#------------------------------------------------------------------------------ #$Date: 2024-06-13 05:30:55 +0300 (Thu, 13 Jun 2024) $ #$Revision: 292346 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/18/1571818.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_1571818 loop_ _publ_author_name 'Carroll, Robert C.' 'Coles, Simon J.' _publ_section_title ; Statistical optimization of guest uptake in crystalline sponges: grading structural outcomes. ; _journal_coeditor_code LT5068 _journal_issue 4 _journal_name_full IUCrJ _journal_paper_doi 10.1107/S2052252524004871 _journal_volume 11 _journal_year 2024 _chemical_formula_moiety 'C15 H16 O3' _chemical_formula_sum 'C15 H16 O3' _chemical_formula_weight 244.28 _chemical_name_systematic (2',6'dimethoxy-[1,1'-biphenyl]-2-yl)methanol _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-I 2ya' _space_group_name_H-M_alt 'I 1 2/a 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary iterative _audit_creation_date 2024-03-18 _audit_creation_method ; Olex2 1.5-alpha (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _cell_angle_alpha 90 _cell_angle_beta 93.244(7) _cell_angle_gamma 90 _cell_formula_units_Z 16 _cell_length_a 23.913(2) _cell_length_b 7.6350(7) _cell_length_c 27.048(2) _cell_measurement_reflns_used 1441 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 63.7260 _cell_measurement_theta_min 3.1970 _cell_volume 4930.4(7) _computing_cell_refinement 'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)' _computing_molecular_graphics 'Olex2 1.5-alpha (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-alpha (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2016/6 (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve 1.5-alpha (Bourhis et al., 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'hybrid pixel array detector' _diffrn_detector_area_resol_mean 10 _diffrn_detector_dtime 0.000 _diffrn_detector_type 'Rigaku, HyPix Arc-100' _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.968 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w 43.00 109.00 0.50 4.50 -- 51.51 30.00 148.00 132 2 \w -17.00 37.00 0.50 4.50 -- 51.51 -30.00 -11.00 108 3 \w -110.00 -85.00 0.50 4.50 -- -55.01 -30.00 -11.00 50 4 \w -33.00 -8.00 0.50 4.50 -- -55.01 30.00 148.00 50 5 \w -135.00-109.00 0.50 11.00 -- -79.37 -30.00 -11.00 52 6 \w 111.00 154.00 0.50 11.00 -- 83.47 30.00 148.00 86 7 \w -17.00 24.00 0.50 4.50 -- 51.51 -19.00 -60.00 82 8 \w -18.00 23.00 0.50 4.50 -- 51.51 -19.00-150.00 82 9 \w -63.00 -13.00 0.50 11.00 -- -79.37 57.00 -30.00 100 10 \w -39.00 -12.00 0.50 11.00 -- -79.37 57.00-120.00 54 11 \w -56.00 -29.00 0.50 11.00 -- -79.37 77.00 90.00 54 12 \w 87.00 112.00 0.50 11.00 -- 83.47-125.00 -30.00 50 13 \w 23.00 49.00 0.50 11.00 -- 83.47-125.00 -30.00 52 14 \w 25.00 60.00 0.50 11.00 -- 83.47 -57.00 30.00 70 15 \w 12.00 37.00 0.50 11.00 -- 83.47 -37.00 -30.00 50 16 \w 13.00 43.00 0.50 11.00 -- 83.47 -37.00 90.00 60 17 \w 12.00 39.00 0.50 11.00 -- 83.47 -37.00 -90.00 54 18 \w 14.00 43.00 0.50 11.00 -- 83.47 -37.00 60.00 58 19 \w 16.00 68.00 0.50 11.00 -- 83.47 -57.00 150.00 104 20 \w 18.00 44.00 0.50 11.00 -- 83.47 -37.00-120.00 52 21 \w 104.00 153.00 0.50 11.00 -- 83.47 37.00-120.00 98 22 \w 84.00 146.00 0.50 11.00 -- 83.47 125.00 150.00 124 23 \w 106.00 131.00 0.50 11.00 -- 83.47 57.00-180.00 50 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_details 'Rigaku, UG2 \k goniometer' _diffrn_measurement_device_type ; Rigaku 007HF diffractometer equipped with Arc)Sec VHF Varimax confocal mirrors and a UG2 goniometer and HyPix Arc-100 detector ; _diffrn_measurement_method 'profile data from \w-scans' _diffrn_measurement_specimen_support 'MiTeGen loops' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0366345000 _diffrn_orient_matrix_UB_12 0.0301835000 _diffrn_orient_matrix_UB_13 0.0442667000 _diffrn_orient_matrix_UB_21 -0.0470307000 _diffrn_orient_matrix_UB_22 0.0737300000 _diffrn_orient_matrix_UB_23 -0.0352679000 _diffrn_orient_matrix_UB_31 -0.0246135000 _diffrn_orient_matrix_UB_32 -0.1855899000 _diffrn_orient_matrix_UB_33 -0.0068613000 _diffrn_radiation_collimation 