 1 d . U . . . C16 C 0.8646(3) 0.2006(3) 0.13751(15) 0.0391(16) Uani 1 1 d . U . . . H16 H 0.8510 0.1555 0.1445 0.047 Uiso 1 1 calc R U . . . C8 C 0.7280(4) 0.4337(3) 0.19710(14) 0.0452(19) Uani 1 1 d . U . . . C2 C 0.6406(3) 0.4297(3) 0.30289(13) 0.0276(13) Uani 1 1 d . U . . . C18 C 0.9486(3) 0.2805(3) 0.11022(13) 0.0338(15) Uani 1 1 d . U . . . H18 H 0.9902 0.2911 0.0980 0.041 Uiso 1 1 calc R U . . . C3 C 0.6975(4) 0.3880(5) 0.29625(15) 0.078(3) Uani 1 1 d . U . . . H3 H 0.7161 0.3587 0.3142 0.093 Uiso 1 1 calc R U . . . C4 C 0.7258(4) 0.3913(4) 0.26223(14) 0.052(2) Uani 1 1 d . U . . . H4 H 0.7672 0.3669 0.2576 0.063 Uiso 1 1 calc R U . . . C14 C 0.8408(3) 0.3199(3) 0.13759(14) 0.0385(16) Uani 1 1 d . U . . . C6 C 0.6358(4) 0.4716(4) 0.24102(16) 0.069(3) Uani 1 1 d . U . . . H6 H 0.6154 0.5005 0.2235 0.083 Uiso 1 1 calc R U . . . C13 C 0.7228(3) 0.4932(3) 0.17458(12) 0.0348(15) Uani 1 1 d . U . . . H13 H 0.6971 0.5315 0.1829 0.042 Uiso 1 1 calc R U . . . C19 C 0.9051(3) 0.3325(3) 0.11947(13) 0.0357(15) Uani 1 1 d . U . . . H19 H 0.9175 0.3785 0.1138 0.043 Uiso 1 1 calc R U . . . C10 C 0.7967(3) 0.3811(3) 0.14915(13) 0.0375(15) Uani 1 1 d . U . . . C15 C 0.8245(4) 0.2487(3) 0.14471(14) 0.0394(16) Uani 1 1 d . U . . . H15 H 0.7814 0.2381 0.1554 0.047 Uiso 1 1 calc R U . . . C12 C 0.7539(4) 0.4975(3) 0.14086(13) 0.0403(16) Uani 1 1 d . U . . . C11 C 0.7938(4) 0.4418(3) 0.12910(14) 0.0406(16) Uani 1 1 d . U . . . H11 H 0.8191 0.4454 0.1074 0.049 Uiso 1 1 calc R U . . . C9 C 0.7633(4) 0.3727(3) 0.18303(14) 0.0440(18) Uani 1 1 d . U . . . H9 H 0.7639 0.3302 0.1956 0.053 Uiso 1 1 calc R U . . . O8 O 0.8265(2) 0.8055(2) 0.08817(8) 0.0311(10) Uani 1 1 d . U . . . O10 O 0.73488(18) 0.3950(2) 0.48164(8) 0.0307(10) Uani 1 1 d . U . . . O5 O 1.03950(19) 0.16541(19) 0.09767(8) 0.0251(9) Uani 1 1 d . U . . . O6 O 0.9578(2) 0.09060(19) 0.11695(9) 0.0244(9) Uani 1 1 d . U . . . O9 O 0.70548(18) 0.4371(2) 0.42587(8) 0.0226(9) Uani 1 1 d . U . . . O7 O 0.8007(2) 0.76024(19) 0.03253(8) 0.0299(10) Uani 1 1 d . U . . . C28 C 0.7475(3) 0.4263(3) 0.45162(13) 0.0247(13) Uani 1 1 d . U . . . C6G C 0.8496(3) 0.4806(4) 0.41767(16) 0.0483(18) Uani 1 1 d . U . . . H6G H 0.8215 0.4899 0.3974 0.058 Uiso 1 1 calc R U . . . C1G C 0.8210(3) 0.4519(3) 0.44816(14) 0.0349(15) Uani 1 1 d . U . . . C5G C 0.9181(4) 0.4956(5) 0.41665(18) 0.073(3) Uani 1 1 d . U . . . H5G H 0.9380 0.5097 0.3946 0.087 Uiso 1 1 calc R U . . . C2G C 0.8640(3) 0.4414(5) 0.47882(17) 0.059(2) Uani 1 1 d . U . . . H2G H 0.8431 0.4291 0.5009 0.071 Uiso 1 1 calc R U . . . C4G C 0.9595(4) 0.4909(6) 0.44677(17) 0.069(2) Uani 1 1 d . U . . . C3G C 0.9363(4) 0.4488(6) 0.47748(19) 0.093(3) Uani 1 1 d . U . . . H3G H 0.9667 0.4290 0.4945 0.112 Uiso 1 1 calc R 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 0.0208(8) 0.0208(8) 0.0145(9) -0.0039(7) -0.0039(7) 0.0047(13) Al2 0.0191(9) 0.0175(9) 0.0138(6) 0.0029(6) 0.0009(6) 0.0026(9) Al3 0.0147(11) 0.0203(12) 0.0136(9) 0.000 0.000 0.0020(13) O2 0.0163(18) 0.0112(17) 0.0098(13) -0.0012(12) -0.0033(13) 0.0119(19) O3 0.025(2) 0.037(2) 0.0216(16) 0.0023(15) 0.0043(15) 0.008(2) O1 0.0127(17) 0.0234(19) 0.0096(14) 0.0049(13) -0.0057(12) 0.006(2) O4 0.039(2) 0.055(3) 0.0128(16) -0.0017(16) 0.0016(16) 0.022(3) C1 0.031(3) 0.036(3) 0.013(2) 0.006(2) 0.009(2) 0.005(3) C26 0.083(5) 0.030(3) 0.018(2) 0.006(2) 0.000(3) -0.008(4) C23 0.082(5) 0.027(3) 0.023(2) 0.001(2) 0.007(3) -0.008(4) C20 0.027(3) 0.015(3) 0.005(2) -0.0051(18) 0.0014(19) -0.004(3) C25 0.061(4) 0.029(3) 0.023(2) 0.001(2) 0.005(3) -0.008(4) C22 0.092(6) 0.025(3) 0.036(3) 0.002(2) 0.021(3) -0.006(4) C24 0.048(4) 0.031(3) 0.022(2) 0.000(2) 0.013(2) -0.002(3) C27 0.027(3) 0.022(3) 0.024(2) 0.007(2) 0.004(2) 0.001(3) C17 0.032(3) 0.022(3) 0.024(2) -0.005(2) 0.008(2) -0.004(3) C7 0.061(4) 0.068(4) 0.013(2) 0.011(3) 0.022(3) 0.035(4) C21 0.050(4) 0.030(3) 0.032(3) 0.002(2) 0.011(3) -0.006(4) C5 0.060(4) 0.044(4) 0.024(3) 0.018(2) 0.020(3) 0.021(4) C16 0.036(4) 0.022(3) 0.059(4) -0.004(3) 0.026(3) -0.012(3) C8 0.075(5) 0.029(3) 0.033(3) 0.013(2) 0.029(3) 0.023(4) C2 0.036(3) 0.023(3) 0.024(2) 0.001(2) 0.011(2) 0.004(3) C18 0.037(4) 0.023(3) 0.041(3) -0.003(2) 0.015(3) -0.005(3) C3 0.100(6) 0.102(6) 0.030(3) 0.034(4) 0.043(3) 0.066(6) C4 0.060(4) 0.064(5) 0.032(3) 0.022(3) 0.023(3) 0.033(5) C14 0.041(4) 0.035(3) 0.040(3) 0.000(3) 0.025(3) -0.001(3) C6 0.081(5) 0.085(6) 0.040(3) 0.021(3) 0.025(3) 0.050(6) C13 0.047(4) 0.023(3) 0.034(3) 0.002(2) 0.018(3) 0.005(3) C19 0.043(4) 0.031(3) 0.033(3) 0.006(3) 0.023(3) 0.001(3) C10 0.045(4) 0.037(3) 0.030(3) 0.001(2) 0.021(3) 0.001(4) C15 0.044(4) 0.028(3) 0.046(3) 0.000(3) 0.035(3) -0.002(4) C12 0.057(4) 0.034(3) 0.030(3) -0.001(2) 0.015(3) -0.005(4) C11 0.055(4) 0.038(3) 0.028(3) 0.001(2) 0.026(3) -0.006(4) C9 0.066(4) 0.032(3) 0.034(3) 0.008(2) 0.034(3) 0.010(4) O8 0.042(3) 0.029(2) 0.0233(16) 0.0006(15) 0.0032(16) -0.017(3) O10 0.017(2) 0.046(3) 0.0283(17) 0.0058(17) 0.0009(15) 0.002(2) O5 0.022(2) 0.023(2) 0.0294(18) 0.0067(16) 0.0144(16) 0.004(2) O6 0.021(2) 0.015(2) 0.0376(19) -0.0032(15) 0.0122(16) 0.004(2) O9 0.0113(18) 