#------------------------------------------------------------------------------ #$Date: 2026-09-24 07:42:57 +0100 (Thu, 24 Sep 2026) $ #$Revision: 306901 $ #$URL: svn://www.crystallography.net/cod/cif/4/51/95/4519527.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_4519527 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_1.47 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 19.182(3) _cell_length_b 19.182(3) _cell_length_c 36.534(7) _cell_measurement_reflns_used 4625 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 11.91 _cell_measurement_theta_min 2.21 _cell_volume 13443(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 0.332 _diffrn_measured_fraction_theta_max 0.945 _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 0.0491 _diffrn_reflns_av_unetI/netI 0.0568 _diffrn_reflns_Laue_measured_fraction_full 0.332 _diffrn_reflns_Laue_measured_fraction_max 0.945 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 9518 _diffrn_reflns_point_group_measured_fraction_full 0.316 _diffrn_reflns_point_group_measured_fraction_max 0.944 _diffrn_reflns_theta_full 17.311 _diffrn_reflns_theta_max 11.925 _diffrn_reflns_theta_min 0.837 _diffrn_source ; Advanced Light Source, station 12.2.2 ; _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.029 _exptl_absorpt_correction_T_max 0.7436 _exptl_absorpt_correction_T_min 0.6380 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1253 before and 0.0622 after correction. The Ratio of minimum to maximum transmission is 0.8580. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 0.562 _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 0.115 _refine_diff_density_min -0.185 _refine_diff_density_rms 0.023 _refine_ls_abs_structure_details ; Flack x determined using 1289 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.1(3) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 362 _refine_ls_number_reflns 3850 _refine_ls_number_restraints 336 _refine_ls_restrained_S_all 1.062 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0361 _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^)+(0.0630P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1009 _refine_ls_wR_factor_ref 0.1045 _reflns_Friedel_coverage 0.695 _reflns_Friedel_fraction_full 0.297 _reflns_Friedel_fraction_max 0.942 _reflns_number_gt 3381 _reflns_number_total 3850 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file oc7b00169_si_002.cif _cod_data_source_block MOF520_1.47GPa _cod_original_cell_volume 13443(5) _cod_database_code 4519527 _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 0.7436 _shelx_estimated_absorpt_t_min 0.6380 _exptl_absorpt_special_details ; Data was collected in a Merril Bassett DAC. DAC opening angle of 40 degrees. The pressure of 1.47 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 C5, Al1, O1, O10, Al2, C28, O2, O3, O9, H28, Al3, C1, O4, C2, C7, C3, H7, C6, H3, C4, H6, H4, C8, C13, 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, O10, C28, Al2, O2, Al2, O3, Al2, O9, O9, C28, C28, H28, Al3, O2, O3, C1, Al3, O4, O4, C1, C2, C1, C7, C2, C2, C3, C7, H7, C7, C6, C3, H3, C4, C3, C6, H6, C5, C6, C5, C4, C4, H4, C5, C8, C8, C13, C9, C8, C13, H13, C13, C12, C9, C10, C9, H9, C21, C12, C11, C12, 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), C6(H6), C13(H13), C19(H19), C15(H15), C9(H9), C28(H28), C3(H3), C4(H4), C11(H11) ; _shelx_res_file ; TITL P4_25kev_0m in P42212 #94 REM reset to P42212 #94 CELL 0.49594 19.182 19.182 36.534 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 0.031 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 RIGU C5 Al1 O1 O10 Al2 C28 O2 O3 O9 H28 Al3 C1 O4 C2 C7 C3 H7 C6 H3 C4 H6 H4 = C8 C13 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 O10 C28 AL2 O2 AL2 O3 AL2 O9 O9 C28 C28 H28 AL3 O2 O3 C1 AL3 O4 O4 C1 C2 = C1 C7 C2 C2 C3 C7 H7 C7 C6 C3 H3 C4 C3 C6 H6 C5 C6 C5 C4 C4 H4 C5 C8 C8 C13 = C9 C8 C13 H13 C13 C12 C9 C10 C9 H9 C21 C12 C11 C12 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. 