0.3 _diffrn_radiation_monochromator 'Arc)Sec VHF Varimax focusing mirrors' _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_unetI/netI 0.0774 _diffrn_reflns_Laue_measured_fraction_full 0.983 _diffrn_reflns_Laue_measured_fraction_max 0.968 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 7946 _diffrn_reflns_point_group_measured_fraction_full 0.983 _diffrn_reflns_point_group_measured_fraction_max 0.968 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 69.689 _diffrn_reflns_theta_min 3.273 _diffrn_source 'Rotating anode' _diffrn_source_current 30.0 _diffrn_source_power 1.2 _diffrn_source_target Cu _diffrn_source_type 'Rigaku 007 HF' _diffrn_source_voltage 40.0 _exptl_absorpt_coefficient_mu 0.737 _exptl_absorpt_correction_T_max 0.987 _exptl_absorpt_correction_T_min 0.949 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.316 _exptl_crystal_description needle _exptl_crystal_F_000 2080 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.295 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.076 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 448 _refine_ls_number_reflns 7946 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.060 _refine_ls_R_factor_all 0.1524 _refine_ls_R_factor_gt 0.0797 _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^)+(0.1039P)^2^+7.8365P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2118 _refine_ls_wR_factor_ref 0.2463 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4183 _reflns_number_total 7946 _reflns_threshold_expression 'I > 2\s(I)' _twin_special_details ; Component 2 rotated by 98.3032\% around [-0.00 1.00 0.01] (reciprocal) or [-0.00 1.00 0.00] (direct) ; _cod_data_source_file lt5068.cif _cod_data_source_block BBA_8_12_OMe _cod_original_cell_volume 4930.4(8) _cod_database_code 1571818 _shelx_shelxl_version_number 2016/6 _chemical_oxdiff_formula '(C15 H16 O3)2' _chemical_oxdiff_usercomment '9300-04 Pure' _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 0.985 _shelx_estimated_absorpt_t_min 0.910 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.689(2) 0.311(2) 2. Fixed Uiso At 1.5 times of: All O(H) groups 3.a Idealised tetrahedral OH refined as rotating group: O1A(H1AA), O1B(H1BA) ; _shelx_res_file ; TITL rcc_030823_3a_rc4_twin1_hklf4_a.res in I2/a rcc_030823_3a_rc4_twin1_hklf5.res created by SHELXL-2016/6 at 13:22:21 on 18-Mar-2024 REM Old TITL RCC_030823_3a_RC4_twin1_hklf4 in I2/a REM SHELXT solution in I2/a REM R1 0.213, Rweak 0.047, Alpha 0.046, Orientation as input REM Formula found by SHELXT: C3A O1B CELL 1.54184 23.9128 7.635 27.048 90 93.244 90 ZERR 16 0.0021 0.0007 0.0023 0 0.007 0 LATT 2 SYMM 0.5-X,+Y,-Z SFAC C H O UNIT 240 256 48 L.S. 4 PLAN 5 SIZE 0.02 0.02 0.13 TEMP -173(2) CONF MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.103900 7.836501 BASF 0.31097 FVAR 0.97677 O3B 3 0.330847 0.681714 0.334542 11.00000 0.05362 0.03618 = 0.03700 -0.00121 -0.00962 -0.00522 O2A 3 0.408032 0.279112 0.075339 11.00000 0.05443 0.03420 = 0.03966 0.00205 0.00429 0.00120 O3A 3 0.264973 0.323860 0.185433 11.00000 0.05002 0.03523 = 0.04114 0.00234 0.00555 0.00208 O2B 3 0.427756 0.714084 0.488461 11.00000 0.06070 0.03789 = 0.03837 0.00405 -0.00753 -0.00587 O1A 3 0.452085 0.334068 0.246750 11.00000 0.06044 0.04048 = 0.04664 -0.01031 -0.00916 -0.00444 AFIX 147 H1AA 2 0.458067 0.424433 0.263959 11.00000 -1.50000 AFIX 0 O1B 3 0.469102 0.633933 0.297121 11.00000 0.06677 0.03391 = 0.04648 -0.00940 -0.00073 -0.00411 AFIX 147 H1BA 2 0.496094 0.682441 0.284002 11.00000 -1.50000 AFIX 0 C4A 1 0.357013 0.143880 0.156696 11.00000 0.04032 0.02898 = 0.03943 0.00352 0.00165 -0.00081 C4B 1 0.409452 0.850154 0.395467 11.00000 0.04681 0.02743 = 0.03100 0.00051 -0.00688 -0.00534 C12B 1 0.335258 0.617417 0.382083 11.00000 0.04623 0.02410 = 0.03714 0.00202 0.00247 0.00427 C2A 1 0.367524 -0.172245 0.160746 11.00000 0.04978 0.03411 = 0.04875 -0.00019 -0.00107 0.00366 C12A 1 0.285861 0.383847 0.142386 11.00000 0.04866 0.02439 = 0.03478 -0.00011 -0.00198 -0.00323 C1B 1 0.467971 1.143988 0.365416 11.00000 0.05093 0.03606 = 0.03559 0.00346 -0.00069 -0.00535 