#------------------------------------------------------------------------------ #$Date: 2023-11-14 01:36:13 +0200 (Tue, 14 Nov 2023) $ #$Revision: 287568 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/77/7247705.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_7247705 loop_ _publ_author_name 'Ma, Yali' 'Wang, Haitang' 'Wang, Hailong' 'Wang, Jiani' 'Jiang, Shuaiyu' 'Zheng, Qiang' 'Jia, Songyan' 'Li, Xue' 'Ma, Tianyi' _publ_section_title ; A Stable Ultra-Microporous Hafnium-Based Metal-Organic Framework with High Performance for CO2 Adsorption and Separation ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D3CE01022H _journal_year 2023 _chemical_formula_moiety 'C120 H72 Hf6 O32' _chemical_formula_sum 'C120 H72 Hf6 O32' _chemical_formula_weight 3096.71 _space_group_crystal_system trigonal _space_group_IT_number 148 _space_group_name_Hall '-R 3' _space_group_name_H-M_alt 'R -3 :H' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2022-12-05 _audit_creation_method ; Olex2 1.5-ac5-024 (compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498) ; _audit_update_record ; 2023-10-15 deposited with the CCDC. 2023-11-13 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 3 _cell_length_a 30.238(6) _cell_length_b 30.238(6) _cell_length_c 15.131(5) _cell_measurement_reflns_used 4035 _cell_measurement_temperature 296.15 _cell_measurement_theta_max 21.686 _cell_measurement_theta_min 2.334 _cell_volume 11981(5) _computing_cell_refinement 'SAINT V8.32B (?, 2016)' _computing_data_reduction 'SAINT V8.32B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2019/2 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 296.15 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1138 _diffrn_reflns_av_unetI/netI 0.0662 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 25290 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 24.999 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 1.347 _diffrn_source_current 30.0 _diffrn_source_power 1.2 _diffrn_source_voltage 40.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.938 _exptl_absorpt_correction_T_max 0.08123 _exptl_absorpt_correction_T_min 0.01256 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.288 _exptl_crystal_description block _exptl_crystal_F_000 4440 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _refine_diff_density_max 1.237 _refine_diff_density_min -0.740 _refine_diff_density_rms 0.141 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 238 _refine_ls_number_reflns 4674 _refine_ls_number_restraints 822 _refine_ls_restrained_S_all 0.928 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0504 _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^)+(0.0948P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1386 _refine_ls_wR_factor_ref 0.1593 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2959 _reflns_number_total 4674 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce01022h2.cif _cod_data_source_block 1 _cod_original_cell_volume 11981(6) _cod_original_sg_symbol_H-M 'R -3' _cod_database_code 7247705 _shelx_shelxl_version_number 2019/2 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.629 _shelx_estimated_absorpt_t_min 0.506 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2. Uiso/Uaniso restraints and constraints C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6: within 5A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 5A 3.a Aromatic/amide H