14 PLAN 20 TEMP 23 BOND ABIN ACTA fmap 2 REM REM REM WGHT 0.063000 FVAR 0.11387 AL1 4 0.663494 0.336506 0.500000 10.50000 0.05187 0.05187 = 0.04832 -0.00215 -0.00215 0.00723 AL2 4 0.616702 0.389572 0.416255 11.00000 0.06557 0.04549 = 0.04971 -0.00538 -0.00607 0.01741 AL3 4 0.500000 0.500000 0.383338 10.50000 0.06258 0.04972 = 0.04243 0.00000 0.00000 0.01204 O2 3 0.564946 0.470615 0.418441 11.00000 0.04811 0.05900 = 0.04750 -0.00529 -0.00161 0.00689 AFIX 43 H2 2 0.571662 0.499283 0.438664 11.00000 -1.20000 AFIX 0 O3 3 0.639516 0.401049 0.365653 11.00000 0.07891 0.05648 = 0.05065 0.00043 0.01929 0.01978 O1 3 0.600654 0.366676 0.466456 11.00000 0.05102 0.06601 = 0.04939 0.01667 -0.00530 0.01757 AFIX 43 H1 2 0.555047 0.371604 0.474696 11.00000 -1.20000 AFIX 0 O4 3 0.559020 0.473333 0.344410 11.00000 0.08321 0.05802 = 0.04112 -0.00114 0.00634 0.01885 C1 1 0.611701 0.435383 0.340172 11.00000 0.08142 0.04431 = 0.03916 -0.00142 0.01865 0.02016 C26 1 0.768878 0.631226 0.139997 11.00000 0.15553 0.07262 = 0.04443 0.02273 0.03068 -0.00055 AFIX 43 H26 2 0.764251 0.628952 0.165308 11.00000 -1.20000 AFIX 0 C23 1 0.779254 0.629961 0.067722 11.00000 0.12437 0.09110 = 0.06726 0.00096 0.01685 -0.03139 AFIX 43 H23 2 0.779037 0.630464 0.042268 11.00000 -1.20000 AFIX 0 C20 1 0.975513 0.150520 0.111251 11.00000 0.08430 0.04384 = 0.05330 -0.00058 0.02814 0.01662 C25 1 0.779763 0.692356 0.125204 11.00000 0.15798 0.07204 = 0.04574 0.01890 0.00388 -0.02259 AFIX 43 H25 2 0.782297 0.733087 0.138948 11.00000 -1.20000 AFIX 0 C22 1 0.771240 0.567587 0.085026 11.00000 0.13991 0.06781 = 0.05502 0.01551 0.05729 -0.01944 AFIX 43 H22 2 0.771742 0.526789 0.071275 11.00000 -1.20000 AFIX 0 C24 1 0.787583 0.691739 0.085693 11.00000 0.10306 0.07194 = 0.05694 0.02111 0.02400 -0.02647 C27 1 0.803934 0.756993 0.062676 11.00000 0.07504 0.05213 = 0.04525 0.00710 -0.00806 -0.01275 C17 1 0.932951 0.208441 0.120168 11.00000 0.09495 0.05183 = 0.05193 -0.00895 0.03245 0.02220 C7 1 0.611994 0.475224 0.275759 11.00000 0.13411 0.11897 = 0.07589 0.04796 0.03173 0.07146 AFIX 43 H7 2 0.570614 0.499899 0.278606 11.00000 -1.20000 AFIX 0 C21 1 0.763323 0.563832 0.118507 11.00000 0.07302 0.04946 = 0.06241 0.01060 0.04882 -0.00029 C16 1 0.869294 0.196578 0.138709 11.00000 0.10855 0.03940 = 0.12082 -0.01812 0.06615 0.00495 AFIX 43 H16 2 0.854110 0.152020 0.144801 11.00000 -1.20000 AFIX 0 C2 1 0.643854 0.435294 0.306855 11.00000 0.08656 0.05445 = 0.06332 0.00808 0.02762 0.03874 C18 1 0.957838 0.276242 0.108485 11.00000 0.12709 0.04595 = 0.14706 0.00780 0.04051 0.01216 AFIX 43 H18 2 0.999646 0.283949 0.096248 11.00000 -1.20000 AFIX 0 C14 1 0.842896 0.321519 0.138329 11.00000 0.08720 0.05885 = 0.06370 -0.00641 0.00921 -0.00116 C6 1 0.645363 0.473734 0.244187 11.00000 0.15469 0.10241 = 0.06880 0.04986 0.03329 0.09313 AFIX 43 H6 2 0.628504 0.506277 0.227523 11.00000 -1.20000 AFIX 0 C13 1 0.730345 0.493367 0.174115 11.00000 0.15705 0.04220 = 0.10893 0.01028 0.07015 0.01636 AFIX 43 H13 2 0.707631 0.533209 0.182370 11.00000 -1.20000 AFIX 0 C19 1 0.906775 0.332486 0.118863 11.00000 0.10758 0.07696 = 0.07824 -0.00736 0.01500 -0.00100 AFIX 43 H19 2 0.917571 0.377960 0.112096 11.00000 -1.20000 AFIX 0 C10 1 0.803054 0.381566 0.148207 11.00000 0.10728 0.06671 = 0.08927 0.00011 0.03574 0.00700 C15 1 0.832128 0.254028 0.146959 11.00000 0.10800 0.05458 = 0.07914 -0.01112 0.04323 0.00608 AFIX 43 H15 2 0.792445 0.245783 0.160929 11.00000 -1.20000 AFIX 0 C12 1 0.762728 0.494951 0.136984 11.00000 0.09796 0.05959 = 0.10709 0.00602 0.03847 0.00630 C9 1 0.768147 0.378624 0.182627 11.00000 0.12271 0.04357 = 0.10338 0.01966 0.04473 0.01498 AFIX 43 H9 2 0.769058 0.337595 0.196181 11.00000 -1.20000 AFIX 0 O8 3 0.827009 0.803736 0.088348 11.00000 0.07149 0.07045 = 0.06412 0.02617 0.01295 -0.01740 O10 3 0.733168 0.398954 0.481881 11.00000 0.04823 0.06156 = 0.07765 -0.02050 0.00018 0.00226 O5 3 1.037929 0.166501 0.097995 11.00000 0.08508 0.04225 = 0.04590 -0.01497 0.02316 0.00980 O6 3 0.957400 0.089434 0.119882 11.00000 0.07317 0.04568 = 0.04730 -0.00227 0.01801 0.00966 O7 3 0.801348 0.764550 0.032263 11.00000 0.10289 0.06958 = 0.04790 0.02507 -0.01261 -0.01351 O9 3 0.697090 0.439838 0.426543 11.00000 0.06038 