0.026(2) 0.0307(18) 0.0076(16) -0.0001(15) -0.008(2) O7 0.048(3) 0.024(2) 0.0172(16) 0.0026(15) 0.0015(16) -0.022(2) C28 0.017(3) 0.027(3) 0.030(3) -0.011(2) 0.001(2) 0.011(3) C6G 0.035(3) 0.063(5) 0.047(3) -0.004(3) 0.000(3) 0.000(4) C1G 0.022(3) 0.047(4) 0.036(3) -0.012(3) -0.002(2) 0.005(3) C5G 0.037(4) 0.130(8) 0.052(3) -0.003(4) -0.005(3) -0.015(5) C2G 0.020(3) 0.107(7) 0.051(3) 0.002(4) -0.010(3) -0.001(4) C4G 0.035(4) 0.125(7) 0.047(3) -0.008(4) -0.007(3) -0.011(5) C3G 0.030(4) 0.185(10) 0.064(4) 0.020(5) -0.011(3) -0.010(5) 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 94.3(2) . 8_666 O1 Al1 O10 91.42(15) 8_666 8_666 O1 Al1 O10 94.65(15) 8_666 . O1 Al1 O10 94.65(15) . 8_666 O1 Al1 O10 91.41(15) . . O1 Al1 O7 173.01(15) 8_666 6_645 O1 Al1 O7 91.52(14) 8_666 2_645 O1 Al1 O7 173.01(15) . 2_645 O1 Al1 O7 91.52(14) . 6_645 O10 Al1 O10 171.1(3) 8_666 . O10 Al1 O7 84.27(16) 8_666 6_645 O10 Al1 O7 84.27(16) . 2_645 O10 Al1 O7 89.04(17) 8_666 2_645 O10 Al1 O7 89.04(17) . 6_645 O7 Al1 O7 82.9(2) 6_645 2_645 O2 Al2 O3 93.50(15) . . O2 Al2 O8 174.17(15) . 6_645 O2 Al2 O5 92.94(16) . 5_455 O2 Al2 O9 91.33(16) . . O3 Al2 O9 85.66(15) . . O1 Al2 O2 95.46(14) . . O1 Al2 O3 170.98(18) . . O1 Al2 O8 90.14(15) . 6_645 O1 Al2 O5 91.23(15) . 5_455 O1 Al2 O9 95.21(15) . . O8 Al2 O3 80.94(15) 6_645 . O8 Al2 O9 86.52(17) 6_645 . O5 Al2 O3 87.22(16) 5_455 . O5 Al2 O8 88.57(18) 5_455 6_645 O5 Al2 O9 171.90(16) 5_455 . O2 Al3 O2 99.4(2) . 3_665 O2 Al3 O4 169.65(16) . 3_665 O2 Al3 O4 90.82(14) 3_665 3_665 O2 Al3 O4 90.82(14) . . O2 Al3 O4 169.65(16) 3_665 . O2 Al3 O6 93.43(14) . 5_455 O2 Al3 O6 90.02(15) . 6_655 O2 Al3 O6 93.43(14) 3_665 6_655 O2 Al3 O6 90.02(15) 3_665 5_455 O4 Al3 O4 79.1(2) . 3_665 O4 Al3 O6 88.31(17) . 6_655 O4 Al3 O6 87.58(17) . 5_455 O4 Al3 O6 87.58(17) 3_665 6_655 O4 Al3 O6 88.31(17) 3_665 5_455 O6 Al3 O6 174.7(2) 5_455 6_655 Al3 O2 Al2 127.38(17) . . C1 O3 Al2 128.9(3) . . Al2 O1 Al1 129.04(19) . . C1 O4 Al3 137.2(3) . . O3 C1 C2 116.2(5) . . O4 C1 O3 124.3(4) . . O4 C1 C2 118.8(5) . . C25 C26 C21 124.6(5) . . C24 C23 C22 116.8(5) . . O5 C20 C17 119.1(5) . . O6 C20 C17 117.9(5) . . O6 C20 O5 123.0(5) . . C26 C25 C24 118.0(5) . . C21 C22 C23 124.8(6) . . C23 C24 C25 120.8(5) . . C23 C24 C27 119.2(4) . . C25 C24 C27 119.8(5) . . O8 C27 C24 113.9(4) . . O7 C27 C24 119.1(5) . . O7 C27 O8 127.0(5) . . C20 C17 C16 124.8(5) . . C20 C17 C18 123.3(5) . . C18 C17 C16 112.0(6) . . C2 C7 C6 116.9(6) . . C26 C21 C12 120.8(4) . . C22 C21 C26 114.4(5) . . C22 C21 C12 124.4(6) . . C8 C5 C4 117.9(6) . . C6 C5 C8 