refined with riding coordinates: C2(H2), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C15(H15), C16(H16), C17(H17), C19(H19) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL 1_a.res in R-3 1.res created by SHELXL-2019/2 at 16:34:33 on 05-Dec-2022 REM Old TITL 1 in R-3 REM SHELXT solution in R-3: R1 0.136, Rweak 0.003, Alpha 0.040 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C61 O19 Hf3 CELL 0.71073 30.2379 30.2379 15.131 90 90 120 ZERR 3 0.0063 0.0063 0.0046 0 0 0 LATT 3 SYMM -Y,+X-Y,+Z SYMM +Y-X,-X,+Z SFAC C H Hf O UNIT 360 216 18 96 SIMU 0.01 0.02 5 $c $o L.S. 20 PLAN 18 SIZE 0.2 0.15 0.13 TEMP 23 CONF BOND LIST 4 MORE -1 ABIN BOND $H fmap 2 acta OMIT -3 50 OMIT -1 3 2 OMIT -4 5 0 OMIT 2 4 1 OMIT -2 2 2 OMIT -2 7 0 OMIT -2 4 3 OMIT -5 5 2 OMIT 0 0 3 OMIT 0 3 0 OMIT 1 1 0 OMIT 0 1 -1 OMIT 1 3 1 OMIT 2 3 -1 OMIT 4 2 -1 OMIT 3 5 1 OMIT 2 2 0 OMIT 1 2 -1 OMIT 2 4 -2 REM REM REM WGHT 0.094800 FVAR 0.06578 HF1 3 0.274705 0.594205 0.760652 11.00000 0.05886 0.05880 = 0.06621 0.00275 0.00104 0.02782 O1 4 0.333333 0.666667 0.806075 10.33333 0.08135 0.08135 = 0.10636 0.00000 0.00000 0.04068 O2 4 0.260109 0.516675 0.729691 11.00000 0.12329 0.07761 = 0.10833 -0.01115 -0.01743 0.05052 O3 4 0.036724 0.097619 0.207481 11.00000 0.12306 0.08748 = 0.10818 -0.01720 -0.03237 0.05450 O4 4 0.310265 0.525928 0.598930 11.00000 0.12349 0.07439 = 0.09739 -0.01131 -0.01025 0.04956 O5 4 0.261692 0.653061 0.712757 11.00000 0.12564 0.06792 = 0.10294 -0.00307 -0.04270 0.04127 O6 4 0.093836 0.063727 0.209484 11.00000 0.12523 0.08347 = 0.10904 -0.02083 -0.02670 0.05292 C1 1 0.075613 0.092245 0.235708 11.00000 0.13313 0.08874 = 0.11408 -0.02109 -0.02891 0.05464 C2 1 0.224063 0.412990 0.722393 11.00000 0.14466 0.08735 = 0.11123 -0.01261 -0.00776 0.03911 AFIX 43 H2 2 0.212714 0.425775 0.767461 11.00000 -1.20000 AFIX 0 C3 1 0.219459 0.337626 0.653124 11.00000 0.14243 0.08651 = 0.10909 -0.01344 -0.01297 0.04460 C4 1 0.276868 0.500268 0.663517 11.00000 0.13168 0.08087 = 0.10771 -0.00846 -0.01262 0.04777 C5 1 0.160950 0.206071 0.558913 11.00000 0.14148 0.08633 = 0.11460 -0.01583 -0.02114 0.04928 C6 1 0.180806 0.258371 0.564424 11.00000 0.14289 0.08835 = 0.11417 -0.01589 -0.01776 0.04723 AFIX 43 H6 2 0.182572 0.276800 0.514037 11.00000 -1.20000 AFIX 0 C7 1 0.152942 0.177795 0.635877 11.00000 0.14442 0.08855 = 0.11480 -0.01628 -0.02329 0.04672 AFIX 43 H7 2 0.136800 0.142369 0.632900 11.00000 -1.20000 AFIX 0 C8 1 0.271318 0.422578 0.591686 11.00000 0.14207 0.08705 = 0.11181 -0.01436 -0.00775 0.04354 AFIX 43 H8 2 0.294204 0.443123 0.548348 11.00000 -1.20000 AFIX 0 C9 1 0.146632 0.137947 0.451438 11.00000 0.14270 0.09280 = 0.11777 -0.01943 -0.02896 0.05201 AFIX 43 H9 2 0.163081 0.127036 0.490231 11.00000 -1.20000 AFIX 0 C10 1 0.099649 0.168830 0.334187 11.00000 0.13712 0.08892 = 0.11643 -0.02153 -0.02684 0.05593 AFIX 43 H10 2 0.082999 0.179653 0.295675 11.00000 -1.20000 AFIX 0 C11 1 0.198262 0.283698 0.645533 11.00000 0.14260 0.08603 = 0.11070 -0.01387 -0.01672 0.04508 C12 1 0.168474 0.201497 0.714874 11.00000 0.14781 0.09018 = 0.11367 -0.01328 -0.02150 0.04434 AFIX 43 H12 2 0.164555 0.182511 0.765609 11.00000 -1.20000 AFIX 0 C13 1 0.252138 0.370671 0.587801 11.00000 0.14414 0.08758 = 0.11232 -0.01410 -0.01022 0.03942 AFIX 43 H13 2 0.261112 0.357128 0.540490 11.00000 -1.20000 AFIX 0 C14 1 0.101461 0.125200 0.315333 11.00000 0.13202 0.08956 = 0.11538 -0.01958 -0.03297 0.05975 C15 1 