#------------------------------------------------------------------------------ #$Date: 2026-09-24 07:42:57 +0100 (Thu, 24 Sep 2026) $ #$Revision: 306901 $ #$URL: svn://www.crystallography.net/cod/cif/4/51/95/4519526.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_4519526 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_0.86GPa _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 19.196(3) _cell_length_b 19.196(3) _cell_length_c 36.569(7) _cell_measurement_reflns_used 3798 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 13.02 _cell_measurement_theta_min 2.21 _cell_volume 13475(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 0.930 _diffrn_measured_fraction_theta_max 0.930 _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 0.0826 _diffrn_reflns_av_unetI/netI 0.0942 _diffrn_reflns_Laue_measured_fraction_full 0.930 _diffrn_reflns_Laue_measured_fraction_max 0.930 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 12386 _diffrn_reflns_point_group_measured_fraction_full 0.891 _diffrn_reflns_point_group_measured_fraction_max 0.890 _diffrn_reflns_theta_full 13.027 _diffrn_reflns_theta_max 13.027 _diffrn_reflns_theta_min 0.836 _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 0.2828 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1433 before and 0.0736 after correction. The Ratio of minimum to maximum transmission is 0.3803. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 0.560 _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 0.097 _refine_diff_density_min -0.219 _refine_diff_density_rms 0.019 _refine_ls_abs_structure_details ; Flack x determined using 991 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.50(9) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.897 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 362 _refine_ls_number_reflns 4730 _refine_ls_number_restraints 336 _refine_ls_restrained_S_all 0.883 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0396 _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^)+(0.0260P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0809 _refine_ls_wR_factor_ref 0.0885 _reflns_Friedel_coverage 0.645 _reflns_Friedel_fraction_full 0.835 _reflns_Friedel_fraction_max 0.836 _reflns_number_gt 3219 _reflns_number_total 4730 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file oc7b00169_si_002.cif _cod_data_source_block MOF520_0.86GPa _cod_original_cell_volume 13475(5) _cod_database_code 4519526 _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 0.2828 _exptl_absorpt_special_details ; Data was collected in a Merril Bassett DAC. DAC opening angle of 40 degrees. The pressure of 0.86 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 C13, Al1, O1, O10, Al2, H1, C28, O2, O3, O9, H28, Al3, H2, C1, O4, C2, C7, C3, H7, C6, H3, C4, C5, H6, H4, C8, C9, H13, C12, C10, H9, C21, C11, C14, C26, C22, H11, C19, C15, H26, C25, C23, H22, C18, H19, C16, H15, H25, C24, H23, C17, H18, H16, C27, C20, O8, O7, O5, O6, Al1, O1, Al1, O10, Al2, O1, O1, H1, O10, C28, Al2, O2, Al2, O3, Al2, O9, O9, C28, C28, H28, Al3, O2, O2, H2, O3, C1, Al3, O4, O4, C1, C2, C1, C7, C2, C3, C2, 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 C10, Al1, O1, O10, Al2, H1, C28, O2, O3, O9, H28, Al3, H2, C1, O4, C2, C7, C3, H7, C6, H3, C4, C5, H6, H4, C8, C13, C9, H13, C12, H9, C21, C11, C14, C26, C22, H11, C19, C15, H26, C25, C23, H22, C18, H19, C16, H15, H25, C24, H23, C17, H18, H16, C27, C20, O8, O7, O5, O6, Al1, O1, Al1, O10, Al2, O1, O1, H1, O10, C28, Al2, O2, Al2, O3, Al2, O9, O9, C28, C28, H28, Al3, O2, O2, H2, O3, C1, Al3, O4, O4, C1, C2, C1, C7, C2, C3, C2, 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), C28(H28) ; _shelx_res_file ; p3_25kev_0m.res created by SHELXL-2014/7 TITL P3_25kev_0m in P42212 #94 REM reset to P42212 #94 CELL 0.49594 19.196 19.196 36.569 90 90 90 ZERR 222 