0.07383 = 0.08187 0.00017 0.01199 -0.00968 C28 1 0.739546 0.445434 0.453097 11.00000 0.06950 0.09704 = 0.07218 -0.00016 0.01015 -0.00546 AFIX 43 H28 2 0.773839 0.479706 0.453182 11.00000 -1.20000 AFIX 0 C5 1 0.698712 0.435335 0.230663 11.00000 0.10253 0.07089 = 0.08965 0.02797 0.02538 0.03423 C8 1 0.732247 0.437232 0.196358 11.00000 0.13071 0.04094 = 0.11137 0.00973 0.04901 0.03442 C3 1 0.700048 0.396471 0.297560 11.00000 0.13525 0.10962 = 0.08727 0.03744 0.04527 0.07674 AFIX 43 H3 2 0.719231 0.368136 0.315594 11.00000 -1.20000 AFIX 0 C4 1 0.731460 0.395468 0.263256 11.00000 0.10180 0.11395 = 0.08564 0.01581 0.03330 0.05617 AFIX 43 H4 2 0.772567 0.370591 0.259857 11.00000 -1.20000 AFIX 0 C11 1 0.798698 0.441473 0.126318 11.00000 0.10345 0.04482 = 0.09422 0.01483 0.06057 0.03542 AFIX 43 H11 2 0.821819 0.442840 0.103955 11.00000 -1.20000 AFIX 0 HKLF 4 REM P4_25kev_0m in P42212 #94 REM R1 = 0.0361 for 3381 Fo > 4sig(Fo) and 0.0422 for all 3850 data REM 362 parameters refined using 336 restraints END WGHT 0.0628 0.0000 REM Highest difference peak 0.115, deepest hole -0.185, 1-sigma level 0.023 Q1 1 0.7810 0.4900 0.0687 11.00000 0.05 0.11 Q2 1 0.8008 0.4837 0.4426 11.00000 0.05 0.10 Q3 1 0.7859 0.5158 0.4562 11.00000 0.05 0.10 Q4 1 1.0557 0.2651 0.0810 11.00000 0.05 0.10 Q5 1 0.7180 0.4923 0.4082 11.00000 0.05 0.09 Q6 1 0.9758 0.2680 0.0706 11.00000 0.05 0.09 Q7 1 1.0205 0.2903 0.1277 11.00000 0.05 0.09 Q8 1 1.0445 0.2922 0.0886 11.00000 0.05 0.09 Q9 1 1.0418 0.2827 0.1219 11.00000 0.05 0.09 Q10 1 0.7846 0.2612 0.1413 11.00000 0.05 0.09 Q11 1 0.8349 0.5381 0.1126 11.00000 0.05 0.09 Q12 1 0.9025 0.0789 0.1522 11.00000 0.05 0.09 Q13 1 0.8215 0.5130 0.1098 11.00000 0.05 0.09 Q14 1 0.4990 0.4667 0.3068 11.00000 0.05 0.08 Q15 1 0.8189 0.5806 0.1303 11.00000 0.05 0.08 Q16 1 0.7378 0.7295 0.0520 11.00000 0.05 0.08 Q17 1 0.9590 0.3524 0.0858 11.00000 0.05 0.08 Q18 1 0.8579 0.1081 0.1536 11.00000 0.05 0.08 Q19 1 0.6589 0.5367 0.2314 11.00000 0.05 0.08 Q20 1 0.7240 0.5814 0.0392 11.00000 0.05 0.07 ; _shelx_res_checksum 16205 _shelx_hkl_file ; 1 1 0 360.95 18.33 -1 -1 0 339.13 18.33 1 2 0 354.66 19.02 -1 -2 0 371.30 19.02 -2 -2 0 4.10 0.29 2 2 0 3.90 0.29 0 -3 0 0.01 0.08 -1 -3 0 18.61 1.05 1 3 0 19.15 1.07 -2 -3 0 243.22 14.02 3 2 0 266.02 14.05 2 3 0 291.63 14.05 3 3 0 3.47 0.33 0 -4 0 76.60 4.08 1 4 0 8.10 0.56 -1 -4 0 9.30 0.55 -2 -4 0 162.04 8.44 2 4 0 157.39 8.46 3 4 0 31.76 1.82 -3 -4 0 33.85 1.80 4 3 0 30.71 1.82 4 4 0 103.99 5.59 0 -5 0 0.02 0.14 -1 -5 0 45.30 2.39 1 5 0 42.12 2.40 -2 -5 0 8.96 0.57 2 5 0 7.80 0.59 5 3 0 331.59 18.21 3 5 0 361.21 18.21 -3 -5 0 343.35 18.17 4 5 0 0.61 0.26 5 4 0 0.42 0.22 5 5 0 137.99 7.41 0 -6 0 360.15 18.93 -1 -6 0 26.52 1.47 1 6 0 24.92 1.49 2 6 0 20.41 1.26 -2 -6 0 21.39 1.22 -3 -6 0 12.35 0.77 3 6 0 10.84 0.81 4 6 0 40.16 2.37 -4 -6 0 42.90 2.32 6 4 0 41.00 2.39 6 5 0 29.90 1.84 5 6 0 31.06 1.84 6 6 0 8.20 0.74 0 -7 0 -0.03 0.21 1 7 0 65.78 3.73 -1 -7 0 71.23 3.71 2 7 0 30.78 1.74 -2 -7 0 28.42 1.68 -3 -7 0 30.74 1.67 3 7 0 26.96 1.72 -4 -7 0 11.94 0.89 4 7 0 16.31 1.03 7 5 0 9.83 0.80 5 7 0 9.51 0.83 6 7 0 328.78 17.53 7 6 0 331.57 17.53 7 7 0 48.96 2.87 0 -8 0 14.09 0.90 1 -8 0 100.20 5.14 -1 -8 0 96.24 5.15 1 8 0 91.05 5.16 2 8 0 114.05 6.12 -2 -8 0 111.75 6.04 -3 -8 0 19.41 1.11 3 8 0 16.40 1.20 4 8 0 33.01 1.88 -4 -8 0 27.89 1.74 5 8 0 5.07 0.69 6 8 0 10.50 0.99 8 6 0 10.44 0.94 8 7 0 53.65 3.15 7 8 0 53.43 3.17 8 8 0 10.90 1.06 0 -9 0 -0.23 0.23 1 -9 0 31.07 1.71 1 9 0 28.75 1.74 -1 -9 0 28.55 1.71 -2 -9 0 -0.08 0.20 2 9 0 0.25 0.39 3 9 0 -0.07 0.29 -3 -9 0 1.23 0.26 4 9 0 55.87 3.40 -4 -9 0 63.57 3.31 5 9 0 107.12 5.73 -5 -9 0 99.50 5.58 6 9 0 7.70 0.90 9 7 0 0.37 0.47 7 9 0 -0.05 0.46 8 9 0 -0.11 0.41 9 8 0 0.51 0.42 9 9 0 86.72 5.01 0 -10 0 5.49 0.58 1 -10 0 12.79 0.90 -1 -10 0 13.36 0.91 -2 -10 0 1.41 0.29 2 10 0 1.35 0.36 -3 -10 0 96.52 5.08 3 10 0 91.25 5.19 -4 -10 0 0.56 0.29 4 10 0 0.45 0.42 5 10 0 11.51 1.16 -5 -10 0 17.63 1.05 6 10 0 6.52 0.88 7 10 0 37.87 2.45 8 10 0 91.58 5.30 10 8 0 93.68 5.30 10 9 0 3.38 0.76 9 10 0 3.79 0.87 10 10 0 4.82 0.93 0 -11 0 0.03 0.28 -1 -11 0 0.77 0.27 1 -11 0 0.80 0.40 -2 -11 0 18.82 1.16 2 11 0 17.62 1.29 3 11 0 1.53 0.48 -3 -11 0 1.43 0.31 -4 -11 0 37.55 2.07 4 11 0 33.03 2.25 -5 -11 0 51.33 2.85 5 11 0 48.72 3.01 6 11 0 27.92 1.94 7 11 0 27.25 1.95 8 11 0 20.62 1.71 9 11 0 0.74 0.77 10 11 0 8.20 1.34 11 10 0 12.12 1.40 11 11 0 11.01 1.44 0 -12 0 5.84 0.61 -1 -12 0 1.70 0.37 1 -12 0 1.92 0.41 2 12 0 0.77 0.43 -2 -12 0 0.62 0.29 2 -12 0 0.38 0.41 3 12 0 5.63 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12.9434 0.0000 12 0 7 -0.0000 -11.7530 12 0 8 2.8503 0.0000 12 0 9 -0.0000 -5.7408 12 0 11 -0.0000 -13.5258 12 0 12 8.7478 0.0000 12 0 13 -0.0000 -5.1197 12 0 14 -0.2450 0.0000 12 0 15 0.0000 3.9913 12 0 16 1.0246 -0.0000 12 0 17 -0.0000 -1.5427 12 0 18 7.2446 0.0000 12 0 19 0.0000 2.9483 12 0 20 -0.2533 0.0000 12 1 0 5.3719 -0.0000 12 1 1 8.2876 1.8738 12 1 2 1.1553 -7.1853 12 1 3 2.2482 11.2316 12 1 4 -7.6315 -2.3222 12 1 5 2.6848 6.0843 12 1 7 12.1931 1.6919 12 1 8 -6.2494 -5.9173 12 1 9 3.0486 0.7971 12 1 10 -4.8805 -4.9844 12 1 11 2.4849 8.0909 12 1 12 -1.4415 1.3141 12 1 13 3.4222 2.7338 12 1 14 -4.3363 -1.2353 12 1 15 2.1228 0.0374 12 1 16 3.8530 2.9404 12 1 17 -0.5880 10.6289 12 1 18 -2.1246 -4.5940 12 1 19 -0.8878 -2.4329 12 1 20 0.8973 -1.1702 12 2 0 -0.4865 -0.0000 12 2 1 -8.3864 -1.0810 12 2 8 -5.2174 -4.5686 12 2 9 -2.6354 -7.4608 12 2 10 0.6919 -2.7122 12 2 11 4.5734 -3.9587 12 2 12 0.0572 -1.3264 12 2 13 0.9376 0.2318 12 2 14 5.8108 0.0013 12 2 15 6.5523 -2.0339 12 2 16 -0.3195 3.2412 12 2 17 1.7963 4.5782 12 2 18 -3.0156 0.5573 12 2 19 5.0719 2.4100 12 3 0 4.0229 -0.0000 12 3 1 7.4308 11.0200 12 3 2 -7.6853 1.4037 12 3 3 -0.8975 7.0174 12 3 4 2.2208 -1.3802 12 3 5 8.6674 -4.5540 12 3 6 -7.0789 0.9357 12 3 8 -5.8234 1.0703 12 3 9 12.7388 -0.2515 12 3 10 -3.1183 0.6559 12 3 11 0.8958 11.9527 12 3 12 5.1138 -7.3584 12 3 13 4.5328 2.2682 12 3 14 -0.7410 -2.3022 12 3 15 -0.0806 4.5120 12 3 16 -0.1537 -0.6612 12 3 17 2.7247 -0.7158 12 3 18 2.3184 0.6273 12 3 19 -1.1098 -0.8705 12 4 0 7.3228 -0.0000 12 4 1 0.7478 1.4144 12 4 2 -1.0331 -3.8144 12 4 3 -2.4758 4.6505 12 4 4 -0.1362 -3.9839 12 4 5 -1.4209 4.6467 12 4 6 3.8511 -4.6593 12 4 7 1.6106 -2.2068 12 4 8 9.9398 -5.4457 12 4 9 3.5897 7.5357 12 4 10 3.9844 1.0337 12 4 11 0.8605 0.4061 12 4 12 4.9546 1.5208 12 4 13 -2.7118 -5.0893 12 4 14 6.5496 4.6080 12 4 15 -2.0009 -4.6596 12 4 16 -0.7412 -0.1050 12 4 17 0.8716 -2.2664 12 4 18 2.4007 4.4418 12 5 0 -2.2317 0.0000 12 5 1 -5.7204 8.6545 12 5 2 -2.4195 7.0290 12 5 3 7.8728 4.2012 12 5 4 -9.1873 6.7882 12 5 5 -1.3258 -3.7708 12 5 6 1.1738 6.3409 12 5 7 5.0127 1.2206 12 5 8 1.5280 -1.1467 12 5 9 4.1736 -5.3025 12 5 10 -4.8662 -2.5271 12 5 11 2.5152 3.6493 12 5 12 4.2181 -9.0347 12 5 13 -0.3397 -5.7938 12 5 14 0.0115 -5.0588 12 5 15 3.1886 1.2983 12 5 16 -0.6697 1.6404 12 5 17 0.7619 1.2017 12 6 0 -0.1766 0.0000 12 6 1 -4.8482 -4.0518 12 6 2 3.9413 5.1726 12 6 3 -3.2233 10.9372 12 6 4 2.7026 -8.8409 12 6 5 -3.5198 -2.2056 12 6 6 6.6645 -7.8707 12 6 7 -1.9308 6.2401 12 6 8 -0.8906 -1.1594 12 6 9 -3.3064 3.2157 12 6 10 -10.5079 -5.1199 12 6 11 4.3128 -1.7464 12 6 12 0.3833 2.5405 12 6 13 0.3489 6.4051 12 6 14 -6.3663 1.4741 12 6 15 -0.4256 -2.0757 12 6 16 -1.4217 4.6801 12 7 0 -0.4505 -0.0000 12 7 1 8.3114 -4.6163 12 7 2 -3.4332 -10.4955 12 7 3 6.5457 3.7002 12 7 4 4.1046 -0.7245 12 7 5 0.8786 7.8186 12 7 6 -4.7186 3.2789 12 7 7 -1.6190 1.0383 12 7 8 -0.9936 2.1420 12 7 9 -7.7953 -0.1154 12 7 10 0.6668 5.3733 12 7 11 -1.5964 -0.1733 12 7 12 -0.4135 -4.3995 12 7 13 -3.4599 3.1436 12 7 14 -1.2173 4.5022 12 7 15 -4.2641 1.5581 12 8 0 3.3286 -0.0000 12 8 1 -8.3037 -1.6610 12 8 2 3.9717 -2.9565 12 8 3 -0.4280 3.5604 12 8 4 2.4892 -1.5842 12 8 5 -0.4629 3.5113 12 8 6 -5.0305 4.6896 12 8 7 -0.7744 -3.4775 12 8 8 -3.7319 0.6739 12 8 9 1.6650 2.6227 12 8 10 -4.6570 3.7464 12 8 11 0.7694 -3.0509 12 8 12 -3.3045 -0.3324 12 8 13 0.0824 3.0911 12 9 0 -6.3713 0.0000 12 9 1 3.3827 -5.0597 12 9 2 -6.9664 -4.6994 12 9 3 5.1050 0.8141 12 9 4 -2.4073 -3.3999 12 9 5 3.3886 -6.8539 12 9 6 -2.5608 0.9452 12 9 7 -0.5021 3.2415 12 9 8 -3.0514 -2.0978 