0.207273 0.360646 0.718755 11.00000 0.14551 0.08840 = 0.11143 -0.01260 -0.01059 0.04017 AFIX 43 H15 2 0.186372 0.340157 0.764217 11.00000 -1.20000 AFIX 0 C16 1 0.121607 0.195796 0.407361 11.00000 0.13760 0.08966 = 0.11603 -0.01728 -0.02585 0.05361 AFIX 43 H16 2 0.122781 0.226932 0.414172 11.00000 -1.20000 AFIX 0 C17 1 0.190194 0.253964 0.720349 11.00000 0.14785 0.08946 = 0.11279 -0.01302 -0.01681 0.04107 AFIX 43 H17 2 0.199611 0.269695 0.775366 11.00000 -1.20000 AFIX 0 C18 1 0.257612 0.445899 0.658930 11.00000 0.13914 0.08522 = 0.10901 -0.01314 -0.00873 0.04093 C19 1 0.126678 0.111294 0.373090 11.00000 0.14019 0.09287 = 0.11831 -0.02035 -0.03126 0.05413 AFIX 43 H19 2 0.130678 0.083442 0.360016 11.00000 -1.20000 AFIX 0 C20 1 0.142636 0.180661 0.473442 11.00000 0.13879 0.08743 = 0.11554 -0.01832 -0.02467 0.05367 HKLF 4 REM 1_a.res in R-3 REM wR2 = 0.1593, GooF = S = 0.974, Restrained GooF = 0.928 for all data REM R1 = 0.0504 for 2959 Fo > 4sig(Fo) and 0.0765 for all 4674 data REM 238 parameters refined using 822 restraints END WGHT 0.0947 0.0000 REM Highest difference peak 1.237, deepest hole -0.740, 1-sigma level 0.141 Q1 1 0.2437 0.5678 0.7631 11.00000 0.05 1.24 Q2 1 0.2843 0.6265 0.7730 11.00000 0.05 1.18 Q3 1 0.3026 0.5906 0.7587 11.00000 0.05 1.16 Q4 1 0.2466 0.5997 0.7586 11.00000 0.05 0.96 Q5 1 0.2703 0.5598 0.7639 11.00000 0.05 0.92 Q6 1 0.3077 0.6250 0.7620 11.00000 0.05 0.91 Q7 1 0.2439 0.5100 0.7852 11.00000 0.05 0.84 Q8 1 0.3333 0.6667 0.8561 10.33333 0.05 0.63 Q9 1 0.2296 0.4657 0.7589 11.00000 0.05 0.57 Q10 1 0.2406 0.6401 0.7505 11.00000 0.05 0.50 Q11 1 0.0460 0.1368 0.2811 11.00000 0.05 0.48 Q12 1 0.0229 0.1147 0.2164 11.00000 0.05 0.47 Q13 1 0.1734 0.2159 0.2851 11.00000 0.05 0.41 Q14 1 0.1304 0.0897 0.2836 11.00000 0.05 0.41 Q15 1 0.1782 0.6321 0.7648 11.00000 0.05 0.40 Q16 1 0.3028 0.4779 0.5755 11.00000 0.05 0.40 Q17 1 0.0574 0.0732 0.3319 11.00000 0.05 0.40 Q18 1 0.3216 0.4949 0.6454 11.00000 0.05 0.39 ; _shelx_res_checksum 86252 _shelx_fab_file ; 0 0 3 10.9256 40.7201 0 0 6 35.9150 28.1740 0 0 9 12.9247 -35.2701 0 0 12 4.5268 -3.1699 0 0 15 3.6019 17.1098 0 1 -16 2.1563 15.5011 0 1 -13 -6.9840 -14.8171 0 1 -10 -0.5954 -24.9438 0 1 -7 -14.8300 42.4690 0 1 -4 -5.2324 17.3724 0 1 -1 -21.9501 -57.0688 0 1 2 -12.6686 6.6355 0 1 5 -27.4709 41.3104 0 1 8 -7.9352 -19.5105 0 1 11 2.8689 -16.1255 0 1 14 -1.3708 13.3300 0 1 17 -7.0496 2.1195 0 2 -17 -10.7504 7.6283 0 2 -14 -6.7914 13.0242 0 2 -11 -0.4175 -25.7532 0 2 -8 15.1525 -12.7912 0 2 -5 16.9187 51.0862 0 2 -2 47.4610 -7.7582 0 2 1 80.3350 -58.5674 0 2 4 1.7063 31.7576 0 2 7 -7.1415 36.2874 0 2 10 -4.0539 -31.7659 0 2 13 6.3123 -10.1332 0 2 16 -3.5600 16.1699 0 3 -15 0.2842 6.5755 0 3 -12 2.6992 -8.2065 0 3 -9 5.7106 -11.3921 0 3 -6 7.6329 20.6946 0 3 -3 -15.1015 8.0304 0 3 0 186.3612 -37.3307 0 3 3 26.1363 5.4407 0 3 6 -6.4953 35.7706 0 3 9 1.9610 -14.8258 0 3 12 7.6866 -16.1253 0 3 15 -1.8476 11.6876 0 4 -16 0.7893 7.3383 0 4 -13 -16.8701 0.5317 0 4 -10 -8.5013 -16.7572 0 4 -7 -2.0091 8.0208 0 4 -4 3.8491 23.4411 0 4 -1 15.9138 -21.6353 0 4 2 20.3999 -18.6596 0 4 5 -6.2910 26.7938 0 4 8 -0.9941 6.8136 0 4 11 -3.9994 -18.4866 0 4 14 5.6526 1.5677 0 4 17 14.1651 5.6954 0 5 -17 16.8414 2.7664 0 5 -14 -4.6341 0.7916 0 5 -11 -0.6591 -3.3473 0 5 -8 -2.9724 2.6535 0 5 -5 15.2864 3.4941 0 5 -2 -22.0600 -8.6455 0 5 1 29.2848 1.0908 0 5 4 -3.7538 10.5830 0 5 7 -6.0342 -6.3532 0 5 10 -17.4576 -5.1236 