0.00271 0.00271 0.00731 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 0.12 0.11 744.346 DISP C 0.009 0.004 30.879 DISP H -0 0 0.639 DISP O 0.025 0.014 100.516 UNIT 224 144 80 16 RIGU C13 Al1 O1 O10 Al2 H1 C28 O2 O3 O9 H28 Al3 H2 C1 O4 C2 C7 C3 H7 C6 H3 = C4 C5 H6 H4 C8 C9 H13 C12 C10 H9 C21 C11 C14 C26 C22 H11 C19 C15 H26 C25 C23 = H22 C18 H19 C16 H15 H25 C24 H23 C17 H18 H16 C27 C20 O8 O7 O5 O6 AL1 O1 AL1 = O10 AL2 O1 O1 H1 O10 C28 AL2 O2 AL2 O3 AL2 O9 O9 C28 C28 H28 AL3 O2 O2 H2 O3 = C1 AL3 O4 O4 C1 C2 C1 C7 C2 C3 C2 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 RIGU C10 Al1 O1 O10 Al2 H1 C28 O2 O3 O9 H28 Al3 H2 C1 O4 C2 C7 C3 H7 C6 H3 = C4 C5 H6 H4 C8 C13 C9 H13 C12 H9 C21 C11 C14 C26 C22 H11 C19 C15 H26 C25 C23 = H22 C18 H19 C16 H15 H25 C24 H23 C17 H18 H16 C27 C20 O8 O7 O5 O6 AL1 O1 AL1 = O10 AL2 O1 O1 H1 O10 C28 AL2 O2 AL2 O3 AL2 O9 O9 C28 C28 H28 AL3 O2 O2 H2 O3 = C1 AL3 O4 O4 C1 C2 C1 C7 C2 C3 C2 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 ABIN ACTA fmap 2 REM REM REM WGHT 0.026000 FVAR 0.11317 AL1 4 0.662996 0.337004 0.500000 10.50000 0.06046 0.06046 = 0.06041 0.00119 0.00119 0.00091 AL2 4 0.617703 0.390452 0.416292 11.00000 0.06737 0.05720 = 0.07811 0.00169 -0.00354 0.00999 AL3 4 0.500000 0.500000 0.382822 10.50000 0.06609 0.05369 = 0.05616 0.00000 0.00000 0.01465 O2 3 0.565625 0.472174 0.417615 11.00000 0.07174 0.06540 = 0.04364 -0.00519 0.00265 0.01380 AFIX 43 H2 2 0.572913 0.501821 0.437361 11.00000 -1.20000 AFIX 0 O3 3 0.642146 0.402755 0.366320 11.00000 0.07286 0.07687 = 0.08135 0.01061 0.02602 0.02031 O1 3 0.600947 0.366763 0.465490 11.00000 0.05538 0.07634 = 0.07551 0.02065 -0.00074 -0.00529 AFIX 43 H1 2 0.554980 0.370743 0.473246 11.00000 -1.20000 AFIX 0 O4 3 0.559259 0.475536 0.343525 11.00000 0.08047 0.06809 = 0.05997 -0.00535 -0.00085 0.01481 C1 1 0.610966 0.438321 0.339333 11.00000 0.08504 0.05955 = 0.06969 0.00586 0.02419 0.01193 C26 1 0.772550 0.628122 0.143471 11.00000 0.18139 0.07606 = 0.07643 0.00971 0.02784 0.01735 AFIX 43 H26 2 0.768829 0.625755 0.168796 11.00000 -1.20000 AFIX 0 C23 1 0.780259 0.636284 0.064447 11.00000 0.15007 0.08911 = 0.07490 0.00200 0.02334 -0.02019 AFIX 43 H23 2 0.775386 0.638912 0.039182 11.00000 -1.20000 AFIX 0 C20 1 0.981856 0.149735 0.112458 11.00000 0.08800 0.06221 = 0.07861 -0.00907 0.02641 -0.00488 C25 1 0.780063 0.694593 0.120697 11.00000 0.21896 0.08987 = 0.06924 0.00361 0.02236 -0.01382 AFIX 43 H25 2 0.777223 0.737000 0.132903 11.00000 -1.20000 AFIX 0 C22 1 0.778377 0.570272 0.083870 11.00000 0.19236 0.08311 = 0.10348 0.00454 0.06394 -0.00227 AFIX 43 H22 2 0.781706 0.528759 0.070876 11.00000 -1.20000 AFIX 0 C24 1 0.789925 0.696120 0.086237 11.00000 0.12598 0.08467 = 0.07801 0.00541 0.01728 -0.01084 C27 1 0.806135 0.761392 0.065585 11.00000 0.10228 0.08071 = 0.07574 0.00961 0.00411 0.00376 C17 1 0.935237 0.211649 0.121196 11.00000 0.09964 0.06650 = 0.09172 -0.01229 0.03207 0.00634 C7 1 0.614095 0.477135 0.273702 11.00000 0.14328 0.16789 = 0.08973 0.05144 0.05275 0.09999 AFIX 43 H7 2 0.571587 0.500015 0.275852 11.00000 -1.20000 AFIX 0 C21 1 0.772274 0.568797 0.118163 11.00000 0.15297 0.07629 = 0.10633 0.00870 0.05934 0.01438 C5 1 0.697533 0.434356 0.230989 11.00000 0.12021 0.07881 = 0.10143 0.02462 0.04182 0.02409 C16 1 0.871495 0.199169 0.138909 11.00000 0.11153 0.07152 = 0.13200 -0.01192 0.05352 0.00159 AFIX 43 H16 2 0.857887 0.154055 0.144819 11.00000 -1.20000 AFIX 0 C8 1 0.734198 0.435581 0.196172 11.00000 0.15193 0.08337 = 0.12169 0.02106 0.05611 0.03837 C2 1 0.647282 0.438137 0.306938 11.00000 0.10866 0.08758 = 0.09616 0.02550 0.03962 0.05438 C18 1 0.953903 0.276222 0.110313 11.00000 0.12204 0.06187 = 0.18965 0.00306 0.07663 0.00501 AFIX 43 H18 2 0.993600 0.284134 0.096338 11.00000 -1.20000 AFIX 0 C3 1 0.701986 0.395406 0.298180 11.00000 0.14153 0.14527 = 0.11588 0.03982 