C5B 1 0.455786 0.829789 0.366747 11.00000 0.05316 0.02633 = 0.03398 -0.00013 -0.00685 0.00147 C6B 1 0.484961 0.980411 0.352415 11.00000 0.05277 0.02839 = 0.03915 -0.00119 0.00500 -0.00254 C3A 1 0.349286 -0.022649 0.135698 11.00000 0.05048 0.03025 = 0.03901 0.00009 0.00115 -0.00186 C3B 1 0.393394 1.019179 0.408488 11.00000 0.04822 0.03146 = 0.03735 -0.00153 -0.00643 0.00197 C11A 1 0.260830 0.516893 0.113475 11.00000 0.05049 0.02597 = 0.04421 -0.00153 -0.00228 0.00030 C1A 1 0.392779 -0.156685 0.207651 11.00000 0.05410 0.02772 = 0.04940 0.00673 -0.00197 0.00373 C8A 1 0.358965 0.360332 0.085833 11.00000 0.04711 0.03027 = 0.03557 -0.00186 -0.00193 0.00319 C8B 1 0.384772 0.633928 0.460919 11.00000 0.04817 0.02872 = 0.03542 0.00071 -0.00167 -0.00316 C7A 1 0.334260 0.299564 0.128470 11.00000 0.05290 0.02616 = 0.03497 0.00013 -0.00618 -0.00687 C11B 1 0.301719 0.483173 0.399035 11.00000 0.05087 0.02627 = 0.04635 -0.00254 -0.00020 0.00062 C2B 1 0.422011 1.166515 0.393162 11.00000 0.05232 0.03361 = 0.03914 0.00161 -0.00832 -0.00265 C7B 1 0.376650 0.697953 0.412981 11.00000 0.04100 0.02712 = 0.04264 -0.00135 0.00392 0.00494 C9B 1 0.351823 0.500960 0.479010 11.00000 0.05842 0.03519 = 0.03908 0.00277 0.00665 -0.00134 C13A 1 0.395458 0.332359 0.228171 11.00000 0.05570 0.03439 = 0.04787 -0.00752 -0.00948 -0.00136 C10B 1 0.310588 0.428231 0.447575 11.00000 0.05575 0.02733 = 0.04443 0.00210 0.00416 -0.00037 C15B 1 0.290243 0.604609 0.300689 11.00000 0.05308 0.03353 = 0.04119 -0.00173 -0.00173 -0.00508 C5A 1 0.383677 0.158207 0.203696 11.00000 0.04346 0.03215 = 0.04521 -0.00265 0.00231 -0.00035 C6A 1 0.401201 0.003675 0.228945 11.00000 0.05200 0.03648 = 0.04216 0.00593 -0.00407 -0.00008 C13B 1 0.475487 0.653576 0.349984 11.00000 0.05429 0.03169 = 0.04181 -0.00082 0.00319 0.00070 C9A 1 0.334706 0.493177 0.056549 11.00000 0.05408 0.03928 = 0.03417 -0.00359 -0.00003 -0.00322 C14A 1 0.440162 0.354128 0.037360 11.00000 0.05869 0.03569 = 0.04421 0.00285 0.00765 -0.00156 C10A 1 0.285739 0.569209 0.070965 11.00000 0.06242 0.03022 = 0.04062 0.00267 -0.01113 0.00053 C15A 1 0.214862 0.401829 0.201163 11.00000 0.05333 0.03568 = 0.04429 0.00134 0.00487 0.00355 C14B 1 0.443506 0.641228 0.536061 11.00000 0.07343 0.04440 = 0.03711 0.00873 -0.01282 -0.01166 H1B 2 0.487907 1.229337 0.351605 11.00000 0.01872 H13C 2 0.451268 0.562296 0.363075 11.00000 0.05020 H14A 2 0.448295 0.462389 0.043505 11.00000 0.03350 H1A 2 0.403563 -0.262475 0.225146 11.00000 0.05112 H14B 2 0.420954 0.333125 0.003319 11.00000 0.03423 H2B 2 0.409307 1.293860 0.402755 11.00000 0.04759 H11B 2 0.272179 0.427563 0.373873 11.00000 0.04835 H6A 2 0.420575 0.018387 0.262470 11.00000 0.03704 H15A 2 0.208436 0.349341 0.233805 11.00000 0.03771 H3B 2 0.361827 1.032905 0.429371 11.00000 0.05462 H10A 2 0.268003 0.664487 0.049012 11.00000 0.02613 H14C 2 0.476349 0.281135 0.037014 11.00000 0.06046 H6B 2 0.518445 0.964515 0.331199 11.00000 0.02350 H14D 2 0.411011 0.664802 0.560423 11.00000 0.04696 H15D 2 0.299012 0.475901 0.299797 11.00000 0.04256 H14E 2 0.475779 0.709430 0.547427 11.00000 0.04822 H13D 2 0.514983 0.634884 0.362703 11.00000 0.03561 H15E 2 0.251991 0.626721 0.312783 11.00000 0.03510 H10B 2 0.285308 0.348393 0.463238 11.00000 0.03757 H13A 2 0.389011 0.425418 0.205142 11.00000 0.08055 H2A 2 0.362754 -0.286727 0.142971 11.00000 0.04556 H15B 2 0.182473 0.379052 0.176363 11.00000 0.04183 H3A 2 0.327332 -0.026641 0.101168 11.00000 0.04242 H14F 2 0.450537 0.522698 0.534435 11.00000 0.07370 H13B 2 0.371632 0.362971 0.257305 11.00000 0.06624 H9B 2 0.355258 0.464114 0.511266 11.00000 0.05263 H15C 2 0.217955 0.537501 0.206710 11.00000 0.04275 H11A 2 0.227429 0.567859 0.125368 11.00000 0.04555 H15F 2 0.297944 0.650692 0.268449 11.00000 0.05654 H9A 2 0.353930 0.530112 0.025349 11.00000 0.06514 HKLF 5 REM rcc_030823_3a_rc4_twin1_hklf4_a.res in I2/a REM R1 = 0.0797 for 4183 Fo > 4sig(Fo) and 0.1524 for all 7946 data REM 448 parameters refined using 0 restraints END WGHT 0.1038 7.8185 REM Highest difference peak 0.295, deepest hole -0.315, 1-sigma level 0.076 Q1 1 0.4168 0.5003 0.0766 11.00000 0.05 0.30 