0 5 13 0.8729 4.9867 0 5 16 2.0398 0.9405 0 6 -15 15.3343 -2.6838 0 6 -12 5.0247 -5.7179 0 6 -9 8.9765 7.0054 0 6 -6 7.0207 5.4762 0 6 -3 -21.6807 -12.0710 0 6 0 38.9557 -1.0208 0 6 3 -11.1477 12.1566 0 6 6 -5.9856 -3.3244 0 6 9 -17.4851 -6.5101 0 6 12 1.3250 4.0586 0 6 15 7.0532 1.9171 0 7 -16 -2.0091 -5.4635 0 7 -13 -13.4432 -6.3737 0 7 -10 1.6914 14.1541 0 7 -7 -5.7207 3.8751 0 7 -4 1.5707 -21.7441 0 7 -1 5.3190 5.8731 0 7 2 41.9834 19.0561 0 7 5 -17.4618 -12.1898 0 7 8 -1.9964 -8.8681 0 7 11 0.8936 9.9036 0 7 14 4.4349 0.8403 0 7 17 14.3966 -4.5179 0 8 -17 -2.7422 -0.3539 0 8 -14 8.1221 -7.6941 0 8 -11 0.1619 9.6439 0 8 -8 -0.9924 9.6222 0 8 -5 -3.3615 -19.7007 0 8 -2 9.9696 -1.8340 0 8 1 -33.3509 21.4508 0 8 4 7.6952 -7.8954 0 8 7 -3.3099 -11.7090 0 8 10 -4.5746 8.6955 0 8 13 -17.5382 2.3660 0 8 16 -2.1733 -2.3292 0 9 -15 13.3732 -6.6805 0 9 -12 -7.6969 0.4222 0 9 -9 -2.8515 14.4995 0 9 -6 12.5959 -9.0938 0 9 -3 -21.9704 -16.2817 0 9 0 2.2382 18.0118 0 9 3 3.0311 8.4801 0 9 6 -1.0978 -17.3214 0 9 9 -5.4146 -0.1522 0 9 12 -11.3344 9.2615 0 9 15 6.1932 -2.1424 0 10 -16 -0.1040 -3.4841 0 10 -13 4.8018 -5.5209 0 10 -10 1.5293 10.0415 0 10 -7 7.5077 4.8624 0 10 -4 -0.0500 -17.1183 0 10 -1 -36.9295 0.7368 0 10 2 27.1067 18.9554 0 10 5 1.4475 -7.4930 0 10 8 6.9766 -11.4495 0 10 11 0.5342 7.9266 0 10 14 3.2933 3.0677 0 10 17 5.4361 -3.9131 0 11 -14 -13.3315 -5.4708 0 11 -11 -8.2227 -3.4162 0 11 -8 1.4341 12.0740 0 11 -5 1.5163 -0.5375 0 11 -2 -5.9980 -16.4220 0 11 1 6.4158 7.7790 0 11 4 -7.0692 12.8460 0 11 7 -6.2360 -10.1979 0 11 10 -4.2368 -4.8756 0 11 13 4.3408 6.9998 0 11 16 -1.3674 -0.1263 0 12 -15 15.6818 0.4627 0 12 -12 -8.4989 -9.1451 0 12 -9 0.7903 3.5015 0 12 -6 6.1129 14.5627 0 12 -3 6.7575 -11.1992 0 12 0 9.5262 -13.1433 0 12 3 -5.4967 16.1297 0 12 6 -3.2907 5.2441 0 12 9 -14.4702 -11.9831 0 12 12 -8.3105 0.3452 0 12 15 1.8643 5.4175 0 13 -16 21.9684 4.4066 0 13 -13 -28.2408 -5.7432 0 13 -10 -4.8618 -9.4072 0 13 -7 -5.9248 16.5237 0 13 -4 0.1945 7.8681 0 13 -1 -2.0518 -25.3224 0 13 2 -12.8887 0.4293 0 13 5 10.6172 22.3281 0 13 8 2.3208 -7.4251 0 13 11 -1.2071 -10.9434 0 13 14 14.6263 6.9138 0 14 -14 11.8635 2.1817 0 14 -11 -5.2807 -14.5854 0 14 -8 -3.8497 4.5983 0 14 -5 1.2045 23.5070 0 14 -2 2.4553 -18.3308 0 14 1 -6.1246 -19.5588 0 14 4 16.5062 24.6770 0 14 7 0.6445 6.4432 0 14 10 -3.9526 -17.1072 0 14 13 -11.7131 0.8232 0 14 16 0.2852 6.1573 0 15 -15 -8.9151 7.8419 0 15 -12 -11.6265 -11.1929 0 15 -9 -13.8215 -10.1327 0 15 -6 0.5554 27.5873 0 15 -3 -9.4966 1.0539 0 15 0 7.6267 -34.0793 0 15 3 4.4313 12.5467 0 15 6 -11.9957 23.4605 0 15 9 2.4927 -16.6654 0 15 12 2.1401 -7.4786 0 15 15 -8.2386 8.4929 0 16 -13 2.5825 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0.5579 25 1 9 -9.0726 7.4848 25 2 -7 -4.5956 -2.9808 25 2 -4 1.4160 1.7504 25 2 -1 0.4190 1.5957 25 2 2 -2.7792 -3.0224 25 2 5 -7.9262 -1.2500 25 2 8 -14.8820 3.3663 25 3 -8 -5.8612 1.1041 25 3 -5 9.1907 -1.9366 25 3 -2 3.2632 2.9886 25 3 1 -1.7858 1.0887 25 3 4 -13.0725 -3.2013 25 3 7 2.8401 0.3677 25 4 -6 3.7565 -1.0373 25 4 -3 7.1241 -2.4387 25 4 0 1.8298 2.0481 25 4 3 -4.2319 1.4562 25 4 6 -11.7499 -2.6794 25 5 -7 3.5383 1.5497 25 5 -4 -4.2483 -2.6417 25 5 -1 15.1159 1.4113 25 5 2 -10.6332 0.9212 25 5 5 -7.1735 -0.8868 25 5 8 3.0889 -1.8666 25 6 -5 -10.3218 -1.6510 25 6 -2 1.8905 -0.3575 25 6 1 9.4467 1.3830 25 6 4 -11.9705 -0.5356 25 6 7 -14.7762 0.5039 25 7 -6 -10.2000 2.2634 25 