12 9 9 -3.4007 -2.6174 12 9 10 -1.9507 -2.8246 12 10 0 -1.1849 -0.0000 12 10 1 0.0915 -3.8309 12 10 2 -2.1682 2.3851 12 10 3 -3.5115 5.6709 12 10 4 -0.9215 0.8036 12 10 5 -3.2455 0.6271 12 10 6 -0.7396 0.0980 13 0 1 -2.3172 0.0000 13 0 2 0.0000 0.2028 13 0 3 -1.7791 0.0000 13 0 4 -0.0000 -13.1919 13 0 5 -5.7678 0.0000 13 0 6 -0.0000 -11.6009 13 0 7 5.0137 0.0000 13 0 8 -0.0000 -13.4834 13 0 9 6.2935 -0.0000 13 0 10 -0.0000 -7.9873 13 0 11 8.8830 -0.0000 13 0 12 -0.0000 -8.5333 13 0 13 -3.2472 -0.0000 13 0 14 -0.0000 -3.2256 13 0 15 -5.8721 0.0000 13 0 16 -0.0000 -0.8479 13 0 17 9.1650 0.0000 13 1 0 0.5983 0.0000 13 1 1 3.2869 -1.4839 13 1 2 -2.6643 0.1659 13 1 3 0.0297 2.3884 13 1 4 3.6018 -3.0819 13 1 5 3.1544 -11.1592 13 1 6 3.7150 5.0961 13 1 7 10.8358 -12.1148 13 1 8 5.6472 3.6986 13 1 9 2.4974 1.5053 13 1 10 -0.3338 7.3025 13 1 11 -0.2786 2.5845 13 1 12 -1.3350 3.4663 13 1 13 0.4395 -0.0514 13 1 14 -2.7720 6.5388 13 1 15 -5.6368 -1.0118 13 1 16 2.6877 2.4226 13 1 17 0.9161 -1.6190 13 2 0 0.1371 -0.0000 13 2 1 5.5806 11.6868 13 2 2 1.7902 2.9248 13 2 3 8.6879 -5.4797 13 2 9 2.6885 10.9543 13 2 10 4.5304 5.7876 13 2 11 4.4296 -3.9060 13 2 12 1.8775 -0.3939 13 2 13 5.5769 -0.7090 13 2 14 3.3455 2.1977 13 2 15 -2.9751 -2.8114 13 2 16 4.4662 -0.3808 13 2 17 -3.2974 0.5606 13 3 0 10.7638 -0.0000 13 3 1 -9.4275 -2.1880 13 3 2 -0.5154 -1.0858 13 3 3 -2.4312 4.1940 13 3 4 4.0242 -14.1607 13 3 9 -5.6706 -1.7087 13 3 10 7.6928 -4.3293 13 3 11 -4.6538 -1.3965 13 3 12 1.7271 2.2474 13 3 13 -0.2369 3.0924 13 3 14 4.4869 4.1026 13 3 15 1.0343 4.0869 13 3 16 10.0997 -1.2040 13 4 0 0.1590 -0.0000 13 4 1 5.9591 -4.2258 13 4 2 0.6893 7.7890 13 4 3 6.9837 -5.7360 13 4 4 4.5103 0.5744 13 4 5 0.9536 -10.6029 13 4 6 0.9586 -2.5057 13 4 7 2.3311 -3.2436 13 4 8 0.9625 9.4546 13 4 9 1.2710 -8.3771 13 4 10 11.4027 0.1816 13 4 11 4.3597 -7.5434 13 4 12 2.2381 -4.8822 13 4 13 5.6590 -0.8736 13 4 14 -0.3676 3.1963 13 4 15 1.3857 -5.5745 13 5 0 1.8625 0.0000 13 5 1 -0.6324 1.3443 13 5 2 -3.7905 0.9571 13 5 3 4.1064 -4.2892 13 5 4 0.8548 -5.0873 13 5 5 3.3510 3.9911 13 5 6 5.0531 3.7818 13 5 7 4.7317 -1.8228 13 5 8 -2.2647 -2.6492 13 5 9 1.5579 -0.1531 13 5 10 2.0551 1.0563 13 5 11 0.5020 6.0736 13 5 12 0.2533 2.6277 13 5 13 0.6891 3.3060 13 5 14 3.7678 -6.1951 13 6 0 -2.1811 0.0000 13 6 1 2.8788 -3.0936 13 6 2 1.5865 7.3235 13 6 3 -0.2224 3.2982 13 6 4 5.5784 9.5455 13 6 5 0.0859 3.2309 13 6 6 3.2845 -2.2360 13 6 7 -6.8335 -2.1076 13 6 8 8.4332 1.7890 13 6 9 2.3538 -4.1650 13 6 10 3.7217 -3.1939 13 6 11 -2.7864 -1.6339 13 6 12 1.7707 -2.5718 13 6 13 -2.5616 -6.3743 13 7 0 3.6919 -0.0000 13 7 1 8.0982 -3.6053 13 7 2 -1.5903 5.4331 13 7 3 2.4115 -4.0999 13 7 4 -6.8403 -0.4700 13 7 5 2.0485 -6.0474 13 7 6 2.5230 4.8339 13 7 7 4.1152 -0.4869 13 7 8 -0.3918 3.3548 13 7 9 1.1450 0.5994 13 7 10 -1.3066 -0.0781 13 7 11 -6.7583 0.5823 13 8 0 6.3851 -0.0000 13 8 1 2.8095 -1.3414 13 8 2 2.1394 4.0853 13 8 3 5.1732 6.0851 13 8 4 -5.6364 0.1454 13 8 5 -3.8749 1.3520 13 8 6 0.1703 0.3783 13 8 7 1.9371 3.3587 13 8 8 -1.6752 1.1189 13 8 9 -4.5453 4.5182 13 9 0 2.1489 -0.0000 13 9 1 0.9915 0.0537 13 9 2 2.7283 -1.5802 13 9 3 4.4423 -0.3894 13 9 4 1.0058 2.7251 14 0 0 0.7488 -0.0000 14 0 1 -0.0000 -0.9739 14 0 2 3.2213 0.0000 14 0 3 0.0000 3.5508 14 0 4 1.3666 0.0000 14 0 5 0.0000 1.4706 14 0 6 -1.0872 -0.0000 14 0 7 0.0000 3.8364 14 0 8 -7.8459 0.0000 14 0 9 0.0000 1.5329 14 0 10 -4.2793 0.0000 14 0 13 0.0000 2.3617 14 0 14 0.2989 0.0000 14 1 0 3.8052 -0.0000 14 1 1 0.4551 -6.0822 14 1 2 5.3225 -4.6019 14 1 3 5.2943 -0.2659 14 1 4 5.0064 5.0474 14 1 5 0.9921 -0.8703 14 1 6 -1.1495 2.9114 14 1 9 -3.6004 -0.3396 14 1 10 1.8188 -3.2464 14 1 11 -0.9175 -0.9725 14 1 12 2.2680 3.6429 14 1 13 0.2561 -5.7290 14 1 14 -0.6726 -4.4220 14 2 0 1.9108 -0.0000 14 2 1 -6.6029 -11.1071 14 2 2 -3.1443 -8.3704 14 2 3 -3.2390 -2.6028 14 2 4 7.7282 -1.7146 14 2 10 6.5703 -1.0059 14 2 11 -2.8385 2.1271 14 2 12 3.2035 4.9706 14 2 13 -2.4238 2.8790 14 2 14 3.9070 -0.2993 14 3 0 3.3255 -0.0000 14 3 1 3.1356 4.7300 14 3 2 1.9824 -1.9372 14 3 3 -1.5574 2.2883 14 3 10 -1.6312 