Q2 1 0.2922 0.1993 0.0741 11.00000 0.05 0.29 Q3 1 0.3711 -0.4601 0.1287 11.00000 0.05 0.27 Q4 1 0.4188 0.4858 0.4884 11.00000 0.05 0.26 Q5 1 0.3887 0.5417 0.4109 11.00000 0.05 0.26 ; _shelx_res_checksum 58989 _shelx_hkl_file ; 0 0 -2 2206.11 21.7215 1 0 0 -4 32848.7 78.2427 1 0 0 6 120.039 74.6869 1 0 0 -8 563.630 67.0423 1 0 0 -10 56.0514 55.4519 1 0 0 12 4984.82 44.9008 1 0 0 14 803.040 50.2186 1 14 0 2 4170.60 118.719 -2 0 0 -16 4170.60 118.719 1 -16 0 -2 4148.82 69.8428 -2 0 0 18 4148.82 69.8428 1 0 0 -20 2185.73 68.3849 1 0 0 22 259.931 65.6595 1 0 0 24 220.072 157.730 1 0 0 26 66.7580 92.6443 1 0 0 28 121.801 65.7534 1 0 0 30 156.916 85.2981 1 0 0 32 255.222 71.2480 1 0 1 1 57.2499 16.5302 1 -1 -1 0 570.135 60.8857 -2 0 -1 1 570.135 60.8857 1 0 1 3 241.217 30.3557 1 0 -1 5 31490.1 91.7796 1 0 1 7 792.458 42.9186 1 8 -1 1 1269.66 43.4231 -2 0 -1 -9 1269.66 43.4231 1 0 -1 11 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-24 -3 7 488.329 45.9811 2 -24 -3 5 172.620 53.3809 2 -24 -3 1 92.9270 38.7755 2 -24 -3 -1-11.2086 73.9951 2 -24 3 -3 60.9887 37.0795 2 -24 -3 -5 16.4685 47.6918 2 -24 3 -7 3.43303 46.1961 2 -24 3 -9 54.2242 43.2180 2 -24 -4 12 89.0314 51.0364 2 -24 -4 8 37.7736 55.9020 2 -24 -4 6 107.062 56.3966 2 -24 -4 2 195.405 44.2553 2 -24 -4 0 11.7393 44.8644 2 -24 -4 -2-19.7774 52.3238 2 -24 -4 -4 50.3831 53.9445 2 -24 -4 -6-33.8508 52.1516 2 24 -4 8 364.298 81.3373 2 24 -4 10 135.300 71.3752 2 -24 -5 7-76.0564 67.1915 2 -24 -5 5 7.19699 71.3268 2 -24 -5 1 21.8513 77.0903 2 25 1 -18 28.9143 68.0417 2 25 -1 -14-39.5657 62.6142 2 25 -1 -12 89.0479 68.2159 2 25 -1 -8-30.2161 72.3570 2 25 -1 -6-43.0973 72.0174 2 25 -1 -2 12.2300 65.8011 2 25 -1 0-0.69665 47.8706 2 25 1 2 29.7538 40.7703 2 -25 -1 -4 257.809 85.3406 2 -25 1 -6 61.7972 57.7771 2 -25 1 -8 41.4159 56.8971 2 -25 1 -12 65.2929 42.0892 2 25 -2 -15 1.08153 68.6922 2 -25 -2 13 32.0859 47.1092 2 -25 -2 11 24.9070 51.5166 2 -25 -2 7 87.9854 54.5124 2 -25 -2 3 155.401 51.9985 2 -25 2 1 4.67792 40.6169 2 -25 2 -3-0.22516 45.6093 2 -25 2 -5 68.4434 45.3002 2 -25 2 -7-90.6760 43.9885 2 -25 2 -9 58.9878 38.7248 2 -25 -3 14 34.2311 65.4487 2 -25 -3 12 66.6699 43.0852 2 -25 -3 8-34.1385 57.0907 2 -25 -3 6 94.7286 57.7591 2 -25 3 2 33.2607 32.3141 2 -25 3 0 87.6263 38.5018 2 -25 3 -2 6.68204 42.6002 2 -25 -3 -4-86.7039 55.8172 2 -25 3 -6 80.4218 41.2469 2 -25 -3 -8 5.16903 52.0758 2 -25 -4 7 87.1729 77.9058 2 -25 -4 3-19.8016 83.9790 2 25 -4 -1 85.2089 56.7264 2 25 -4 1-73.0040 78.4774 2 25 -4 3-53.3677 77.6694 2 25 -4 5 147.846 75.0520 2 25 -4 7-106.410 69.0556 2 26 0 -14 75.8884 82.0923 2 26 0 -12 26.3712 90.5496 2 26 0 -10 28.7808 128.483 2 26 0 -8-31.2411 97.6538 2 26 0 -6-11.6719 97.0753 2 26 0 -2 33.4010 90.4978 2 26 0 0 161.649 85.0879 2 -26 0 -2 162.984 83.6288 2 -26 0 -4 82.3612 79.7698 2 -26 0 -6 21.9905 76.1350 2 -26 0 -8 75.9451 74.2299 2 -26 0 -10 243.590 85.2590 2 -26 0 -12 3.78718 64.0285 2 26 -1 -15 71.2583 51.1864 2 26 -1 -13 11.4186 57.8758 2 26 -1 -9-33.5999 65.5657 2 26 -1 -7 133.945 67.4295 2 26 -1 -3 10.5028 62.3585 2 26 -1 -1 222.107 59.8391 2 -26 1 -1-11.0258 57.3243 2 -26 1 -3 35.3780 44.2900 2 -26 1 -5 14.2353 43.4119 2 -26 1 -7-23.4503 52.1257 2 -26 1 -11 49.0235 46.1927 2 26 -2 -12-8.01176 42.2662 2 -26 -2 8-26.5532 39.4940 2 26 -2 -6 80.9467 48.7833 2 -26 2 2-37.0347 44.0308 2 -26 -2 0-12.3427 63.3759 2 -26 2 -2 28.0352 40.5375 2 -26 -2 -4-83.4118 47.7255 2 -26 2 -6-20.4864 36.3556 2 -26 2 -8 21.0156 34.8420 2 -26 -3 9 141.124 75.8341 2 -26 -3 7 21.7458 80.8947 2 26 -3 -3 44.2527 59.5185 2 -26 3 1 30.7350 40.9478 2 26 -3 1 19.9879 90.1819 2 26 -3 3 241.812 90.2409 2 26 -3 5-3.64179 83.1487 2 26 -3 7 260.741 78.3088 2 -26 -4 2 2.80166 73.7774 2 27 -1 -12 55.0521 52.7463 2 27 -1 -10 21.1282 56.7980 2 27 -1 -8-19.5048 58.5999 2 27 -1 -4 49.1586 57.1604 2 27 1 -2 228.203 43.4205 2 -27 1 -2 98.5514 51.3621 2 -27 1 -4 60.0300 50.0950 2 -27 1 -6 83.4004 47.4814 2 27 -1 8 40.0494 81.3961 2 27 -2 -9 20.2364 73.4469 2 27 -2 -7 69.3876 78.2538 2 -27 2 3 42.0407 44.0212 2 -27 2 -1-3.73503 43.4161 2 -27 -2 -3 77.4601 59.6236 2 -27 2 -5 20.8146 