7 -3 4.7314 -1.4934 25 7 0 -3.8045 -0.0780 25 7 3 -0.1283 -0.6642 25 7 6 -8.9896 1.1879 25 8 -4 -10.4594 -0.1061 25 8 -1 15.1138 -0.8454 25 8 2 -7.3412 1.1069 25 8 5 -3.8771 1.8182 25 9 -2 -16.1824 -0.8051 25 9 1 2.6070 -0.3958 26 1 -8 -9.5289 -2.8426 26 1 -5 -8.7009 -2.5485 26 1 -2 3.7277 5.5867 26 1 1 -1.3713 0.0139 26 1 4 0.0894 -3.9278 26 1 7 20.5744 3.5122 26 2 -6 12.8360 -0.7247 26 2 -3 8.5159 3.2506 26 2 0 -8.3656 0.0580 26 2 3 -5.6197 -3.5157 26 2 6 -4.8039 0.1088 26 3 -7 8.9703 -0.0212 26 3 -4 -2.0745 0.2584 26 3 -1 -3.0850 2.9723 26 3 2 -6.6580 -2.0025 26 3 5 -2.4060 -3.6866 26 3 8 1.9050 0.7913 26 4 -5 -0.1554 -0.6497 26 4 -2 -4.4830 -0.7412 26 4 1 -0.3001 1.4828 26 4 4 -1.5392 -0.7594 26 4 7 6.8566 0.4537 26 5 -6 -14.1936 2.4605 26 5 -3 -0.8977 0.9409 26 5 0 2.6347 0.4162 26 5 3 11.8597 -0.8347 26 5 6 2.3459 3.2700 26 6 -4 -9.9749 -0.3278 26 6 -1 -7.9564 1.3291 26 6 2 -5.6768 0.5638 26 6 5 -5.5442 2.2228 26 7 -2 -16.7722 -2.0720 26 7 1 9.3180 -0.8192 26 7 4 -6.8025 3.3028 26 8 0 6.4643 -0.6236 27 1 -7 -2.5324 -0.0035 27 1 -4 -5.2269 -1.5609 27 1 -1 -3.6650 2.2506 27 1 2 -8.2829 0.7959 27 1 5 3.0888 -2.1446 27 1 8 3.7863 0.7092 27 2 -5 2.5829 0.6070 27 2 -2 -0.0243 2.5636 27 2 1 -5.2639 -0.4977 27 2 4 20.7674 -3.1683 27 2 7 4.8378 -0.0492 27 3 -6 -1.6907 0.9132 27 3 -3 -5.0912 3.1861 27 3 0 8.0573 -1.2259 27 3 3 8.9063 -3.5011 27 3 6 -3.8683 2.1778 27 4 -4 -7.4325 0.5540 27 4 -1 -6.8789 -0.7632 27 4 2 -4.0301 -0.8735 27 4 5 -10.9102 2.2635 27 5 -5 -4.6045 2.5790 27 5 -2 -10.2551 -1.0987 27 5 1 10.5569 -0.9802 27 5 4 3.4543 3.3206 27 6 -3 18.8177 -0.2258 27 6 0 -2.7980 -0.3307 27 6 3 8.7071 2.0615 28 1 -6 10.8423 0.2478 28 1 -3 -11.3345 -5.4953 28 1 0 -2.7075 2.4355 28 1 3 9.2261 2.7355 28 1 6 6.0701 -1.5335 28 2 -4 14.7645 -0.4143 28 2 -1 11.6478 -0.9510 28 2 2 -2.1661 -0.2275 28 2 5 -7.6085 0.1356 28 3 -5 -1.7153 2.0526 28 3 -2 -4.2521 1.9658 28 3 1 -1.2584 -2.3696 28 3 4 10.1850 1.0709 28 4 -3 10.4987 1.7608 28 4 0 7.2413 -1.4894 28 4 3 7.8872 0.3662 28 5 -1 6.5278 -1.4899 28 5 2 -11.2057 -1.0753 29 1 -5 6.3789 -2.2657 29 1 -2 -2.2884 -4.8592 29 1 1 8.0060 3.6795 29 1 4 -0.6131 2.9368 29 2 -3 12.8451 -2.6474 29 2 0 -1.0482 1.0052 29 2 3 12.5790 1.8155 29 3 -1 3.3489 -0.4786 29 3 2 -10.0414 -2.4483 30 1 -1 -18.9890 -1.3915 30 1 2 -0.7442 5.6217 30 2 1 -8.7353 0.9787 0 0 0 0.0 0.0 ; _shelx_fab_checksum 60505 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' 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 Hf1 Hf 0.27470(2) 0.59421(2) 0.76065(3) 0.06200(19) Uani 1 1 d . . . . . O1 O 0.333333 0.666667 0.8061(9) 0.090(3) Uani 1 3 d S TU P . . O2 O 0.2601(3) 0.5167(3) 0.7297(5) 0.1029(17) Uani 1 1 d . U . . . O3 O 0.0367(3) 0.0976(3) 0.2075(6) 0.1054(18) Uani 1 1 d . U . . . O4 O 0.3103(3) 0.5259(3) 0.5989(5) 0.0984(17) Uani 1 1 d . U . . . O5 O 0.2617(3) 0.6531(2) 0.7128(6) 0.102(2) Uani 1 1 d . U . . . O6 O 0.0938(3) 0.0637(3) 0.2095(5) 0.1056(19) Uani 1 1 d . U . . . C1 C 0.0756(6) 0.0922(5) 0.2357(10) 0.112(2) Uani 1 1 d . U . . . C2 C 0.2241(5) 0.4130(5) 0.7224(9) 0.123(2) Uani 1 1 d . U . . . H2 H 0.212714 0.425775 0.767461 0.147 Uiso 1 1 calc R U . . . C3 C 0.2195(6) 0.3376(5) 0.6531(10) 0.118(2) Uani 1 1 d . U . . . C4 C 0.2769(5) 0.5003(5) 0.6635(9) 0.109(2) Uani 1 1 d . U . . . C5 C 0.1610(5) 0.2061(5) 0.5589(9) 0.118(2) Uani 1 1 d . U . . . C6 C 0.1808(5) 0.2584(5) 0.5644(10) 0.120(2) Uani 1 1 d . U . . . H6 H 0.182572 0.276800 