6.5103 14 3 11 -4.9881 -0.5969 14 3 12 1.9049 2.3710 14 3 13 -2.2394 3.1003 14 4 0 2.8296 0.0000 14 4 1 -0.9310 5.3458 14 4 2 -5.3811 -2.1676 14 4 3 -0.0927 -6.9223 14 4 4 1.1235 1.2746 14 4 5 0.0584 3.2542 14 4 6 0.2431 4.2053 14 4 7 -3.4919 0.6288 14 4 10 3.3917 -0.2130 14 4 11 -1.0699 3.6121 14 4 12 -2.2796 -5.9242 14 5 0 0.9539 -0.0000 14 5 1 -1.6521 0.4743 14 5 2 0.9313 -2.2173 14 5 3 -5.9645 -4.6829 14 5 4 -1.2035 -1.0661 14 5 5 1.2739 -0.7995 14 5 6 3.9577 -0.8581 14 5 7 0.7369 -3.4683 14 5 8 -4.3753 3.3564 14 5 9 -0.7099 -0.9666 14 5 10 6.4244 -0.0339 14 5 11 4.5327 -0.3357 14 6 0 -0.4759 0.0000 14 6 1 -4.1184 -5.8627 14 6 2 -1.0335 2.6976 14 6 3 0.6423 -1.3216 14 6 4 3.4146 0.6821 14 6 5 -2.4546 0.0574 14 6 6 0.5760 1.4980 14 6 7 9.9280 -4.6678 14 6 8 2.5726 -2.6224 14 6 9 -1.4038 -4.2767 14 7 0 2.6753 -0.0000 14 7 1 -2.1491 1.5380 14 7 2 2.6412 -2.0411 14 7 3 -3.4251 -4.9761 14 7 4 3.1878 -3.0464 14 7 5 2.2626 0.5283 14 7 6 -4.3927 -1.1385 15 0 1 0.5297 0.0000 15 0 2 0.0000 7.1458 15 0 3 -5.0086 -0.0000 15 0 4 0.0000 1.0517 15 0 5 0.7239 -0.0000 15 0 6 -0.0000 -3.5860 15 0 7 -0.9420 -0.0000 15 0 8 -0.0000 -1.9686 15 0 9 6.3568 0.0000 15 0 10 -0.0000 -6.0036 15 1 0 -2.7584 -0.0000 15 1 1 -3.4002 -0.7217 15 1 2 -1.2306 0.2741 15 1 3 -4.5870 1.6391 15 1 4 0.1962 5.3316 15 1 5 2.3987 -5.2104 15 1 6 0.8866 4.5010 15 1 7 -7.3989 5.3135 15 1 8 0.5530 -1.8551 15 1 10 -1.2291 6.5880 15 2 0 -0.8254 0.0000 15 2 1 5.1565 -1.9136 15 2 2 3.2346 4.4634 15 2 3 0.8413 -3.2744 15 2 4 6.6312 6.8230 15 2 5 4.1373 -1.4505 15 3 0 8.5462 -0.0000 15 4 0 -4.6029 0.0000 15 4 1 -9.9662 -2.5885 15 4 2 -0.5266 1.3786 15 4 3 -0.8724 -0.3187 15 4 4 1.0886 -0.7128 15 4 5 -7.6517 -4.1520 15 5 0 -3.4598 -0.0000 15 5 1 1.5571 -3.7991 15 5 2 -5.0914 2.8000 15 5 3 -3.3238 3.6839 15 5 4 1.0145 0.1704 0 0 0 0.0 0.0 ; _shelx_fab_checksum 31049 _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 0.66349(8) 0.33651(8) 0.5000 0.0507(8) Uani 1 2 d S TU P . . Al2 Al 0.61670(9) 0.38957(9) 0.41625(5) 0.0536(6) Uani 1 1 d . U . . . Al3 Al 0.5000 0.5000 0.38334(7) 0.0516(8) Uani 1 2 d S TU P . . O2 O 0.56495(16) 0.47062(16) 0.41844(11) 0.0515(11) Uani 1 1 d . U . . . H2 H 0.5717 0.4993 0.4387 0.062 Uiso 1 1 calc R . . . . O3 O 0.6395(2) 0.4010(2) 0.36565(13) 0.0620(13) Uani 1 1 d . U . . . O1 O 0.60065(17) 0.36668(17) 0.46646(10) 0.0555(12) Uani 1 1 d . U . . . H1 H 0.5550 0.3716 0.4747 0.067 Uiso 1 1 calc R . . . . O4 O 0.5590(2) 0.47333(19) 0.34441(11) 0.0608(13) Uani 1 1 d . U . . . C1 C 0.6117(4) 0.4354(3) 0.3402(2) 0.0550(19) Uani 1 1 d . U . . . C26 C 0.7689(4) 0.6312(4) 0.1400(2) 0.091(2) Uani 1 1 d . U . . . H26 H 0.7643 0.6290 0.1653 0.109 Uiso 1 1 calc R U . . . C23 C 0.7793(4) 0.6300(4) 0.0677(2) 0.094(2) Uani 1 1 d . U . . . H23 H 0.7790 0.6305 0.0423 0.113 Uiso 1 1 calc R U . . . C20 C 0.9755(4) 0.1505(4) 0.11125(18) 0.060(2) Uani 1 1 d . U . . . C25 C 0.7798(4) 0.6924(4) 0.1252(2) 0.092(2) Uani 1 1 d . U . . . H25 H 0.7823 0.7331 0.1389 0.110 Uiso 1 1 calc R U . . . C22 C 0.7712(4) 0.5676(4) 0.0850(2) 0.088(3) Uani 1 1 d . U . . . H22 H 0.7717 0.5268 0.0713 0.105 Uiso 1 1 calc R U . . . C24 C 0.7876(3) 0.6917(4) 0.0857(2) 0.077(2) Uani 1 1 d . U . . . C27 C 0.8039(3) 0.7570(4) 0.0627(2) 0.057(2) Uani 1 1 d . U . . . C17 C 0.9330(4) 0.2084(3) 0.12017(18) 0.066(2) Uani 1 1 d . U . . . C7 C 0.6120(4) 0.4752(4) 0.2758(2) 0.110(3) Uani 1 1 d . U . . . H7 H 0.5706 0.4999 0.2786 0.132 Uiso 1 1 calc R U . . . C21 C 0.7633(3) 0.5638(3) 0.1185(2) 0.062(2) Uani 1 1 d . U . . . C16 C 0.8693(4) 0.1966(3) 0.1387(2) 0.090(3) Uani 1 1 d . U . . . H16 H 0.8541 0.1520 0.1448 0.108 Uiso 1 1 calc R U . . . C2 C 0.6439(4) 0.4353(3) 0.3069(2) 0.068(2) Uani 1 1 d . U . . . C18 C 0.9578(4) 0.2762(3) 0.1085(2) 0.107(3) Uani 1 1 d . U . . . H18 H 0.9996 0.2839 0.0962 0.128 Uiso 1 1 calc R U . . . C14 C 0.8429(4) 0.3215(4) 0.13833(19) 0.070(2) Uani 1 1 d . U . . . C6 C 0.6454(4) 0.4737(4) 0.2442(2) 0.109(3) Uani 1 1 d . U . . . H6 H 0.6285 0.5063 0.2275 0.130 Uiso 1 1 calc R U . . . C13 C 0.7303(4) 0.4934(4) 0.1741(2) 0.103(3) Uani 1 1 d . U . . . H13 H 0.7076 