0.06683 0.07508 AFIX 43 H3 2 0.719063 0.365077 0.315870 11.00000 -1.20000 AFIX 0 C4 1 0.732777 0.395783 0.263881 11.00000 0.12737 0.07660 = 0.12131 0.00669 0.04418 0.04016 AFIX 43 H4 2 0.774911 0.372828 0.260362 11.00000 -1.20000 AFIX 0 C14 1 0.848324 0.322930 0.136325 11.00000 0.10870 0.07669 = 0.10152 -0.01214 0.02963 0.00086 C6 1 0.647881 0.476435 0.243107 11.00000 0.14790 0.12523 = 0.10387 0.03508 0.05002 0.07254 AFIX 43 H6 2 0.635174 0.511423 0.226830 11.00000 -1.20000 AFIX 0 C13 1 0.735962 0.495570 0.174239 11.00000 0.18148 0.07895 = 0.11841 0.01947 0.08641 0.04397 AFIX 43 H13 2 0.713668 0.535395 0.182769 11.00000 -1.20000 AFIX 0 C19 1 0.911517 0.328676 0.120917 11.00000 0.11647 0.07910 = 0.10635 0.00024 0.04252 0.00588 AFIX 43 H19 2 0.927934 0.373680 0.117121 11.00000 -1.20000 AFIX 0 C10 1 0.808248 0.381687 0.151161 11.00000 0.10687 0.07818 = 0.11731 0.00183 0.04403 -0.00429 C15 1 0.831079 0.253164 0.147036 11.00000 0.11112 0.07226 = 0.09285 -0.01314 0.04467 0.00049 AFIX 43 H15 2 0.790238 0.245466 0.160106 11.00000 -1.20000 AFIX 0 C12 1 0.767578 0.498679 0.142079 11.00000 0.12765 0.08275 = 0.11495 0.00392 0.05606 0.02064 C11 1 0.804521 0.444556 0.129831 11.00000 0.13252 0.08574 = 0.09996 0.00914 0.06725 0.02243 AFIX 43 H11 2 0.827779 0.447490 0.107575 11.00000 -1.20000 AFIX 0 C9 1 0.772782 0.377781 0.184886 11.00000 0.13545 0.07112 = 0.11714 0.01974 0.07109 0.01645 AFIX 43 H9 2 0.775036 0.337811 0.199209 11.00000 -1.20000 AFIX 0 O8 3 0.827998 0.807472 0.089379 11.00000 0.08776 0.07275 = 0.06385 0.00236 0.01265 -0.01652 O10 3 0.734035 0.399118 0.482072 11.00000 0.06417 0.07361 = 0.09772 -0.00130 0.00095 0.00222 O5 3 1.039016 0.165196 0.098344 11.00000 0.09151 0.04992 = 0.09541 -0.00299 0.02885 -0.00001 O6 3 0.960198 0.089360 0.120083 11.00000 0.07567 0.05893 = 0.07323 -0.01064 0.01788 -0.00007 O9 3 0.699135 0.440685 0.427898 11.00000 0.06734 0.08391 = 0.09783 0.01302 0.00748 -0.00051 O7 3 0.802704 0.765523 0.033972 11.00000 0.08870 0.09340 = 0.07289 0.00772 -0.00468 -0.01232 C28 1 0.738991 0.440910 0.455925 11.00000 0.07919 0.10126 = 0.10134 0.01168 0.00426 -0.00731 AFIX 43 H28 2 0.773988 0.474355 0.456946 11.00000 -1.20000 AFIX 0 HKLF 4 REM P3_25kev_0m in P42212 #94 REM R1 = 0.0396 for 3219 Fo > 4sig(Fo) and 0.0658 for all 4730 data REM 362 parameters refined using 336 restraints END WGHT 0.0267 0.0000 REM Highest difference peak 0.097, deepest hole -0.219, 1-sigma level 0.019 Q1 1 0.6410 0.3565 0.5187 11.00000 0.05 0.10 Q2 1 0.5406 0.3574 0.5009 11.00000 0.05 0.09 Q3 1 0.5399 0.4809 0.3625 11.00000 0.05 0.09 Q4 1 0.6898 0.3231 0.5189 11.00000 0.05 0.09 Q5 1 0.6373 0.3543 0.3947 11.00000 0.05 0.08 Q6 1 0.6084 0.5264 0.2593 11.00000 0.05 0.08 Q7 1 0.8431 0.5578 0.1128 11.00000 0.05 0.08 Q8 1 0.8038 0.1992 0.1724 11.00000 0.05 0.08 Q9 1 0.5000 0.5000 0.4551 10.50000 0.05 0.08 Q10 1 0.5652 0.4492 0.2475 11.00000 0.05 0.08 Q11 1 0.8579 0.6887 0.1116 11.00000 0.05 0.08 Q12 1 0.5000 0.5000 0.4026 10.50000 0.05 0.07 Q13 1 0.7632 0.6524 0.1286 11.00000 0.05 0.07 Q14 1 0.7791 0.5119 0.4549 11.00000 0.05 0.07 Q15 1 0.7210 0.6303 0.0391 11.00000 0.05 0.07 Q16 1 0.6354 0.5058 0.3817 11.00000 0.05 0.07 Q17 1 1.0206 0.1191 0.1590 11.00000 0.05 0.07 Q18 1 0.7360 0.2942 0.3316 11.00000 0.05 0.07 Q19 1 0.6063 0.3945 0.4751 11.00000 0.05 0.07 Q20 1 0.7369 0.7463 0.0446 11.00000 0.05 0.07 ; _shelx_res_checksum 75070 _shelx_hkl_file ; 0 -3 0 0.02 0.08 0 -4 0 53.78 3.48 0 -5 0 -0.01 0.14 -1 -5 0 42.31 2.79 0 -6 0 190.29 12.26 -1 -6 0 21.77 1.49 -2 -6 0 27.41 1.88 0 -7 0 -0.18 0.22 -1 -7 0 69.16 4.52 -2 -7 0 16.33 1.19 0 -8 0 3.43 0.45 -1 -8 0 85.21 5.56 -2 -8 0 97.19 6.35 -3 -8 0 12.13 0.99 -4 8 0 17.60 1.19 0 -9 0 -0.05 0.33 -1 -9 0 20.04 1.62 1 -9 0 26.43 1.62 -2 -9 0 0.59 0.39 -3 -9 0 0.61 0.42 -5 9 0 93.45 6.06 -6 9 0 3.34 0.42 0 -10 0 5.25 0.64 1 -10 0 7.16 0.75 -1 -10 0 