0.514037 0.144 Uiso 1 1 calc R U . . . C7 C 0.1529(5) 0.1778(5) 0.6359(10) 0.121(2) Uani 1 1 d . U . . . H7 H 0.136800 0.142369 0.632900 0.145 Uiso 1 1 calc R U . . . C8 C 0.2713(6) 0.4226(5) 0.5917(10) 0.120(2) Uani 1 1 d . U . . . H8 H 0.294204 0.443123 0.548348 0.144 Uiso 1 1 calc R U . . . C9 C 0.1466(6) 0.1379(5) 0.4514(10) 0.121(2) Uani 1 1 d . U . . . H9 H 0.163081 0.127036 0.490231 0.145 Uiso 1 1 calc R U . . . C10 C 0.0996(5) 0.1688(5) 0.3342(9) 0.114(2) Uani 1 1 d . U . . . H10 H 0.082999 0.179653 0.295675 0.137 Uiso 1 1 calc R U . . . C11 C 0.1983(6) 0.2837(5) 0.6455(10) 0.118(2) Uani 1 1 d . U . . . C12 C 0.1685(5) 0.2015(5) 0.7149(10) 0.124(2) Uani 1 1 d . U . . . H12 H 0.164555 0.182511 0.765609 0.149 Uiso 1 1 calc R U . . . C13 C 0.2521(6) 0.3707(5) 0.5878(9) 0.123(2) Uani 1 1 d . U . . . H13 H 0.261112 0.357128 0.540490 0.147 Uiso 1 1 calc R U . . . C14 C 0.1015(5) 0.1252(5) 0.3153(9) 0.110(2) Uani 1 1 d . U . . . C15 C 0.2073(5) 0.3606(5) 0.7188(10) 0.123(2) Uani 1 1 d . U . . . H15 H 0.186372 0.340157 0.764217 0.148 Uiso 1 1 calc R U . . . C16 C 0.1216(5) 0.1958(5) 0.4074(10) 0.116(2) Uani 1 1 d . U . . . H16 H 0.122781 0.226932 0.414172 0.139 Uiso 1 1 calc R U . . . C17 C 0.1902(6) 0.2540(5) 0.7203(10) 0.125(2) Uani 1 1 d . U . . . H17 H 0.199611 0.269695 0.775366 0.150 Uiso 1 1 calc R U . . . C18 C 0.2576(6) 0.4459(5) 0.6589(10) 0.118(2) Uani 1 1 d . U . . . C19 C 0.1267(5) 0.1113(5) 0.3731(9) 0.119(2) Uani 1 1 d . U . . . H19 H 0.130678 0.083442 0.360016 0.143 Uiso 1 1 calc R U . . . C20 C 0.1426(5) 0.1807(5) 0.4734(10) 0.115(2) Uani 1 1 d . 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 Hf1 0.0589(3) 0.0588(3) 0.0662(3) 0.00275(18) 0.00104(18) 0.0278(2) O1 0.081(3) 0.081(3) 0.106(5) 0.000 0.000 0.0407(16) O2 0.123(3) 0.078(3) 0.108(3) -0.011(3) -0.017(3) 0.051(3) O3 0.123(4) 0.087(3) 0.108(4) -0.017(3) -0.032(3) 0.055(3) O4 0.123(4) 0.074(3) 0.097(3) -0.011(3) -0.010(3) 0.050(3) O5 0.126(4) 0.068(3) 0.103(4) -0.003(3) -0.043(4) 0.041(3) O6 0.125(4) 0.083(3) 0.109(4) -0.021(3) -0.027(3) 0.053(3) C1 0.133(4) 0.089(4) 0.114(4) -0.021(3) -0.029(4) 0.055(3) C2 0.145(4) 0.087(3) 0.111(4) -0.013(3) -0.008(3) 0.039(3) C3 0.142(3) 0.087(3) 0.109(3) -0.013(3) -0.013(3) 0.045(3) C4 0.132(4) 0.081(3) 0.108(4) -0.008(3) -0.013(3) 0.048(3) C5 0.141(3) 0.086(3) 0.115(3) -0.016(3) -0.021(3) 0.049(3) C6 0.143(3) 0.088(3) 0.114(3) -0.016(3) -0.018(3) 0.047(3) C7 0.144(4) 0.089(3) 0.115(4) -0.016(3) -0.023(3) 0.047(3) C8 0.142(4) 0.087(3) 0.112(4) -0.014(3) -0.008(3) 0.044(3) C9 0.143(3) 0.093(3) 0.118(3) -0.019(3) -0.029(3) 0.052(3) C10 0.137(4) 0.089(3) 0.116(4) -0.022(3) -0.027(3) 0.056(3) C11 0.143(3) 0.086(3) 0.111(3) -0.014(3) -0.017(3) 0.045(3) C12 0.148(4) 0.090(3) 0.114(4) -0.013(3) -0.021(3) 0.044(3) C13 0.144(3) 0.088(3) 0.112(3) -0.014(3) -0.010(3) 0.039(3) C14 0.132(4) 0.090(3) 0.115(4) -0.020(3) -0.033(3) 0.060(3) C15 0.146(3) 0.088(3) 0.111(3) -0.013(3) -0.011(3) 0.040(3) C16 0.138(3) 0.090(3) 0.116(3) -0.017(3) -0.026(3) 0.054(3) C17 0.148(4) 0.089(3) 0.113(4) -0.013(3) -0.017(3) 0.041(3) C18 0.139(4) 0.085(3) 0.109(4) -0.013(3) -0.009(4) 0.041(3) C19 0.140(4) 0.093(3) 0.118(4) -0.020(3) -0.031(3) 0.054(3) C20 0.139(3) 0.087(3) 0.116(3) -0.018(3) -0.025(3) 0.054(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _geom_angle_publ_flag Hf1 Hf1 Hf1 59.960(11) 15_556 2_665 ? Hf1 Hf1 Hf1 90.0 14_456 2_665 ? Hf1 Hf1 Hf1 60.0 3_565 2_665 ? Hf1 Hf1 Hf1 59.959(11) 14_456 3_565 ? Hf1 Hf1 Hf1 90.0 15_556 3_565 ? Hf1 Hf1 Hf1 60.08(2) 15_556 14_456 ? O1 Hf1 Hf1 89.4(3) . 