37.7649 2 27 -2 7 45.1515 80.5220 2 27 -3 0 92.9626 75.1368 2 27 -3 2 49.4727 75.4969 2 27 -3 4-84.8665 70.2526 2 28 0 -10 152.628 69.6237 2 28 0 -8 152.484 73.5266 2 28 0 -4 318.597 52.0868 2 -28 0 2-31.6915 92.7583 2 -28 0 0-9.02689 69.1016 2 -28 0 -2 29.3861 67.1409 2 -28 0 -4-58.4802 63.5309 2 -28 0 -6 31.5734 60.5772 2 28 -1 -9-1.08901 68.9457 2 28 -1 -7 49.8338 50.0479 2 28 -1 -5 228.919 34.2436 2 -28 1 3-0.53807 45.8274 2 -28 1 -1 63.7828 44.9110 2 -28 1 -3 46.8351 43.4890 2 -28 1 -5-3.02408 41.4546 2 28 -2 -2-127.929 76.0628 2 28 -2 0-50.4355 80.6917 2 28 -2 2 6.52730 79.2609 2 0 0 0 0.00000 0.00000 0 TITL RCC_030823_3a_RC4_twin1_hklf4 in I2/a REM I2/a (#15 in standard setting) CELL 1.54184 23.912830 7.635001 27.047982 90.0000 93.2438 90.0000 ZERR 8.00 0.002104 0.000744 0.002317 0.0000 0.0069 0.0000 LATT 2 SYMM -x+1/2, y,-z SFAC C H O UNIT 240.00 256.00 48.00 REM CrysAlisPro recorded range (K): Min=100.0; max=100.1; aver:100.0 TEMP -173 SIZE 0.02 0.02 0.13 TREF HKLF 5 BASF 0.30687 END ; _shelx_hkl_checksum 20505 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling - B-factor correction ; _oxdiff_exptl_absorpt_empirical_full_max 1.659 _oxdiff_exptl_absorpt_empirical_full_min 0.739 _oxdiff_twin_integration_method simultaneous _oxdiff_twin_items 2 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' 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 O3B O 0.33085(16) 0.6817(5) 0.33454(13) 0.0427(10) Uani 1 1 d . . . . . O2A O 0.40803(16) 0.2791(5) 0.07534(13) 0.0427(10) Uani 1 1 d . . . . . O3A O 0.26497(16) 0.3239(5) 0.18543(13) 0.0420(10) Uani 1 1 d . . . . . O2B O 0.42776(16) 0.7141(5) 0.48846(13) 0.0460(11) Uani 1 1 d . . . . . O1A O 0.45208(17) 0.3341(6) 0.24675(14) 0.0496(11) Uani 1 1 d . . . . . H1AA H 0.458067 0.424433 0.263959 0.074 Uiso 1 1 calc R U . . . O1B O 0.46910(17) 0.6339(6) 0.29712(14) 0.0492(11) Uani 1 1 d . . . . . H1BA H 0.496094 0.682441 0.284002 0.074 Uiso 1 1 calc R U . . . C4A C 0.3570(2) 0.1439(8) 0.15670(19) 0.0363(13) Uani 1 1 d . . . . . C4B C 0.4095(2) 0.8502(8) 0.39547(18) 0.0354(13) Uani 1 1 d . . . . . C12B C 0.3353(2) 0.6174(7) 0.38208(19) 0.0358(13) Uani 1 1 d . . . . . C2A C 0.3675(2) -0.1722(9) 0.1607(2) 0.0444(15) Uani 1 1 d . . . . . C12A C 0.2859(2) 0.3838(7) 0.14239(19) 0.0361(13) Uani 1 1 d . . . . . C1B C 0.4680(3) 1.1440(9) 0.3654(2) 0.0410(14) Uani 1 1 d . . . . . C5B C 0.4558(2) 0.8298(8) 0.36675(18) 0.0382(14) Uani 1 1 d . . . . . C6B C 0.4850(3) 0.9804(8) 0.3524(2) 0.0400(14) Uani 1 1 d . . . . . C3A C 0.3493(2) -0.0226(8) 0.1357(2) 0.0400(14) Uani 1 1 d . . . . . C3B C 0.3934(3) 1.0192(8) 0.4085(2) 0.0393(14) Uani 1 1 d . . . . . C11A C 0.2608(3) 0.5169(8) 0.1135(2) 0.0404(14) Uani 1 1 d . . . . . C1A C 0.3928(3) -0.1567(9) 0.2077(2) 0.0439(15) Uani 1 1 d . . . . . C8A C 0.3590(2) 0.3603(8) 0.08583(19) 0.0378(13) Uani 1 1 d . . . . . C8B C 0.3848(2) 0.6339(8) 0.46092(19) 0.0376(13) Uani 1 1 d . . . . . C7A C 0.3343(2) 0.2996(7) 0.12847(19) 0.0383(14) Uani 1 1 d . . . . . C11B C 0.3017(3) 0.4832(8) 0.3990(2) 0.0413(14) Uani 1 1 d . . . . . C2B C 0.4220(3) 1.1665(9) 0.3932(2) 0.0421(14) Uani 1 1 d . . . . . C7B C 0.3766(2) 0.6980(7) 0.4130(2) 0.0369(13) Uani 1 1 d . . . . . C9B C 0.3518(3) 0.5010(8) 0.4790(2) 0.0441(15) Uani 1 1 d . . . . . C13A C 0.3955(3) 0.3324(9) 0.2282(3) 0.0465(16) Uani 1 1 d . . . . . C10B C 0.3106(3) 0.4282(8) 0.4476(2) 0.0425(15) Uani 1 1 d . . . . . C15B C 0.2902(3) 0.6046(9) 0.3007(2) 0.0428(15) Uani 1 1 d . . . . . C5A C 0.3837(2) 0.1582(8) 0.2037(2) 0.0403(14) Uani 1 1 d . . . . . C6A C 0.4012(3) 0.0037(9) 0.2289(2) 0.0438(15) Uani 1 1 d . . . . . C13B C 0.4755(3) 0.6536(9) 0.3500(2) 0.0426(14) Uani 1 1 d . . . . . C9A C 0.3347(3) 0.4932(8) 0.0565(2) 0.0426(15) Uani 1 1 d . . . . . C14A C 0.4402(3) 0.3541(10) 0.0374(2) 0.0460(16) Uani 1 1 d . . . . . C10A C 0.2857(3) 0.5692(8) 0.0710(2) 0.0449(15) Uani 1 1 d . . . . . C15A C 0.2149(3) 0.4018(9) 0.2012(2) 0.0444(15) Uani 1 1 d . . . . . C14B C 0.4435(3) 0.6412(11) 0.5361(2) 0.0522(18) Uani 1 1 d . . . . . H1B H 0.4879(19) 1.229(7) 0.3516(16) 0.019(13) Uiso 1 1 d . . . . . H13C H 