8.04 0.78 -2 -10 0 0.05 0.36 -3 -10 0 84.12 5.57 -4 -10 0 -0.02 0.39 -5 10 0 10.35 0.76 -6 10 0 6.19 0.57 -7 10 0 25.86 1.81 0 -11 0 -0.11 0.50 1 -11 0 0.42 0.56 -1 -11 0 1.05 0.48 -2 -11 0 7.05 0.77 -3 -11 0 1.08 0.44 -4 -11 0 28.79 2.11 -6 11 0 23.23 1.60 -7 11 0 26.42 1.83 -8 11 0 17.03 1.28 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232.32 17.23 2 5 -4 148.66 9.59 -5 -2 4 147.50 9.63 5 -2 -4 150.56 9.58 5 2 -4 138.63 9.61 -2 -5 4 141.15 9.60 2 -5 -4 157.79 9.56 -5 2 4 145.13 9.61 5 -3 -4 915.47 60.59 -3 5 4 1000.00 60.61 3 5 -4 908.52 60.60 -5 -3 4 874.16 60.65 -5 3 4 948.89 60.63 -3 -5 4 959.17 60.67 3 -5 -4 987.18 60.56 5 3 -4 949.63 60.66 4 5 -4 85.09 5.92 -5 -4 4 88.24 5.97 5 -4 -4 91.15 5.88 -4 -5 4 94.02 5.98 4 -5 -4 89.00 5.84 5 4 -4 90.47 5.95 -5 4 4 88.90 5.93 -5 -5 4 38.40 2.74 -5 5 4 35.50 2.68 5 5 -4 40.48 2.72 5 -5 -4 40.08 2.61 6 0 -4 3.02 0.52 -6 0 4 4.52 0.63 1 6 -4 15.06 1.15 -6 -1 4 12.65 1.19 6 -1 -4 15.29 1.15 -6 1 4 12.05 1.16 -1 -6 4 16.84 1.29 6 1 -4 12.60 1.17 -1 6 -4 16.38 1.27 -6 -2 4 104.69 6.63 6 -2 -4 109.69 6.58 2 6 -4 101.84 6.54 6 2 -4 115.31 6.64 2 -6 -4 90.98 6.50 -6 2 4 88.08 6.56 -2 -6 4 88.37 6.57 3 6 -4 55.51 3.79 -3 6 4 55.48 3.75 -6 -3 4 53.27 3.85 3 -6 -4 60.10 3.71 6 3 -4 57.34 3.88 -6 3 4 54.76 3.81 -3 -6 4 57.48 3.87 -4 6 4 118.06 7.26 4 6 -4 108.15 7.29 -6 -4 4 110.28 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4.1250 13 8 3 7.0585 -3.9544 13 8 4 -3.2039 -1.4846 13 8 5 -2.0219 -8.4005 13 8 6 1.1549 -0.9041 13 8 7 0.6476 -0.5117 13 8 8 1.1234 0.7195 13 8 9 -2.4207 2.6646 13 8 10 -4.1433 4.7448 13 8 11 -1.5040 -0.0535 13 8 12 -0.2141 5.8105 13 8 13 0.9538 1.6939 13 8 14 -1.5390 4.6557 13 8 15 1.2025 -0.6910 13 8 16 1.2846 3.1968 13 9 0 5.7080 -0.0000 13 9 1 -1.0290 2.9069 13 9 2 3.7099 -1.7877 13 9 3 4.3477 -0.2893 13 9 4 0.4771 -0.2293 13 9 5 -1.1146 1.0172 13 9 6 1.0068 -0.7700 13 9 7 -0.8954 0.8034 13 9 8 -0.0338 -0.0808 13 9 9 1.6880 0.5098 13 9 10 -2.1807 4.4341 13 9 11 -0.9901 -2.0747 13 9 12 0.8928 -0.2863 13 9 13 -0.2002 1.2321 13 9 14 -3.9802 1.8792 13 10 0 5.1985 -0.0000 13 10 1 -2.8325 2.8253 13 10 2 3.5579 -0.4271 13 10 3 3.0746 -1.6501 13 10 4 -1.6959 0.0691 13 10 5 1.0734 -1.5033 13 10 6 3.4501 4.2061 13 10 7 0.3464 1.8543 13 10 8 2.4883 -0.4423 13 10 9 5.2738 -3.9474 13 10 10 -2.0995 3.4562 13 10 11 3.3578 1.5195 13 11 0 -3.6216 0.0000 13 11 1 0.2685 -2.1177 13 11 2 -2.2613 4.0153 13 11 3 -1.9117 -2.9911 13 11 4 -0.5765 -2.6476 13 11 5 -2.9122 1.5766 13 11 6 1.7554 2.1424 13 11 7 0.5272 -2.4931 14 0 0 -5.8987 0.0000 14 0 1 -0.0000 -2.0013 14 0 2 -6.1727 -0.0000 14 0 3 0.0000 3.4423 14 0 4 2.3773 0.0000 14 0 5 -0.0000 -8.6195 14 0 6 -8.0636 -0.0000 14 0 7 0.0000 1.7081 14 0 8 4.4854 -0.0000 14 0 9 -0.0000 -4.1113 14 0 10 1.2188 -0.0000 14 0 11 -0.0000 -7.0716 14 0 12 -4.1136 0.0000 14 0 13 -0.0000 -2.4575 14 0 14 0.0899 -0.0000 14 0 15 0.0000 0.8833 14 0 16 0.1831 0.0000 14 0 17 0.0000 2.4872 14 0 18 2.7430 0.0000 14 0 19 0.0000 1.9059 14 1 0 2.5801 -0.0000 14 1 1 3.3964 0.5162 14 1 2 2.2299 1.6141 14 1 6 -0.0784 -3.7879 14 1 7 1.1472 -3.3613 14 1 8 -2.1373 -1.6948 14 1 9 -7.5617 7.5075 14 1 10 2.1790 -2.5998 14 1 11 -0.3877 2.1965 14 1 12 -3.8882 2.6748 14 1 13 -4.6112 -5.3833 14 1 14 -0.2196 -3.6720 14 1 15 3.6621 -1.5804 14 1 16 -0.9229 5.1767 14 1 17 1.4173 5.8945 14 1 18 1.4184 -2.4876 14 1 19 6.5725 1.7230 14 2 0 1.1172 0.0000 14 2 1 -5.7109 -5.7700 14 2 2 -6.1910 -0.9063 14 2 7 -2.7377 5.5125 14 2 9 0.1772 5.4794 14 2 10 -10.1222 -3.2025 14 2 11 -5.0505 0.8707 14 2 12 5.6278 2.0637 14 2 13 -0.7123 4.2166 14 2 14 1.1403 3.0691 14 2 15 -0.2528 0.3008 14 2 16 -1.3081 3.9985 14 2 17 -2.3298 2.2129 14 2 18 -6.9928 -2.4954 14 2 19 -2.6406 2.4007 14 3 0 0.4843 -0.0000 14 3 1 5.0994 -1.0178 14 3 2 6.2953 -0.4584 14 3 7 -1.9313 -6.3295 14 3 8 3.5548 -0.7817 14 3 9 -1.9328 -4.7093 14 