0.5332 0.1824 0.123 Uiso 1 1 calc R U . . . C19 C 0.9068(4) 0.3325(4) 0.1189(2) 0.088(2) Uani 1 1 d . U . . . H19 H 0.9176 0.3780 0.1121 0.105 Uiso 1 1 calc R U . . . C10 C 0.8031(4) 0.3816(4) 0.1482(2) 0.088(2) Uani 1 1 d . U . . . C15 C 0.8321(4) 0.2540(4) 0.14696(19) 0.081(2) Uani 1 1 d . U . . . H15 H 0.7924 0.2458 0.1609 0.097 Uiso 1 1 calc R U . . . C12 C 0.7627(4) 0.4950(4) 0.1370(2) 0.088(2) Uani 1 1 d . U . . . C9 C 0.7681(4) 0.3786(3) 0.1826(2) 0.090(2) Uani 1 1 d . U . . . H9 H 0.7691 0.3376 0.1962 0.108 Uiso 1 1 calc R U . . . O8 O 0.82701(19) 0.8037(2) 0.08835(12) 0.0687(13) Uani 1 1 d . U . . . O10 O 0.73317(18) 0.3990(2) 0.48188(12) 0.0625(13) Uani 1 1 d . U . . . O5 O 1.0379(2) 0.16650(18) 0.09799(11) 0.0577(13) Uani 1 1 d . U . . . O6 O 0.95740(18) 0.0894(2) 0.11988(11) 0.0554(12) Uani 1 1 d . U . . . O7 O 0.8013(2) 0.7646(2) 0.03226(16) 0.0735(17) Uani 1 1 d . U . . . O9 O 0.6971(2) 0.4398(2) 0.42654(14) 0.0720(14) Uani 1 1 d . U . . . C28 C 0.7395(4) 0.4454(4) 0.4531(2) 0.080(2) Uani 1 1 d . U . . . H28 H 0.7738 0.4797 0.4532 0.095 Uiso 1 1 calc R U . . . C5 C 0.6987(4) 0.4353(4) 0.2307(2) 0.088(2) Uani 1 1 d . U . . . C8 C 0.7322(4) 0.4372(4) 0.1964(3) 0.094(3) Uani 1 1 d . U . . . C3 C 0.7000(4) 0.3965(4) 0.2976(2) 0.111(3) Uani 1 1 d . U . . . H3 H 0.7192 0.3681 0.3156 0.133 Uiso 1 1 calc R U . . . C4 C 0.7315(4) 0.3955(4) 0.2633(2) 0.100(3) Uani 1 1 d . U . . . H4 H 0.7726 0.3706 0.2599 0.121 Uiso 1 1 calc R U . . . C11 C 0.7987(3) 0.4415(3) 0.1263(2) 0.081(2) Uani 1 1 d . U . . . H11 H 0.8218 0.4428 0.1040 0.097 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 0.0519(11) 0.0519(11) 0.048(2) -0.0022(11) -0.0022(11) 0.0072(13) Al2 0.0656(14) 0.0455(13) 0.0497(17) -0.0054(10) -0.0061(10) 0.0174(10) Al3 0.0626(19) 0.0497(19) 0.042(2) 0.000 0.000 0.0120(13) O2 0.048(2) 0.059(3) 0.048(3) -0.0053(19) -0.0016(18) 0.0069(19) O3 0.079(3) 0.056(3) 0.051(4) 0.000(2) 0.019(2) 0.020(2) O1 0.051(2) 0.066(3) 0.049(3) 0.017(2) -0.0053(19) 0.018(2) O4 0.083(3) 0.058(3) 0.041(3) -0.001(2) 0.006(2) 0.019(3) C1 0.081(5) 0.044(4) 0.039(5) -0.001(4) 0.019(4) 0.020(4) C26 0.156(7) 0.073(5) 0.044(6) 0.023(4) 0.031(4) -0.001(4) C23 0.124(7) 0.091(5) 0.067(6) 0.001(4) 0.017(4) -0.031(5) C20 0.084(5) 0.044(5) 0.053(6) -0.001(4) 0.028(4) 0.017(4) C25 0.158(7) 0.072(5) 0.046(6) 0.019(4) 0.004(5) -0.023(5) C22 0.140(7) 0.068(5) 0.055(6) 0.016(4) 0.057(5) -0.019(4) C24 0.103(5) 0.072(5) 0.057(6) 0.021(4) 0.024(4) -0.026(4) C27 0.075(5) 0.052(5) 0.045(6) 0.007(4) -0.008(4) -0.013(3) C17 0.095(5) 0.052(5) 0.052(6) -0.009(3) 0.032(4) 0.022(4) C7 0.134(7) 0.119(7) 0.076(7) 0.048(5) 0.032(5) 0.071(5) C21 0.073(4) 0.049(4) 0.062(6) 0.011(4) 0.049(4) 0.000(3) C16 0.109(5) 0.039(4) 0.121(7) -0.018(4) 0.066(5) 0.005(4) C2 0.087(5) 0.054(4) 0.063(6) 0.008(4) 0.028(4) 0.039(4) C18 0.127(6) 0.046(5) 0.147(8) 0.008(4) 0.041(5) 0.012(4) C14 0.087(5) 0.059(5) 0.064(6) -0.006(4) 0.009(4) -0.001(4) C6 0.155(7) 0.102(6) 0.069(7) 0.050(5) 0.033(5) 0.093(6) C13 0.157(7) 0.042(4) 0.109(7) 0.010(4) 0.070(5) 0.016(5) C19 0.108(5) 0.077(5) 0.078(6) -0.007(4) 0.015(4) -0.001(4) C10 0.107(6) 0.067(5) 0.089(7) 0.000(4) 0.036(4) 0.007(4) C15 0.108(6) 0.055(5) 0.079(6) -0.011(4) 0.043(4) 0.006(4) C12 0.098(6) 0.060(5) 0.107(7) 0.006(4) 0.038(4) 0.006(4) C9 0.123(6) 0.044(4) 0.103(7) 0.020(4) 0.045(5) 0.015(4) O8 0.071(3) 0.070(3) 0.064(4) 0.026(2) 0.013(2) -0.017(2) O10 0.048(3) 0.062(3) 0.078(4) -0.020(2) 0.000(2) 0.002(2) O5 0.085(3) 0.042(3) 0.046(3) -0.015(2) 0.023(2) 0.010(2) O6 0.073(3) 0.046(3) 0.047(3) -0.002(2) 0.018(2) 0.010(2) O7 0.103(4) 0.070(3) 0.048(4) 0.025(3) -0.013(3) -0.014(2) O9 0.060(3) 0.074(3) 0.082(4) 0.000(3) 0.012(3) -0.010(2) C28 0.069(5) 0.097(6) 0.072(7) 0.000(5) 0.010(4) -0.005(4) C5 0.103(6) 0.071(5) 0.090(6) 0.028(4) 0.025(5) 0.034(4) C8 0.131(6) 0.041(5) 0.111(7) 0.010(4) 0.049(5) 0.034(4) C3 0.135(7) 0.110(6) 0.087(7) 0.037(5) 0.045(5) 0.077(5) C4 0.102(6) 0.114(6) 0.086(7) 0.016(5) 0.033(5) 0.056(5) C11 0.103(5) 0.045(4) 0.094(6) 0.015(4) 0.061(4) 0.035(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0010 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 91.9(3) . 