0.451(2) 0.562(9) 0.363(2) 0.050(18) Uiso 1 1 d . . . . . H14A H 0.448(2) 0.462(8) 0.0435(19) 0.033(16) Uiso 1 1 d . . . . . H1A H 0.404(2) -0.262(9) 0.225(2) 0.051(18) Uiso 1 1 d . . . . . H14B H 0.421(2) 0.333(7) 0.003(2) 0.034(14) Uiso 1 1 d . . . . . H2B H 0.409(2) 1.294(8) 0.4028(19) 0.048(17) Uiso 1 1 d . . . . . H11B H 0.272(2) 0.428(8) 0.374(2) 0.048(17) Uiso 1 1 d . . . . . H6A H 0.421(2) 0.018(7) 0.2625(19) 0.037(15) Uiso 1 1 d . . . . . H15A H 0.208(2) 0.349(8) 0.234(2) 0.038(15) Uiso 1 1 d . . . . . H3B H 0.362(3) 1.033(9) 0.429(2) 0.055(19) Uiso 1 1 d . . . . . H10A H 0.2680(19) 0.664(7) 0.0490(17) 0.026(13) Uiso 1 1 d . . . . . H14C H 0.476(3) 0.281(9) 0.037(2) 0.060(19) Uiso 1 1 d . . . . . H6B H 0.518(2) 0.965(6) 0.3312(16) 0.023(13) Uiso 1 1 d . . . . . H14D H 0.411(2) 0.665(8) 0.560(2) 0.047(16) Uiso 1 1 d . . . . . H15D H 0.299(2) 0.476(9) 0.2998(19) 0.043(16) Uiso 1 1 d . . . . . H14E H 0.476(2) 0.709(8) 0.547(2) 0.048(17) Uiso 1 1 d . . . . . H13D H 0.515(2) 0.635(7) 0.3627(18) 0.036(14) Uiso 1 1 d . . . . . H15E H 0.252(2) 0.627(7) 0.3128(18) 0.035(15) Uiso 1 1 d . . . . . H10B H 0.285(2) 0.348(8) 0.4632(19) 0.038(15) Uiso 1 1 d . . . . . H13A H 0.389(3) 0.425(10) 0.205(3) 0.08(2) Uiso 1 1 d . . . . . H2A H 0.363(2) -0.287(8) 0.143(2) 0.046(16) Uiso 1 1 d . . . . . H15B H 0.182(2) 0.379(7) 0.176(2) 0.042(16) Uiso 1 1 d . . . . . H3A H 0.327(2) -0.027(7) 0.101(2) 0.042(15) Uiso 1 1 d . . . . . H14F H 0.451(3) 0.523(11) 0.534(3) 0.07(3) Uiso 1 1 d . . . . . H13B H 0.372(3) 0.363(9) 0.257(2) 0.07(2) Uiso 1 1 d . . . . . H9B H 0.355(2) 0.464(8) 0.511(2) 0.053(18) Uiso 1 1 d . . . . . H15C H 0.218(2) 0.538(9) 0.2067(19) 0.043(16) Uiso 1 1 d . . . . . H11A H 0.227(2) 0.568(8) 0.125(2) 0.046(17) Uiso 1 1 d . . . . . H15F H 0.298(2) 0.651(9) 0.268(2) 0.057(18) Uiso 1 1 d . . . . . H9A H 0.354(3) 0.530(9) 0.025(2) 0.065(19) Uiso 1 1 d . . . . . 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 O3B 0.054(2) 0.036(3) 0.037(2) -0.0012(18) -0.0096(17) -0.0052(19) O2A 0.054(2) 0.034(3) 0.040(2) 0.0020(18) 0.0043(18) 0.001(2) O3A 0.050(2) 0.035(3) 0.041(2) 0.0023(18) 0.0056(17) 0.002(2) O2B 0.061(3) 0.038(3) 0.038(2) 0.0040(18) -0.0075(19) -0.006(2) O1A 0.060(3) 0.040(3) 0.047(2) -0.010(2) -0.0092(19) -0.004(2) O1B 0.067(3) 0.034(3) 0.046(2) -0.0094(19) -0.0007(19) -0.004(2) C4A 0.040(3) 0.029(3) 0.039(3) 0.004(3) 0.002(2) -0.001(3) C4B 0.047(3) 0.027(3) 0.031(3) 0.001(2) -0.007(2) -0.005(3) C12B 0.046(3) 0.024(3) 0.037(3) 0.002(2) 0.002(2) 0.004(3) C2A 0.050(4) 0.034(4) 0.049(3) 0.000(3) -0.001(3) 0.004(3) C12A 0.049(3) 0.024(3) 0.035(3) 0.000(2) -0.002(2) -0.003(3) C1B 0.051(4) 0.036(4) 0.036(3) 0.003(3) -0.001(3) -0.005(3) C5B 0.053(3) 0.026(3) 0.034(3) 0.000(2) -0.007(3) 0.001(3) C6B 0.053(4) 0.028(4) 0.039(3) -0.001(3) 0.005(3) -0.003(3) C3A 0.050(3) 0.030(4) 0.039(3) 0.000(3) 0.001(3) -0.002(3) C3B 0.048(3) 0.031(4) 0.037(3) -0.002(3) -0.006(3) 0.002(3) C11A 0.050(4) 0.026(4) 0.044(3) -0.002(3) -0.002(3) 0.000(3) C1A 0.054(4) 0.028(4) 0.049(3) 0.007(3) -0.002(3) 0.004(3) C8A 0.047(3) 0.030(4) 0.036(3) -0.002(3) -0.002(2) 0.003(3) C8B 0.048(3) 0.029(4) 0.035(3) 0.001(3) -0.002(2) -0.003(3) C7A 0.053(3) 0.026(4) 0.035(3) 0.000(2) -0.006(2) -0.007(3) C11B 0.051(4) 0.026(3) 0.046(3) -0.003(3) 0.000(3) 0.001(3) C2B 0.052(4) 0.034(4) 0.039(3) 0.002(3) -0.008(3) -0.003(3) C7B 0.041(3) 0.027(3) 0.043(3) -0.001(3) 0.004(2) 0.005(3) C9B 0.058(4) 0.035(4) 0.039(3) 0.003(3) 0.007(3) -0.001(3) C13A 0.056(4) 0.034(4) 0.048(4) -0.008(3) -0.009(3) -0.001(3) C10B 0.056(4) 0.027(4) 0.044(3) 0.002(3) 0.004(3) 0.000(3) C15B 0.053(4) 0.034(4) 0.041(3) -0.002(3) -0.002(3) -0.005(3) C5A 0.043(3) 0.032(4) 0.045(3) -0.003(3) 0.002(3) 0.000(3) C6A 0.052(4) 0.036(4) 0.042(3) 0.006(3) -0.004(3) 0.000(3) C13B 0.054(4) 0.032(4) 0.042(3) -0.001(3) 0.003(3) 0.001(3) C9A 0.054(4) 0.039(4) 0.034(3) -0.004(3) 0.000(3) -0.003(3) C14A 0.059(4) 0.036(4) 0.044(4) 0.003(3) 0.008(3) -0.002(4) C10A 0.062(4) 0.030(4) 0.041(3) 0.003(3) -0.011(3) 0.001(3) C15A 0.053(4) 0.036(4) 0.044(4) 0.001(3) 0.005(3) 0.004(3) C14B 0.073(5) 0.044(5) 0.037(3) 