3 10 2.2585 8.3953 14 3 11 -1.0429 -4.1839 14 3 12 0.4159 2.2861 14 3 13 1.4855 4.4582 14 3 14 -1.9971 1.8879 14 3 15 2.5656 -1.8466 14 3 16 2.7871 4.4701 14 3 17 7.1717 1.9142 14 3 18 4.9944 1.4034 14 3 19 4.3779 1.9055 14 4 0 5.9064 -0.0000 14 4 1 7.3285 6.7094 14 4 8 3.9033 -2.2919 14 4 9 0.1688 0.2808 14 4 10 1.1031 -2.1007 14 4 11 -7.6300 1.6517 14 4 12 -1.0118 -2.0295 14 4 13 -3.8365 2.4310 14 4 14 6.2860 -3.3327 14 4 15 0.0522 -0.3097 14 4 16 1.3411 1.7284 14 4 17 1.7006 5.1034 14 4 18 1.2681 0.8622 14 5 0 2.6840 -0.0000 14 5 9 2.8501 2.3472 14 5 10 9.5744 3.2438 14 5 11 7.1214 3.8010 14 5 12 1.7396 -0.1292 14 5 13 4.2139 -3.9994 14 5 14 6.1478 -2.6639 14 5 15 -1.5545 0.5136 14 5 16 3.6679 1.4606 14 5 17 -3.5307 -0.4853 14 6 9 -0.7394 -0.9222 14 6 10 2.4178 -1.1893 14 6 11 2.5810 -1.5687 14 6 12 -4.4707 -1.9516 14 6 13 -0.1836 1.6252 14 6 14 -1.1491 -4.7206 14 6 15 -1.9242 1.0648 14 6 16 2.1791 -1.8460 14 7 10 3.4800 -1.2033 14 7 11 4.2937 -1.5980 14 7 12 -0.3563 0.4043 14 7 13 2.8610 1.8403 14 7 14 1.7227 -2.9757 14 8 0 3.2019 -0.0000 14 8 1 1.5597 -2.2486 14 8 2 1.1356 2.5579 14 8 3 -1.3658 -3.2180 14 8 4 3.0857 3.4106 14 8 5 2.8538 1.1733 14 8 10 -1.6828 -0.2348 14 8 11 0.5579 -1.8968 14 8 12 1.4728 -2.7746 14 9 0 4.1290 -0.0000 14 9 1 4.3831 -0.9189 14 9 2 -1.9284 -3.8959 14 9 3 10.9381 -3.2076 14 9 4 4.2265 0.2838 14 9 5 1.4684 2.4291 14 9 6 -0.8311 -3.6099 14 9 8 -3.5109 1.8866 14 9 9 1.3112 1.0544 14 10 0 -2.2714 0.0000 14 10 1 -0.5142 -1.5694 14 10 2 -1.1958 -3.5510 14 10 3 7.7410 -3.3519 14 10 4 0.2780 -2.8485 14 10 5 2.0563 -1.4016 15 0 1 -2.2564 0.0000 15 0 2 0.0000 5.4702 15 0 3 4.9084 0.0000 15 0 4 0.0000 0.8315 15 0 5 7.9526 0.0000 15 0 6 -0.0000 -3.7263 15 0 7 -1.9778 -0.0000 15 0 8 -0.0000 -2.5018 15 0 9 1.6765 -0.0000 15 0 10 -0.0000 -8.5189 15 0 11 -1.6002 -0.0000 15 0 12 -0.0000 -0.1742 15 0 13 -5.0082 -0.0000 15 0 14 0.0000 5.3917 15 0 15 0.8777 0.0000 15 0 16 0.0000 5.9752 15 1 0 9.3095 -0.0000 15 1 1 -3.7997 -1.3288 15 1 3 -3.4806 3.4825 15 1 7 -9.0120 1.0592 15 1 8 9.0605 -12.3373 15 1 9 -0.4023 -2.6679 15 1 10 -0.1448 4.0316 15 1 11 -1.5190 -3.2137 15 1 12 -2.2881 -1.4003 15 1 13 -6.0400 -3.7485 15 1 14 5.2348 -3.5297 15 1 15 -1.0591 -2.9624 15 1 16 -3.3105 -0.7772 15 2 0 -1.5546 0.0000 15 2 1 5.2059 7.6049 15 2 2 1.6185 -5.3043 15 2 3 -1.0525 -4.9908 15 2 9 0.2463 -10.9129 15 2 10 5.6568 0.2244 15 2 11 2.4503 6.9236 15 2 12 0.7882 1.1988 15 2 13 2.6184 -2.1822 15 2 14 2.7055 0.2416 15 2 15 -2.6233 3.4838 15 2 16 1.4637 -5.2587 15 3 0 5.7191 -0.0000 15 3 1 3.4088 -5.8020 15 3 2 2.6098 -9.0228 15 3 8 2.6089 4.6505 15 3 10 -0.8525 -2.5033 15 3 11 -5.2014 -0.6952 15 3 12 0.5814 6.8941 15 3 13 0.8118 3.9092 15 3 14 0.3601 -1.7135 15 3 15 -2.1747 4.5952 15 4 0 0.6760 -0.0000 15 4 1 -6.7963 -2.2243 15 4 9 4.5204 -0.8718 15 4 10 -0.9669 1.7361 15 4 11 0.1414 -1.7281 15 4 12 2.7234 -0.6120 15 4 13 1.9780 2.8463 15 4 14 0.2278 0.6456 15 4 15 -2.7309 2.0118 15 5 0 5.1985 -0.0000 15 5 1 2.4169 -0.9969 15 5 10 0.3595 -1.2066 15 5 11 1.6105 -0.4810 15 5 12 -1.8755 3.0507 15 5 13 3.8103 -4.5106 15 5 14 -1.8023 -3.3547 15 6 0 -8.1822 0.0000 15 6 11 -0.7511 1.1561 15 6 12 2.8292 1.4966 16 0 0 -11.6434 0.0000 16 0 1 0.0000 0.8212 16 0 2 -2.8415 0.0000 16 0 3 0.0000 1.5557 16 0 4 -2.7344 0.0000 16 0 5 -0.0000 -2.1045 16 0 6 2.1292 0.0000 16 0 7 -0.0000 -3.2777 16 0 8 -1.9454 0.0000 16 0 9 0.0000 3.4806 16 0 10 -2.1294 0.0000 16 0 11 -0.0000 -4.7956 16 0 12 -0.0704 0.0000 16 0 13 -0.0000 -3.3571 16 1 0 10.2759 -0.0000 16 1 1 -1.0193 3.8949 16 1 4 -1.3373 1.7354 16 1 5 -2.5431 -0.2673 16 1 8 4.9844 5.1240 16 1 9 -1.6364 -2.2684 16 1 10 0.4016 2.2032 16 1 11 2.4303 -2.4907 16 1 12 0.3740 3.6894 16 1 13 0.9040 -3.8318 16 2 0 -6.9479 0.0000 16 2 1 6.9208 8.2440 16 2 2 -3.6220 -5.3222 16 2 3 3.7705 4.3641 16 2 4 -9.2632 -9.6370 16 2 8 -3.0634 2.9475 16 2 