8_666 O1 Al1 O10 91.76(17) 8_666 8_666 O1 Al1 O10 92.33(16) 8_666 . O1 Al1 O10 92.33(16) . 8_666 O1 Al1 O10 91.76(17) . . O1 Al1 O7 92.73(18) 8_666 2_645 O1 Al1 O7 175.0(2) 8_666 6_645 O1 Al1 O7 92.73(19) . 6_645 O1 Al1 O7 175.0(2) . 2_645 O10 Al1 O10 174.1(3) 8_666 . O10 Al1 O7 86.02(19) . 2_645 O10 Al1 O7 89.57(18) 8_666 2_645 O10 Al1 O7 86.02(19) 8_666 6_645 O10 Al1 O7 89.57(18) . 6_645 O7 Al1 O7 82.8(3) 2_645 6_645 O2 Al2 O3 93.89(18) . . O2 Al2 O1 93.75(17) . . O2 Al2 O8 177.5(2) . 6_645 O2 Al2 O5 93.44(17) . 5_455 O2 Al2 O9 90.03(17) . . O3 Al2 O8 83.61(18) . 6_645 O3 Al2 O5 89.00(18) . 5_455 O1 Al2 O3 172.35(17) . . O1 Al2 O8 88.75(18) . 6_645 O1 Al2 O5 90.27(18) . 5_455 O5 Al2 O8 86.58(17) 5_455 6_645 O9 Al2 O3 86.9(2) . . O9 Al2 O1 93.4(2) . . O9 Al2 O8 89.78(18) . 6_645 O9 Al2 O5 174.8(2) . 5_455 O2 Al3 O2 93.7(3) . 3_665 O2 Al3 O4 92.03(16) 3_665 3_665 O2 Al3 O4 174.3(2) 3_665 . O2 Al3 O4 92.03(16) . . O2 Al3 O4 174.3(2) . 3_665 O2 Al3 O6 93.24(16) . 5_455 O2 Al3 O6 93.24(16) 3_665 6_655 O2 Al3 O6 91.60(16) 3_665 5_455 O2 Al3 O6 91.60(16) . 6_655 O4 Al3 O4 82.3(3) . 3_665 O4 Al3 O6 88.09(17) 3_665 6_655 O4 Al3 O6 86.57(17) 3_665 5_455 O4 Al3 O6 88.09(17) . 5_455 O4 Al3 O6 86.57(17) . 6_655 O6 Al3 O6 172.9(3) 5_455 6_655 Al2 O2 Al3 125.5(2) . . C1 O3 Al2 132.7(5) . . Al1 O1 Al2 127.9(2) . . C1 O4 Al3 137.1(4) . . O3 C1 C2 117.9(7) . . O4 C1 O3 123.6(7) . . O4 C1 C2 118.3(7) . . C25 C26 C21 124.2(7) . . C22 C23 C24 123.6(8) . . O5 C20 C17 115.0(6) . . O6 C20 C17 120.8(7) . . O6 C20 O5 123.6(6) . . C26 C25 C24 114.8(7) . . C21 C22 C23 121.7(8) . . C23 C24 C25 118.3(6) . . C23 C24 C27 117.8(8) . . C25 C24 C27 123.9(7) . . O8 C27 C24 102.9(7) . . O7 C27 C24 129.6(8) . . O7 C27 O8 127.4(7) . . C20 C17 C18 116.5(6) . . C16 C17 C20 118.8(6) . . C16 C17 C18 124.7(6) . . C6 C7 C2 117.0(7) . . C22 C21 C26 117.0(7) . . C22 C21 C12 120.2(7) . . C12 C21 C26 121.6(7) . . C15 C16 C17 115.6(6) . . C1 C2 C7 119.4(7) . . C3 C2 C1 125.8(7) . . C3 C2 C7 114.5(7) . . C17 C18 C19 110.8(6) . . C10 C14 C19 117.7(7) . . C15 C14 C19 112.8(7) . . C15 C14 C10 129.3(7) . . C7 C6 C5 134.2(7) . . C8 C13 C12 123.5(7) . . C14 C19 C18 125.2(7) . . C9 C10 C14 116.2(7) . . C11 C10 C14 123.3(7) . . C11 C10 C9 120.5(7) . . C16 C15 C14 130.7(7) . . C21 C12 C13 115.8(6) . . C11 C12 C21 124.3(7) . . C11 C12 C13 118.6(7) . . C8 C9 C10 120.8(7) . . C27 O8 Al2 131.5(5) . 6_655 C28 O10 Al1 136.7(5) . . C20 O5 Al2 132.6(4) . 5 C20 O6 Al3 134.7(4) . 5 C27 O7 Al1 132.8(5) . 4_564 C28 O9 Al2 136.9(6) . . O9 C28 O10 118.0(7) . . C6 C5 C8 130.9(7) . . C6 C5 C4 107.1(7) . . C8 C5 C4 120.8(7) . . C13 C8 C9 115.8(8) . . C13 C8 C5 122.9(7) . . C5 C8 C9 121.2(7) . . C2 C3 C4 125.4(7) . . C3 C4 C5 120.7(7) . . C12 C11 C10 120.6(7) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Al1 O1 1.814(4) . Al1 O1 1.814(4) 8_666 Al1 O10 1.913(4) . Al1 O10 1.913(4) 8_666 Al1 O7 1.936(5) 2_645 Al1 O7 1.936(5) 6_645 Al2 O2 1.846(4) . Al2 O3 1.913(5) . Al2 O1 1.911(4) . Al2 O8 1.976(4) 6_645 Al2 O5 1.926(4) 5_455 Al2 O9 1.857(5) . Al3 O2 1.875(4) . Al3 O2 1.875(4) 3_665 Al3 O4 1.889(5) 3_665 Al3 O4 1.888(5) . Al3 O6 1.904(4) 5_455 Al3 O6 1.904(4) 6_655 O3 C1 1.259(8) . O4 C1 1.255(7) . C1 C2 1.365(9) . C26 C25 1.308(8) . C26 C21 1.516(9) . C23 C22 1.362(9) . C23 C24 1.364(9) . C20 C17 1.417(8) . C20 O5 1.327(7) . C20 O6 1.262(7) . C25 C24 1.451(9) . C22 C21 1.235(8) . C24 C27 1.540(10) . C27 O8 1.371(8) . C27 O7 1.122(7) . C17 C16 1.415(8) . C17 C18 1.450(8) . C7 C2 1.500(9) . C7 C6 1.319(9) . C21 C12 1.484(9) . C16 C15 1.347(8) . C2 C3 1.353(8) . C18 C19 1.506(9) . C14 C19 1.432(9) . C14 C10 1.429(9) . C14 C15 1.348(8) . C6 C5 1.354(9) . C13 C12 1.492(9) . C13 C8 1.350(9) . C10 C9 1.426(9) . C10 C11 1.402(9) . C12 C11 1.296(8) . C9 C8 1.411(8) . O8 Al2 1.976(4) 6_655 O10 C28 1.384(8) . O5 Al2 1.926(4) 5 O6 Al3 1.904(4) 5 O7 Al1 1.936(5) 4_564 O9 C28 1.271(8) . C5 C8 1.409(9) . C5 C4 1.548(10) . C3 C4 1.391(9) . 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 -0.437 -0.834 -0.615 9495.8 13890.3