126.6(6) . . C6 C5 C4 115.2(5) . . C15 C16 C17 125.3(6) . . C5 C8 C9 121.7(5) . . C13 C8 C5 119.6(6) . . C13 C8 C9 118.4(5) . . C7 C2 C1 114.6(5) . . C3 C2 C1 120.4(5) . . C3 C2 C7 125.0(5) . . C19 C18 C17 121.6(5) . . C4 C3 C2 116.8(6) . . C3 C4 C5 122.8(6) . . C19 C14 C10 119.1(6) . . C19 C14 C15 116.0(6) . . C15 C14 C10 124.8(5) . . C5 C6 C7 122.9(6) . . C12 C13 C8 123.0(6) . . C18 C19 C14 122.1(6) . . C11 C10 C14 121.9(5) . . C11 C10 C9 123.4(6) . . C9 C10 C14 114.6(5) . . C16 C15 C14 122.9(6) . . C13 C12 C21 121.5(6) . . C13 C12 C11 118.4(6) . . C11 C12 C21 119.0(5) . . C10 C11 C12 120.4(5) . . C10 C9 C8 115.9(5) . . C27 O8 Al2 134.8(3) . 6_655 C28 O10 Al1 136.5(3) . . C20 O5 Al2 135.9(4) . 5 C20 O6 Al3 134.3(4) . 5 C28 O9 Al2 126.4(3) . . C27 O7 Al1 128.2(4) . 4_564 O10 C28 C1G 113.8(5) . . O9 C28 O10 127.3(5) . . O9 C28 C1G 118.9(5) . . C5G C6G C1G 120.1(6) . . C6G C1G C28 125.4(5) . . C6G C1G C2G 118.7(6) . . C2G C1G C28 115.8(5) . . C6G C5G C4G 122.0(7) . . C3G C2G C1G 122.5(6) . . C5G C4G C4G 123.5(5) . 3_765 C5G C4G C3G 119.2(7) . . C3G C4G C4G 114.8(6) . 3_765 C2G C3G C4G 112.8(7) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Al1 O1 1.834(3) . Al1 O1 1.835(3) 8_666 Al1 O10 1.877(4) . Al1 O10 1.877(4) 8_666 Al1 O7 1.975(4) 2_645 Al1 O7 1.975(4) 6_645 Al2 O2 1.876(3) . Al2 O3 1.924(3) . Al2 O1 1.833(3) . Al2 O8 1.891(4) 6_645 Al2 O5 1.879(4) 5_455 Al2 O9 1.941(4) . Al3 O2 1.816(3) . Al3 O2 1.816(3) 3_665 Al3 O4 1.897(4) . Al3 O4 1.897(4) 3_665 Al3 O6 1.904(4) 6_655 Al3 O6 1.904(4) 5_455 O3 C1 1.333(6) . O4 C1 1.263(7) . C1 C2 1.483(7) . C26 C25 1.347(8) . C26 C21 1.425(8) . C23 C22 1.447(8) . C23 C24 1.355(8) . C20 C17 1.411(8) . C20 O5 1.276(7) . C20 O6 1.253(6) . C25 C24 1.409(7) . C22 C21 1.321(7) . C24 C27 1.484(8) . C27 O8 1.299(6) . C27 O7 1.228(5) . C17 C16 1.476(8) . C17 C18 1.446(8) . C7 C2 1.393(8) . C7 C6 1.421(8) . C21 C12 1.447(8) . C5 C8 1.424(7) . C5 C4 1.510(8) . C5 C6 1.358(9) . C16 C15 1.221(8) . C8 C13 1.404(8) . C8 C9 1.436(8) . C2 C3 1.365(9) . C18 C19 1.334(8) . C3 C4 1.356(7) . C14 C19 1.412(8) . C14 C10 1.495(9) . C14 C15 1.414(9) . C13 C12 1.369(7) . C10 C11 1.370(8) . C10 C9 1.401(7) . C12 C11 1.372(9) . O8 Al2 1.891(4) 6_655 O10 C28 1.271(6) . O5 Al2 1.879(4) 5 O6 Al3 1.904(4) 5 O9 C28 1.251(6) . O7 Al1 1.975(4) 4_564 C28 C1G 1.488(8) . C6G C1G 1.355(8) . C6G C5G 1.333(10) . C1G C2G 1.400(8) . C5G C4G 1.357(9) . C2G C3G 1.384(10) . C4G C4G 1.581(14) 3_765 C4G C3G 1.447(11) . 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 -0.917 -0.395 -0.121 8825.8 9673.1