9 -10.4035 2.0965 16 2 10 -2.0323 -6.4388 16 2 11 -3.7911 -1.9523 16 2 12 1.5720 -5.5606 16 3 0 3.8693 -0.0000 16 3 1 -0.7267 -2.7335 16 3 2 -3.5113 6.3566 16 3 3 -6.0930 0.1060 16 3 9 -0.8620 1.0971 16 3 10 -4.2294 3.4704 16 3 11 -1.7568 -0.5376 16 4 0 5.3473 -0.0000 16 4 1 -0.0204 2.5677 16 4 2 -1.3581 -2.4147 16 4 10 4.2421 2.4681 16 5 0 -4.2986 0.0000 16 5 1 -7.1162 0.9737 16 6 0 -4.4985 0.0000 17 0 1 1.8064 0.0000 17 0 2 -0.0000 -5.0538 17 0 3 4.7510 -0.0000 17 0 4 0.0000 1.3520 17 0 5 2.2632 0.0000 17 0 6 -0.0000 -8.1761 17 1 0 -2.9968 0.0000 17 1 1 -3.5892 -2.8479 17 1 2 3.9092 -0.5117 17 1 3 2.4223 0.2291 17 1 4 -3.2587 -2.9901 17 1 5 2.4256 6.0123 17 2 0 -1.0609 0.0000 17 2 1 -0.9122 0.9303 17 2 2 -2.1614 -0.8319 17 2 3 0.8836 -2.5659 17 2 5 4.2167 4.2154 17 3 0 -0.0203 0.0000 17 3 1 2.5257 -3.6113 17 3 2 0.2851 4.6257 17 3 3 3.7460 2.6287 17 3 4 5.2492 1.6165 0 0 0 0.0 0.0 ; _shelx_fab_checksum 13769 _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 0.66300(8) 0.33700(8) 0.5000 0.0604(7) Uani 1 2 d S TU P . . Al2 Al 0.61770(9) 0.39045(8) 0.41629(5) 0.0676(6) Uani 1 1 d . U . . . Al3 Al 0.5000 0.5000 0.38282(7) 0.0586(7) Uani 1 2 d S TU P . . O2 O 0.56562(15) 0.47217(15) 0.41761(10) 0.0603(11) Uani 1 1 d . U . . . H2 H 0.5729 0.5018 0.4374 0.072 Uiso 1 1 calc R U . . . O3 O 0.64215(18) 0.40276(19) 0.36632(12) 0.0770(13) Uani 1 1 d . U . . . O1 O 0.60095(16) 0.36676(16) 0.46549(10) 0.0691(12) Uani 1 1 d . U . . . H1 H 0.5550 0.3707 0.4732 0.083 Uiso 1 1 calc R U . . . O4 O 0.5593(2) 0.47554(18) 0.34352(10) 0.0695(13) Uani 1 1 d . U . . . C1 C 0.6110(4) 0.4383(3) 0.3393(2) 0.0714(19) Uani 1 1 d . U . . . C26 C 0.7726(3) 0.6281(4) 0.1435(2) 0.111(3) Uani 1 1 d . U . . . H26 H 0.7688 0.6258 0.1688 0.134 Uiso 1 1 calc R U . . . C23 C 0.7803(3) 0.6363(4) 0.0644(2) 0.105(2) Uani 1 1 d . U . . . H23 H 0.7754 0.6389 0.0392 0.126 Uiso 1 1 calc R U . . . C20 C 0.9819(4) 0.1497(3) 0.11246(18) 0.076(2) Uani 1 1 d . U . . . C25 C 0.7801(4) 0.6946(4) 0.1207(2) 0.126(3) Uani 1 1 d . U . . . H25 H 0.7772 0.7370 0.1329 0.151 Uiso 1 1 calc R U . . . C22 C 0.7784(4) 0.5703(4) 0.0839(3) 0.126(3) Uani 1 1 d . U . . . H22 H 0.7817 0.5288 0.0709 0.152 Uiso 1 1 calc R U . . . C24 C 0.7899(4) 0.6961(4) 0.0862(3) 0.096(2) Uani 1 1 d . U . . . C27 C 0.8061(4) 0.7614(4) 0.0656(3) 0.086(3) Uani 1 1 d . U . . . C17 C 0.9352(3) 0.2116(3) 0.12120(18) 0.086(2) Uani 1 1 d . U . . . C7 C 0.6141(4) 0.4771(4) 0.2737(2) 0.134(3) Uani 1 1 d . U . . . H7 H 0.5716 0.5000 0.2759 0.160 Uiso 1 1 calc R U . . . C21 C 0.7723(4) 0.5688(4) 0.1182(3) 0.112(3) Uani 1 1 d . U . . . C5 C 0.6975(4) 0.4344(3) 0.2310(2) 0.100(2) Uani 1 1 d . U . . . C16 C 0.8715(4) 0.1992(3) 0.13891(19) 0.105(3) Uani 1 1 d . U . . . H16 H 0.8579 0.1541 0.1448 0.126 Uiso 1 1 calc R U . . . C8 C 0.7342(4) 0.4356(4) 0.1962(2) 0.119(3) Uani 1 1 d . U . . . C2 C 0.6473(4) 0.4381(3) 0.3069(2) 0.097(2) Uani 1 1 d . U . . . C18 C 0.9539(3) 0.2762(3) 0.1103(2) 0.125(3) Uani 1 1 d . U . . . H18 H 0.9936 0.2841 0.0963 0.149 Uiso 1 1 calc R U . . . C3 C 0.7020(4) 0.3954(4) 0.2982(2) 0.134(3) Uani 1 1 d . U . . . H3 H 0.7191 0.3651 0.3159 0.161 Uiso 1 1 calc R U . . . C4 C 0.7328(4) 0.3958(3) 0.2639(2) 0.108(2) Uani 1 1 d . U . . . H4 H 0.7749 0.3728 0.2604 0.130 Uiso 1 1 calc R U . . . C14 C 0.8483(4) 0.3229(4) 0.13633(19) 0.096(2) Uani 1 1 d . U . . . C6 C 0.6479(4) 0.4764(4) 0.2431(2) 0.126(3) Uani 1 1 d . U . . . H6 H 0.6352 0.5114 0.2268 0.151 Uiso 1 1 calc R U . . . C13 C 0.7360(4) 0.4956(4) 0.1742(2) 0.126(3) Uani 1 1 d . U . . . H13 H 0.7137 0.5354 0.1828 0.152 Uiso 1 1 calc R U . . . C19 C 0.9115(4) 0.3287(3) 0.12092(19) 0.101(2) Uani 1 1 d . U . . . H19 H 0.9279 0.3737 0.1171 0.121 Uiso 1 1 calc R U . . . C10 C 0.8082(3) 0.3817(4) 0.1512(2) 0.101(2) Uani 1 1 d . U . . . C15 C 0.8311(3) 0.2532(3) 0.14704(17) 0.092(2) Uani 