15_556 ? O1 Hf1 Hf1 89.4(3) . 14_456 ? O1 Hf1 Hf1 34.95(17) . 2_665 ? O1 Hf1 Hf1 34.95(17) . 3_565 ? O1 Hf1 O2 141.5(2) . . ? O1 Hf1 O3 79.7(3) . 8 ? O1 Hf1 O4 143.3(2) . 14_456 ? O1 Hf1 O5 70.0(3) . 2_665 ? O1 Hf1 O5 69.9(3) . . ? O1 Hf1 O6 78.3(3) . 9 ? O2 Hf1 Hf1 110.8(2) . 14_456 ? O2 Hf1 Hf1 110.1(2) . 2_665 ? O2 Hf1 Hf1 74.6(2) . 15_556 ? O2 Hf1 Hf1 164.6(2) . 3_565 ? O2 Hf1 O3 119.6(3) . 8 ? O3 Hf1 Hf1 165.7(2) 8 15_556 ? O3 Hf1 Hf1 112.2(2) 8 2_665 ? O3 Hf1 Hf1 75.8(2) 8 3_565 ? O3 Hf1 Hf1 110.2(2) 8 14_456 ? O4 Hf1 Hf1 77.4(2) 14_456 14_456 ? O4 Hf1 Hf1 112.0(2) 14_456 15_556 ? O4 Hf1 Hf1 112.6(2) 14_456 3_565 ? O4 Hf1 Hf1 167.4(2) 14_456 2_665 ? O4 Hf1 O2 74.7(3) 14_456 . ? O4 Hf1 O3 73.2(3) 14_456 8 ? O5 Hf1 Hf1 35.00(19) . 3_565 ? O5 Hf1 Hf1 89.5(2) 15_556 3_565 ? O5 Hf1 Hf1 34.8(2) . 14_456 ? O5 Hf1 Hf1 89.4(3) . 15_556 ? O5 Hf1 Hf1 89.5(2) 15_556 2_665 ? O5 Hf1 Hf1 34.97(18) 15_556 14_456 ? O5 Hf1 Hf1 89.5(2) . 2_665 ? O5 Hf1 Hf1 35.07(19) 15_556 15_556 ? O5 Hf1 Hf1 89.5(2) 2_665 3_565 ? O5 Hf1 Hf1 89.4(3) 2_665 14_456 ? O5 Hf1 Hf1 34.8(2) 2_665 15_556 ? O5 Hf1 Hf1 35.06(19) 2_665 2_665 ? O5 Hf1 O1 108.2(4) 15_556 . ? O5 Hf1 O2 142.3(3) . . ? O5 Hf1 O2 77.6(3) 2_665 . ? O5 Hf1 O2 78.3(3) 15_556 . ? O5 Hf1 O3 78.2(3) . 8 ? O5 Hf1 O3 141.1(3) 15_556 8 ? O5 Hf1 O3 143.8(3) 2_665 8 ? O5 Hf1 O4 142.5(3) 2_665 14_456 ? O5 Hf1 O4 80.5(3) . 14_456 ? O5 Hf1 O4 80.0(3) 15_556 14_456 ? O5 Hf1 O5 69.9(3) 15_556 2_665 ? O5 Hf1 O5 69.8(3) 15_556 . ? O5 Hf1 O5 108.2(5) 2_665 . ? O5 Hf1 O6 143.2(3) 15_556 9 ? O5 Hf1 O6 79.4(3) 2_665 9 ? O5 Hf1 O6 141.6(3) . 9 ? O6 Hf1 Hf1 75.7(2) 9 2_665 ? O6 Hf1 Hf1 111.8(2) 9 15_556 ? O6 Hf1 Hf1 165.6(2) 9 14_456 ? O6 Hf1 Hf1 110.5(2) 9 3_565 ? O6 Hf1 O2 75.8(3) 9 . ? O6 Hf1 O3 75.3(3) 9 8 ? O6 Hf1 O4 116.9(3) 9 14_456 ? Hf1 O1 Hf1 110.1(3) 3_565 . ? Hf1 O1 Hf1 110.1(3) 3_565 2_665 ? Hf1 O1 Hf1 110.1(3) . 2_665 ? C4 O2 Hf1 130.3(8) . . ? C1 O3 Hf1 126.9(8) . 6_454 ? C4 O4 Hf1 126.7(7) . 15_556 ? Hf1 O5 Hf1 109.9(3) 3_565 . ? Hf1 O5 Hf1 110.2(4) 14_456 3_565 ? Hf1 O5 Hf1 110.1(4) 14_456 . ? C1 O6 Hf1 128.8(8) . 5_554 ? O3 C1 C14 111.8(11) . . ? O6 C1 O3 132.6(12) . . ? O6 C1 C14 115.6(12) . . ? C15 C2 H2 119.9 . . ? C18 C2 H2 119.9 . . ? C18 C2 C15 120.3(14) . . ? C13 C3 C11 120.8(13) . . ? C15 C3 C11 124.0(14) . . ? C15 C3 C13 115.0(13) . . ? O2 C4 O4 130.8(11) . . ? O2 C4 C18 116.7(13) . . ? O4 C4 C18 112.5(12) . . ? C6 C5 C7 119.6(13) . . ? C6 C5 C20 119.1(13) . . ? C7 C5 C20 120.8(12) . . ? C5 C6 H6 119.8 . . ? C5 C6 C11 120.4(13) . . ? C11 C6 H6 119.8 . . ? C5 C7 H7 119.8 . . ? C12 C7 C5 120.4(13) . . ? C12 C7 H7 119.8 . . ? C13 C8 H8 118.7 . . ? C13 C8 C18 122.6(14) . . ? C18 C8 H8 118.7 . . ? C19 C9 H9 119.1 . . ? C19 C9 C20 121.8(14) . . ? C20 C9 H9 119.1 . . ? C14 C10 H10 119.7 . . ? C16 C10 H10 119.7 . . ? C16 C10 C14 120.7(14) . . ? C6 C11 C3 121.7(13) . . ? C17 C11 C3 120.5(13) . . ? C17 C11 C6 117.6(12) . . ? C7 C12 H12 120.0 . . ? C7 C12 C17 120.1(14) . . ? C17 C12 H12 120.0 . . ? C3 C13 H13 119.1 . . ? C8 C13 C3 121.9(14) . . ? C8 C13 H13 119.1 . . ? C10 C14 C1 122.8(12) . . ? C19 C14 C1 119.7(11) . . ? C19 C14 C10 117.4(13) . . ? C2 C15 H15 117.7 . . ? C3 C15 C2 124.5(15) . . ? C3 C15 H15 117.7 . . ? C10 C16 H16 117.7 . . ? C10 C16 C20 124.6(13) . . ? C20 C16 H16 117.7 . . ? C11 C17 