0.009(3) -0.013(3) -0.012(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 1 0.0102 -1 0 -1 0.0102 0 1 -1 0.0517 2 0 -2 0.0138 -2 0 2 0.0078 1 -1 1 0.0632 0 0 1 0.0116 0 0 -1 0.0116 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 C12B O3B C15B 117.9(5) . . ? C8A O2A C14A 117.8(5) . . ? C12A O3A C15A 117.8(5) . . ? C8B O2B C14B 117.6(5) . . ? C13A O1A H1AA 109.5 . . ? C13B O1B H1BA 109.5 . . ? C3A C4A C7A 118.5(5) . . ? C5A C4A C3A 119.0(5) . . ? C5A C4A C7A 122.5(5) . . ? C5B C4B C7B 122.5(5) . . ? C3B C4B C5B 118.7(5) . . ? C3B C4B C7B 118.8(5) . . ? O3B C12B C11B 123.7(5) . . ? O3B C12B C7B 114.5(5) . . ? C11B C12B C7B 121.8(5) . . ? C3A C2A H2A 117(3) . . ? C1A C2A C3A 119.2(6) . . ? C1A C2A H2A 123(3) . . ? O3A C12A C11A 123.6(5) . . ? O3A C12A C7A 115.0(5) . . ? C7A C12A C11A 121.4(5) . . ? C6B C1B C2B 120.9(6) . . ? C6B C1B H1B 112(3) . . ? C2B C1B H1B 126(3) . . ? C4B C5B C6B 118.8(5) . . ? C4B C5B C13B 122.6(5) . . ? C6B C5B C13B 118.6(5) . . ? C1B C6B C5B 121.1(6) . . ? C1B C6B H6B 121(3) . . ? C5B C6B H6B 118(3) . . ? C4A C3A H3A 116(3) . . ? C2A C3A C4A 121.3(5) . . ? C2A C3A H3A 123(3) . . ? C4B C3B H3B 119(4) . . ? C2B C3B C4B 121.6(6) . . ? C2B C3B H3B 120(4) . . ? C12A C11A H11A 116(3) . . ? C10A C11A C12A 119.0(6) . . ? C10A C11A H11A 125(3) . . ? C2A C1A H1A 118(4) . . ? C6A C1A C2A 120.8(6) . . ? C6A C1A H1A 121(4) . . ? O2A C8A C7A 115.2(5) . . ? O2A C8A C9A 123.0(5) . . ? C9A C8A C7A 121.8(5) . . ? O2B C8B C7B 114.1(5) . . ? O2B C8B C9B 123.6(5) . . ? C7B C8B C9B 122.2(5) . . ? C12A C7A C4A 120.8(5) . . ? C12A C7A C8A 117.6(5) . . ? C8A C7A C4A 121.5(5) . . ? C12B C11B H11B 118(3) . . ? C10B C11B C12B 118.3(6) . . ? C10B C11B H11B 124(3) . . ? C1B C2B C3B 118.9(6) . . ? C1B C2B H2B 120(3) . . ? C3B C2B H2B 121(3) . . ? C12B C7B C4B 121.2(5) . . ? C8B C7B C4B 121.4(5) . . ? C8B C7B C12B 117.3(5) . . ? C8B C9B H9B 122(4) . . ? C10B C9B C8B 118.4(6) . . ? C10B C9B H9B 119(4) . . ? O1A C13A C5A 108.4(5) . . ? O1A C13A H13A 110(4) . . ? O1A C13A H13B 107(4) . . ? C5A C13A H13A 111(5) . . ? C5A C13A H13B 116(4) . . ? H13A C13A H13B 105(6) . . ? C11B C10B H10B 123(3) . . ? C9B C10B C11B 121.9(6) . . ? C9B C10B H10B 115(3) . . ? O3B C15B H15D 106(3) . . ? O3B C15B H15E 109(3) . . ? O3B C15B H15F 106(4) . . ? H15D C15B H15E 112(5) . . ? H15D C15B H15F 106(5) . . ? H15E C15B H15F 117(5) . . ? C4A C5A C13A 122.4(5) . . ? C4A C5A C6A 118.8(5) . . ? C6A C5A C13A 118.8(5) . . ? C1A C6A C5A 120.8(6) . . ? C1A C6A H6A 122(3) . . ? C5A C6A H6A 117(3) . . ? O1B C13B C5B 112.1(5) . . ? O1B C13B H13C 105(3) . . ? O1B C13B H13D 112(3) . . ? C5B C13B H13C 109(4) . . ? C5B C13B H13D 109(3) . . ? H13C C13B H13D 110(5) . . ? C8A C9A H9A 119(4) . . ? C10A C9A C8A 118.5(5) . . ? C10A C9A H9A 123(4) . . ? O2A C14A H14A 112(4) . . ? O2A C14A H14B 111(3) . . ? O2A C14A H14C 106(3) . . ? H14A C14A H14B 114(5) . . ? H14A C14A H14C 110(5) . . ? H14B C14A H14C 104(4) . . ? C11A C10A H10A 120(3) . . ? C9A C10A C11A 121.6(6) . . ? C9A C10A H10A 118(3) . . ? O3A C15A H15A 106(3) . . ? O3A C15A H15B 111(3) . . ? O3A C15A H15C 114(3) . . ? H15A C15A H15B 112(4) . . ? H15A C15A H15C 107(4) . . ? H15B C15A H15C 108(4) . . ? O2B C14B H14D 109(3) . . ? O2B C14B H14E 104(3) . . ? O2B C14B H14F 112(4) . . ? H14D C14B H14E 108(5) . . ? H14D C14B H14F 110(6) . . ? H14E C14B H14F 114(6) . . ? 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 O3B C12B 1.375(6) . ? O3B C15B 1.424(7) . ? O2A C8A 1.371(6) . ? O2A C14A 1.436(7) . ? O3A C12A 1.371(6) . ? O3A C15A 1.424(7) . ? O2B C8B 1.378(6) . ? O2B C14B 1.433(7) . ? O1A H1AA 0.8400 . ? O1A C13A 1.417(7) . ? O1B H1BA 0.8400 . ? O1B C13B 1.437(7) . ? C4A C3A 1.401(8) . ? C4A C7A 1.498(8) . ? C4A C5A 1.394(7) . ? C4B C5B 1.397(8) . ? C4B C3B 1.397(8) . ? C4B C7B 1.494(8) . ? C12B C11B 1.395(8) . ? C12B C7B 1.401(7) . ? C2A C3A 1.386(8) . ? C2A C1A 1.379(8) . ? C2A H2A 1.00(6) . ? C12A C11A 1.396(8) . ? C12A C7A 1.394(8) . ? C1B C6B 1.366(8) . ? C1B C2B 1.376(8) . ? C1B H1B 0.90(5) . ? C5B C6B 1.411(8) . ? C5B C13B 1.504(8) . ? C6B H6B 1.02(5) . ? C3A H3A 1.05(5) . ? C3B C2B 1.392(8) . ? C3B H3B 