1 1 d . U . . . H15 H 0.7902 0.2455 0.1601 0.110 Uiso 1 1 calc R U . . . C12 C 0.7676(4) 0.4987(4) 0.1421(2) 0.108(3) Uani 1 1 d . U . . . C11 C 0.8045(3) 0.4446(4) 0.12983(19) 0.106(3) Uani 1 1 d . U . . . H11 H 0.8278 0.4475 0.1076 0.127 Uiso 1 1 calc R U . . . C9 C 0.7728(3) 0.3778(3) 0.1849(2) 0.108(3) Uani 1 1 d . U . . . H9 H 0.7750 0.3378 0.1992 0.129 Uiso 1 1 calc R U . . . O8 O 0.82800(18) 0.80747(19) 0.08938(11) 0.0748(13) Uani 1 1 d . U . . . O10 O 0.73403(18) 0.3991(2) 0.48207(13) 0.0785(14) Uani 1 1 d . U . . . O5 O 1.0390(2) 0.16520(17) 0.09834(11) 0.0789(14) Uani 1 1 d . U . . . O6 O 0.96020(17) 0.08936(19) 0.12008(11) 0.0693(12) Uani 1 1 d . U . . . O9 O 0.6991(2) 0.4407(2) 0.42790(14) 0.0830(14) Uani 1 1 d . U . . . O7 O 0.8027(2) 0.7655(2) 0.03397(14) 0.0850(16) Uani 1 1 d . U . . . C28 C 0.7390(4) 0.4409(4) 0.4559(2) 0.094(3) Uani 1 1 d . U . . . H28 H 0.7740 0.4744 0.4569 0.113 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 0.0605(10) 0.0605(10) 0.060(2) 0.0012(11) 0.0012(11) 0.0009(12) Al2 0.0674(13) 0.0572(12) 0.0781(18) 0.0017(11) -0.0035(11) 0.0100(10) Al3 0.0661(17) 0.0537(16) 0.056(2) 0.000 0.000 0.0146(12) O2 0.072(2) 0.065(2) 0.044(3) -0.0052(17) 0.0026(19) 0.0138(19) O3 0.073(3) 0.077(3) 0.081(4) 0.011(2) 0.026(2) 0.020(2) O1 0.055(2) 0.076(3) 0.076(4) 0.021(2) -0.001(2) -0.0053(19) O4 0.080(3) 0.068(3) 0.060(4) -0.005(2) -0.001(2) 0.015(2) C1 0.085(5) 0.060(4) 0.070(6) 0.006(4) 0.024(4) 0.012(4) C26 0.181(7) 0.076(5) 0.076(7) 0.010(4) 0.028(5) 0.017(5) C23 0.150(7) 0.089(5) 0.075(7) 0.002(4) 0.023(4) -0.020(4) C20 0.088(5) 0.062(4) 0.079(6) -0.009(4) 0.026(4) -0.005(4) C25 0.219(8) 0.090(5) 0.069(7) 0.004(5) 0.022(6) -0.014(5) C22 0.192(8) 0.083(5) 0.103(8) 0.005(5) 0.064(6) -0.002(5) C24 0.126(6) 0.085(5) 0.078(7) 0.005(5) 0.017(5) -0.011(4) C27 0.102(5) 0.081(5) 0.076(7) 0.010(5) 0.004(5) 0.004(4) C17 0.100(5) 0.066(4) 0.092(7) -0.012(4) 0.032(4) 0.006(4) C7 0.143(7) 0.168(7) 0.090(7) 0.051(5) 0.053(5) 0.100(6) C21 0.153(6) 0.076(5) 0.106(7) 0.009(5) 0.059(6) 0.014(4) C5 0.120(6) 0.079(5) 0.101(7) 0.025(4) 0.042(5) 0.024(4) C16 0.112(5) 0.072(5) 0.132(8) -0.012(4) 0.054(5) 0.002(4) C8 0.152(7) 0.083(5) 0.122(7) 0.021(5) 0.056(5) 0.038(5) C2 0.109(5) 0.088(5) 0.096(6) 0.026(4) 0.040(4) 0.054(4) C18 0.122(6) 0.062(4) 0.190(9) 0.003(5) 0.077(5) 0.005(4) C3 0.142(6) 0.145(7) 0.116(8) 0.040(5) 0.067(5) 0.075(6) C4 0.127(6) 0.077(5) 0.121(7) 0.007(5) 0.044(5) 0.040(4) C14 0.109(5) 0.077(5) 0.102(7) -0.012(4) 0.030(4) 0.001(4) C6 0.148(7) 0.125(6) 0.104(8) 0.035(5) 0.050(5) 0.073(5) C13 0.181(8) 0.079(5) 0.118(7) 0.019(5) 0.086(6) 0.044(5) C19 0.116(6) 0.079(5) 0.106(7) 0.000(4) 0.043(5) 0.006(4) C10 0.107(5) 0.078(5) 0.117(7) 0.002(4) 0.044(4) -0.004(4) C15 0.111(5) 0.072(5) 0.093(7) -0.013(4) 0.045(4) 0.000(4) C12 0.128(6) 0.083(5) 0.115(7) 0.004(5) 0.056(5) 0.021(4) C11 0.133(6) 0.086(5) 0.100(7) 0.009(4) 0.067(5) 0.022(4) C9 0.135(6) 0.071(5) 0.117(7) 0.020(4) 0.071(5) 0.016(4) O8 0.088(3) 0.073(3) 0.064(4) 0.002(2) 0.013(2) -0.017(2) O10 0.064(3) 0.074(3) 0.098(5) -0.001(2) 0.001(2) 0.002(2) O5 0.092(3) 0.050(3) 0.095(4) -0.003(2) 0.029(3) 0.000(2) O6 0.076(3) 0.059(3) 0.073(4) -0.011(2) 0.018(2) 0.000(2) O9 0.067(3) 0.084(3) 0.098(5) 0.013(3) 0.007(2) -0.001(2) O7 0.089(3) 0.093(3) 0.073(4) 0.008(3) -0.005(3) -0.012(2) C28 0.079(5) 0.101(6) 0.101(7) 0.012(5) 0.004(4) -0.007(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0090 0.0040 '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 0.0250 0.0140 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.1200 0.1100 '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 94.0(2) 8_666 . O1 Al1 O10 93.03(16) . 8_666 O1 Al1 O10 91.88(16) . . O1 Al1 O10 91.89(16) 8_666 8_666 O1 Al1 O10 93.03(16) 8_666 . O1 Al1 O7 175.5(2) 8_666 6_645 O1 Al1 O7 90.01(17) 8_666 2_645 O1 Al1 O7 90.01(17) . 