H17 119.2 . . ? C12 C17 C11 121.5(13) . . ? C12 C17 H17 119.2 . . ? C2 C18 C4 121.1(13) . . ? C2 C18 C8 115.6(13) . . ? C8 C18 C4 123.4(14) . . ? C9 C19 H19 119.4 . . ? C14 C19 C9 121.2(13) . . ? C14 C19 H19 119.4 . . ? C9 C20 C5 120.7(13) . . ? C16 C20 C5 125.6(12) . . ? C16 C20 C9 113.7(13) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hf1 Hf1 3.4854(10) 15_556 ? Hf1 Hf1 3.4897(10) 2_665 ? Hf1 Hf1 3.4897(9) 3_565 ? Hf1 Hf1 3.4855(10) 14_456 ? Hf1 O1 2.129(4) . ? Hf1 O2 2.208(7) . ? Hf1 O3 2.208(8) 8 ? Hf1 O4 2.190(7) 14_456 ? Hf1 O5 2.120(9) 15_556 ? Hf1 O5 2.133(7) . ? Hf1 O5 2.129(7) 2_665 ? Hf1 O6 2.185(8) 9 ? O2 C4 1.325(15) . ? O3 C1 1.335(14) . ? O4 C4 1.339(15) . ? O6 C1 1.296(14) . ? C1 C14 1.509(17) . ? C2 H2 0.9300 . ? C2 C15 1.401(17) . ? C2 C18 1.390(17) . ? C3 C11 1.428(16) . ? C3 C13 1.402(17) . ? C3 C15 1.365(18) . ? C4 C18 1.445(16) . ? C5 C6 1.385(16) . ? C5 C7 1.392(17) . ? C5 C20 1.464(16) . ? C6 H6 0.9300 . ? C6 C11 1.403(17) . ? C7 H7 0.9300 . ? C7 C12 1.351(17) . ? C8 H8 0.9300 . ? C8 C13 1.376(16) . ? C8 C18 1.413(18) . ? C9 H9 0.9300 . ? C9 C19 1.390(16) . ? C9 C20 1.396(17) . ? C10 H10 0.9300 . ? C10 C14 1.377(15) . ? C10 C16 1.338(16) . ? C11 C17 1.389(17) . ? C12 H12 0.9300 . ? C12 C17 1.383(16) . ? C13 H13 0.9300 . ? C14 C19 1.357(16) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C16 C20 1.380(17) . ? C17 H17 0.9300 . ? C19 H19 0.9300 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Hf1 O2 C4 O4 5.1(19) . . . . ? Hf1 O2 C4 C18 -176.3(9) . . . . ? Hf1 O3 C1 O6 -2(2) 6_454 . . . ? Hf1 O3 C1 C14 179.9(8) 6_454 . . . ? Hf1 O4 C4 O2 -4.8(19) 15_556 . . . ? Hf1 O4 C4 C18 176.6(8) 15_556 . . . ? Hf1 O6 C1 O3 6(3) 5_554 . . . ? Hf1 O6 C1 C14 -175.8(8) 5_554 . . . ? O2 C4 C18 C2 -1(2) . . . . ? O2 C4 C18 C8 179.1(13) . . . . ? O3 C1 C14 C10 -24(2) . . . . ? O3 C1 C14 C19 154.0(13) . . . . ? O4 C4 C18 C2 177.4(13) . . . . ? O4 C4 C18 C8 -2(2) . . . . ? O6 C1 C14 C10 157.5(14) . . . . ? O6 C1 C14 C19 -24(2) . . . . ? C1 C14 C19 C9 -173.7(14) . . . . ? C3 C11 C17 C12 178.3(14) . . . . ? C5 C6 C11 C3 179.3(14) . . . . ? C5 C6 C11 C17 -6(2) . . . . ? C5 C7 C12 C17 3(2) . . . . ? C6 C5 C7 C12 -6(2) . . . . ? C6 C5 C20 C9 147.5(14) . . . . ? C6 C5 C20 C16 -31(2) . . . . ? C6 C11 C17 C12 4(2) . . . . ? C7 C5 C6 C11 7(2) . . . . ? C7 C5 C20 C9 -40(2) . . . . ? C7 C5 C20 C16 141.2(16) . . . . ? C7 C12 C17 C11 -2(2) . . . . ? C10 C14 C19 C9 5(2) . . . . ? C10 C16 C20 C5 -171.7(15) . . . . ? C10 C16 C20 C9 10(2) . . . . ? C11 C3 C13 C8 177.2(14) . . . . ? C11 C3 C15 C2 -173.7(14) . . . . ? C13 C3 C11 C6 -40(2) . . . . ? C13 C3 C11 C17 145.4(16) . . . . ? C13 C3 C15 C2 2(2) . . . . ? C13 C8 C18 C2 1(2) . . . . ? C13 C8 C18 C4 -179.2(14) . . . . ? C14 C10 C16 C20 -7(2) . . . . ? C15 C2 C18 C4 -177.6(13) . . . . ? C15 C2 C18 C8 2(2) . . . . ? C15 C3 C11 C6 134.8(16) . . . . ? C15 C3 C11 C17 -39(2) . . . . ? C15 C3 C13 C8 2(2) . . . . ? C16 C10 C14 C1 177.5(14) . . . . ? C16 C10 C14 C19 -1(2) . . . . ? C18 C2 C15 C3 -4(2) . . . . ? C18 C8 C13 C3 -3(2) . . . . ? C19 C9 C20 C5 175.9(14) . . . . ? C19 C9 C20 C16 -6(2) . . . . ? C20 C5 C6 C11 179.5(14) . . . . ? C20 C5 C7 C12 -177.8(14) . . . . ? C20 C9 C19 C14 -1(2) . . . . ? 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 _smtbx_masks_void_content 1 0.000 0.000 0.500 130.0 20.4 ? 2 -0.177 -0.866 -0.195 5472.5 1234.5 ? 3 0.333 0.667 0.167 130.0 20.4 ? 4 0.667 0.333 0.833 130.0 20.4 ?