0.97(6) . ? C11A C10A 1.383(8) . ? C11A H11A 0.96(6) . ? C1A C6A 1.363(9) . ? C1A H1A 0.96(6) . ? C8A C7A 1.404(7) . ? C8A C9A 1.393(8) . ? C8B C7B 1.389(7) . ? C8B C9B 1.391(8) . ? C11B C10B 1.383(8) . ? C11B H11B 1.04(6) . ? C2B H2B 1.06(6) . ? C9B C10B 1.382(8) . ? C9B H9B 0.92(6) . ? C13A C5A 1.505(8) . ? C13A H13A 0.95(8) . ? C13A H13B 1.03(7) . ? C10B H10B 0.97(6) . ? C15B H15D 1.01(6) . ? C15B H15E 1.00(5) . ? C15B H15F 0.97(6) . ? C5A C6A 1.415(8) . ? C6A H6A 1.00(5) . ? C13B H13C 0.98(6) . ? C13B H13D 1.00(5) . ? C9A C10A 1.383(8) . ? C9A H9A 1.02(6) . ? C14A H14A 0.86(6) . ? C14A H14B 1.02(5) . ? C14A H14C 1.03(7) . ? C10A H10A 1.02(5) . ? C15A H15A 0.99(5) . ? C15A H15B 1.01(6) . ? C15A H15C 1.05(6) . ? C14B H14D 1.06(6) . ? C14B H14E 0.97(6) . ? C14B H14F 0.92(8) . ? 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 O3B C12B C11B C10B 179.2(5) . . . . ? O3B C12B C7B C4B 4.4(7) . . . . ? O3B C12B C7B C8B -177.4(5) . . . . ? O2A C8A C7A C4A -6.5(8) . . . . ? O2A C8A C7A C12A 176.7(5) . . . . ? O2A C8A C9A C10A -178.6(5) . . . . ? O3A C12A C11A C10A 179.2(5) . . . . ? O3A C12A C7A C4A 5.8(7) . . . . ? O3A C12A C7A C8A -177.3(5) . . . . ? O2B C8B C7B C4B -4.6(8) . . . . ? O2B C8B C7B C12B 177.3(5) . . . . ? O2B C8B C9B C10B -178.8(5) . . . . ? O1A C13A C5A C4A -131.7(6) . . . . ? O1A C13A C5A C6A 47.1(7) . . . . ? C4A C5A C6A C1A 0.7(9) . . . . ? C4B C5B C6B C1B -1.2(8) . . . . ? C4B C5B C13B O1B 114.1(6) . . . . ? C4B C3B C2B C1B -1.4(8) . . . . ? C12B C11B C10B C9B -0.8(9) . . . . ? C2A C1A C6A C5A 0.7(9) . . . . ? C12A C11A C10A C9A -0.1(9) . . . . ? C5B C4B C3B C2B 0.6(8) . . . . ? C5B C4B C7B C12B -81.8(7) . . . . ? C5B C4B C7B C8B 100.1(6) . . . . ? C6B C1B C2B C3B 0.9(8) . . . . ? C6B C5B C13B O1B -65.2(7) . . . . ? C3A C4A C7A C12A 104.7(6) . . . . ? C3A C4A C7A C8A -72.0(7) . . . . ? C3A C4A C5A C13A 177.8(5) . . . . ? C3A C4A C5A C6A -1.0(8) . . . . ? C3A C2A C1A C6A -1.7(9) . . . . ? C3B C4B C5B C6B 0.7(7) . . . . ? C3B C4B C5B C13B -178.7(5) . . . . ? C3B C4B C7B C12B 98.5(6) . . . . ? C3B C4B C7B C8B -79.6(7) . . . . ? C11A C12A C7A C4A -173.1(5) . . . . ? C11A C12A C7A C8A 3.8(8) . . . . ? C1A C2A C3A C4A 1.3(9) . . . . ? C8A C9A C10A C11A 0.2(9) . . . . ? C8B C9B C10B C11B 0.5(9) . . . . ? C7A C4A C3A C2A -177.6(5) . . . . ? C7A C4A C5A C13A -4.6(8) . . . . ? C7A C4A C5A C6A 176.5(5) . . . . ? C7A C12A C11A C10A -2.0(9) . . . . ? C7A C8A C9A C10A 1.7(9) . . . . ? C11B C12B C7B C4B -175.5(5) . . . . ? C11B C12B C7B C8B 2.6(8) . . . . ? C2B C1B C6B C5B 0.4(8) . . . . ? C7B C4B C5B C6B -179.0(5) . . . . ? C7B C4B C5B C13B 1.7(8) . . . . ? C7B C4B C3B C2B -179.7(5) . . . . ? C7B C12B C11B C10B -0.8(9) . . . . ? C7B C8B C9B C10B 1.5(9) . . . . ? C9B C8B C7B C4B 175.1(5) . . . . ? C9B C8B C7B C12B -3.0(8) . . . . ? C13A C5A C6A C1A -178.2(6) . . . . ? C15B O3B C12B C11B -1.0(8) . . . . ? C15B O3B C12B C7B 179.1(5) . . . . ? C5A C4A C3A C2A 0.1(8) . . . . ? C5A C4A C7A C12A -72.9(7) . . . . ? C5A C4A C7A C8A 110.4(6) . . . . ? C13B C5B C6B C1B 178.2(5) . . . . ? C9A C8A C7A C4A 173.2(5) . . . . ? C9A C8A C7A C12A -3.6(8) . . . . ? C14A O2A C8A C7A -169.8(5) . . . . ? C14A O2A C8A C9A 10.5(8) . . . . ? C15A O3A C12A C11A 0.2(8) . . . . ? C15A O3A C12A C7A -178.6(5) . . . . ? C14B O2B C8B C7B -172.3(6) . . . . ? C14B O2B C8B C9B 8.0(9) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined _oxdiff_twin_reflns_isolated _oxdiff_twin_reflns_overlapped _twin_individual_twin_lattice_type _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.689(2) 9498 5424 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 2 0.311(2) 9533 5424 nmt -0.0893 -0.0084 0.8771 0.0007 1.0003 0.0013 -1.1197 0.0069 -0.1980 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0.9657 0.0007 0.9216 0.0054 -0.0779 -0.0302 -0.9657 -0.0007 -0.9216 -0.0054 0.0779 0.0302 -0.0973 1.0017 -1.1144 -0.0155 0.1177 -0.1759 1.6653 0.0031 -1.5151 -0.1280 -0.0247 -0.0312 -1.6653 -0.0031 1.5151 0.1280 0.0247 0.0312 0.9743 -1.0005 0.9165 -0.0253 -0.1519 0.1554 0.0887 -0.0006 1.1194 0.0463 -0.0437 -0.0098 -0.0887 0.0006 -1.1194 -0.0463 0.0437 0.0098