6_645 O1 Al1 O7 175.5(2) . 2_645 O10 Al1 O10 172.8(2) 8_666 . O10 Al1 O7 85.88(18) . 2_645 O10 Al1 O7 88.85(18) . 6_645 O10 Al1 O7 85.88(18) 8_666 6_645 O10 Al1 O7 88.85(18) 8_666 2_645 O7 Al1 O7 86.1(3) 6_645 2_645 O2 Al2 O3 93.03(16) . . O2 Al2 O1 94.99(16) . . O2 Al2 O8 175.2(2) . 6_645 O2 Al2 O5 93.06(16) . 5_455 O2 Al2 O9 90.48(16) . . O3 Al2 O8 82.24(18) . 6_645 O3 Al2 O5 89.73(18) . 5_455 O1 Al2 O3 171.98(16) . . O1 Al2 O8 89.74(17) . 6_645 O1 Al2 O5 89.87(17) . 5_455 O1 Al2 O9 92.87(19) . . O8 Al2 O5 86.30(17) 6_645 5_455 O9 Al2 O3 87.0(2) . . O9 Al2 O8 89.92(17) . 6_645 O9 Al2 O5 175.3(2) . 5_455 O2 Al3 O2 94.2(2) 3_665 . O2 Al3 O4 173.48(19) . 3_665 O2 Al3 O4 92.34(15) . . O2 Al3 O4 173.48(19) 3_665 . O2 Al3 O4 92.34(15) 3_665 3_665 O2 Al3 O6 92.96(15) 3_665 6_655 O2 Al3 O6 91.45(15) 3_665 5_455 O2 Al3 O6 92.96(15) . 5_455 O2 Al3 O6 91.45(15) . 6_655 O4 Al3 O4 81.1(3) . 3_665 O6 Al3 O4 88.57(16) 6_655 3_665 O6 Al3 O4 86.52(16) 6_655 . O6 Al3 O4 86.52(16) 5_455 3_665 O6 Al3 O4 88.57(16) 5_455 . O6 Al3 O6 173.5(3) 5_455 6_655 Al2 O2 Al3 125.8(2) . . C1 O3 Al2 131.3(4) . . Al1 O1 Al2 128.61(18) . . C1 O4 Al3 136.3(4) . . O3 C1 C2 114.0(7) . . O4 C1 O3 124.3(7) . . O4 C1 C2 121.1(7) . . C21 C26 C25 107.7(7) . . C24 C23 C22 115.9(8) . . O5 C20 C17 114.7(6) . . O5 C20 O6 126.8(6) . . O6 C20 C17 118.5(6) . . C24 C25 C26 124.8(8) . . C21 C22 C23 120.6(8) . . C23 C24 C27 115.1(8) . . C25 C24 C23 121.4(8) . . C25 C24 C27 123.3(9) . . O8 C27 C24 107.3(8) . . O7 C27 C24 123.3(9) . . O7 C27 O8 129.3(9) . . C16 C17 C20 118.4(6) . . C18 C17 C20 119.9(7) . . C18 C17 C16 121.6(6) . . C6 C7 C2 117.6(7) . . C26 C21 C12 107.9(8) . . C22 C21 C26 127.6(8) . . C22 C21 C12 124.4(8) . . C8 C5 C4 118.1(7) . . C6 C5 C8 129.1(8) . . C6 C5 C4 110.0(7) . . C15 C16 C17 118.6(6) . . C13 C8 C5 121.7(7) . . C9 C8 C5 120.2(7) . . C9 C8 C13 118.0(7) . . C1 C2 C7 117.5(7) . . C3 C2 C1 126.3(7) . . C3 C2 C7 114.7(7) . . C17 C18 C19 116.1(6) . . C2 C3 C4 122.3(8) . . C3 C4 C5 120.9(7) . . C19 C14 C10 124.4(7) . . C19 C14 C15 113.6(6) . . C15 C14 C10 119.7(7) . . C7 C6 C5 131.0(8) . . C12 C13 C8 123.7(7) . . C14 C19 C18 127.1(7) . . C11 C10 C14 118.0(7) . . C9 C10 C14 122.3(7) . . C9 C10 C11 119.6(6) . . C16 C15 C14 122.2(6) . . C13 C12 C21 123.1(7) . . C13 C12 C11 120.4(7) . . C11 C12 C21 116.1(7) . . C12 C11 C10 119.8(7) . . C8 C9 C10 118.2(7) . . C27 O8 Al2 131.6(5) . 6_655 C28 O10 Al1 135.3(5) . . C20 O5 Al2 132.3(4) . 5 C20 O6 Al3 133.7(4) . 5 C28 O9 Al2 132.7(5) . . C27 O7 Al1 131.2(6) . 4_564 O10 C28 O9 124.4(8) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Al1 O1 1.827(4) 8_666 Al1 O1 1.827(4) . Al1 O10 1.926(4) . Al1 O10 1.926(4) 8_666 Al1 O7 1.965(5) 6_645 Al1 O7 1.965(5) 2_645 Al2 O2 1.861(3) . Al2 O3 1.901(5) . Al2 O1 1.883(4) . Al2 O8 1.915(4) 6_645 Al2 O5 1.926(4) 5_455 Al2 O9 1.885(4) . Al3 O2 1.868(4) 3_665 Al3 O2 1.868(4) . Al3 O4 1.892(4) 3_665 Al3 O4 1.892(4) . Al3 O6 1.881(3) 6_655 Al3 O6 1.881(3) 5_455 O3 C1 1.341(7) . O4 C1 1.232(7) . C1 C2 1.375(8) . C26 C25 1.531(9) . C26 C21 1.467(9) . C23 C22 1.453(8) . C23 C24 1.410(9) . C20 C17 1.522(8) . C20 O5 1.248(6) . C20 O6 1.262(6) . C25 C24 1.275(8) . C22 C21 1.260(9) . C24 C27 1.496(10) . C27 O8 1.310(8) . C27 O7 1.161(8) . C17 C16 1.405(7) . C17 C18 1.350(7) . C7 C2 1.563(9) . C7 C6 1.293(8) . C21 C12 1.608(9) . C5 C8 1.455(9) . C5 C4 1.566(9) . C5 C6 1.326(8) . C16 C15 1.328(7) . C8 C13 1.404(8) . C8 C9 1.396(8) . C2 C3 1.370(8) . C18 C19 1.351(7) . C3 C4 1.387(8) . C14 C19 1.342(7) . C14 C10 1.469(8) . C14 C15 1.434(8) . C13 C12 1.325(8) . C10 C11 1.439(8) . C10 C9 1.411(8) . C12 C11 1.335(7) . O8 Al2 1.915(4) 6_655 O10 C28 1.252(7) . O5 Al2 1.926(4) 5 O6 Al3 1.881(3) 5 O9 C28 1.279(8) . O7 Al1 1.965(5) 4_564 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 -0.259 -0.456 -0.833 9629.5 10558.6