#------------------------------------------------------------------------------ #$Date: 2021-05-14 01:11:12 +0300 (Fri, 14 May 2021) $ #$Revision: 265191 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/87/4518722.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_4518722 loop_ _publ_author_name 'Sobczak, Szymon' 'Ratajczyk, Paulina' 'Katrusiak, Andrzej' _publ_section_title ; Squeezing Out the Catalysts: A Sustainable Approach to Disulfide Bond Exchange in Aryl Disulfides ; _journal_name_full 'ACS Sustainable Chemistry & Engineering' _journal_paper_doi 10.1021/acssuschemeng.1c02240 _journal_year 2021 _chemical_formula_moiety 'C14 H14 O2 S2' _chemical_formula_sum 'C14 H14 O2 S2' _chemical_formula_weight 278.37 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens difmap _audit_creation_date 2020-09-22 _audit_creation_method ; Olex2 1.3 (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _audit_update_record ; 2020-09-23 deposited with the CCDC. 2020-09-24 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.9037(2) _cell_length_b 12.9800(4) _cell_length_c 17.9041(6) _cell_measurement_reflns_used 7558 _cell_measurement_temperature 299.4(3) _cell_measurement_theta_max 75.8310 _cell_measurement_theta_min 2.4530 _cell_volume 1371.99(8) _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/1 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 299.4(3) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.5357 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.778 _diffrn_measured_fraction_theta_max 0.751 _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 6.00 34.00 1.00 6.50 -- 40.00 85.00 114.25 28 2 \w -97.00 -2.00 1.00 6.50 -- -41.91 125.00 0.00 95 3 \w 18.00 87.00 1.00 6.50 -- 41.91 37.00 -60.00 69 4 \w -37.00 24.00 1.00 6.50 -- 41.91 -19.00 90.00 61 5 \w 79.00 105.00 1.00 6.50 -- 41.91 37.00-180.00 26 6 \w 36.00 64.00 1.00 6.50 -- 41.91 37.00-180.00 28 7 \w 20.00 79.00 1.00 6.50 -- 41.91 37.00 60.00 59 8 \w -8.00 81.00 1.00 6.50 -- 41.91 -99.00-150.00 89 9 \w -32.00 40.00 1.00 6.50 -- 41.91 -37.00-120.00 72 10 \w 15.00 40.00 1.00 6.50 -- 48.00 80.00 18.99 25 11 \w 14.00 40.00 1.00 6.50 -- 48.00 83.00-110.02 26 12 \w 18.00 43.00 1.00 6.50 -- 52.00 81.00 81.65 25 13 \w 19.00 44.00 1.00 6.50 -- 52.00 80.00 -47.73 25 14 \w 18.00 43.00 1.00 6.50 -- 52.00 82.00 171.23 25 15 \w 28.00 54.00 1.00 6.50 -- 60.00 75.00-162.18 26 16 \w 32.00 57.00 1.00 6.50 -- 64.00 77.00 16.29 25 17 \w 105.00 143.00 1.00 6.50 -- 68.00 75.00 103.51 38 18 \w 37.00 65.00 1.00 6.50 -- 68.00 76.00 -47.28 28 19 \w 37.00 76.00 1.00 6.50 -- 68.00 75.00 103.51 39 20 \w 36.00 62.00 1.00 6.50 -- 68.00 76.00 -21.41 26 21 \w 40.00 75.00 1.00 6.50 -- 72.00 76.00-110.88 35 22 \w 44.00 72.00 1.00 6.50 -- 76.00 76.00-153.49 28 23 \w 44.00 105.00 1.00 6.50 -- 76.00 76.00 33.95 61 24 \w 120.00 148.00 1.00 6.50 -- 76.00 47.00 154.70 28 25 \w 52.00 87.00 1.00 6.50 -- 76.00 47.00 154.70 35 26 \w 83.00 111.00 1.00 12.00 -- 111.24 61.00 90.00 28 27 \w 82.00 108.00 1.00 12.00 -- 111.24 61.00-150.00 26 28 \w 85.00 113.00 1.00 12.00 -- 111.24 61.00 30.00 28 29 \w 125.00 157.00 1.00 12.00 -- 111.24 111.00 60.00 32 30 \w 37.00 111.00 1.00 12.00 -- 111.24-111.00 -60.00 74 31 \w 36.00 113.00 1.00 12.00 -- 111.24-111.00 90.00 77 32 \w 39.00 71.00 1.00 12.00 -- 111.24 -61.00-150.00 32 33 \w 80.00 158.00 1.00 12.00 -- 111.24 77.00 -30.00 78 34 \w 36.00 110.00 1.00 12.00 -- 111.24-111.00 30.00 74 35 \w 36.00 108.00 1.00 12.00 -- 111.24 -94.00 120.00 72 36 \w 79.00 146.00 1.00 12.00 -- 111.24 77.00-120.00 67 37 \w 115.00 158.00 1.00 12.00 -- 111.24 77.00-150.00 43 38 \w 79.00 104.00 1.00 12.00 -- 111.24 77.00-150.00 25 39 \w 29.00 80.00 1.00 12.00 -- 111.24 -94.00-180.00 51 40 \w 30.00 86.00 1.00 12.00 -- 111.24 -94.00 -30.00 56 41 \w 133.00 158.00 1.00 12.00 -- 111.24 77.00 -90.00 25 42 \w 40.00 107.00 1.00 12.00 -- 111.24-111.00-120.00 67 43 \w 133.00 158.00 1.00 12.00 -- 111.24 61.00 120.00 25 44 \w 80.00 107.00 1.00 12.00 -- 111.24 77.00 -90.00 27 45 \w 86.00 115.00 1.00 12.00 -- 111.24 61.00 120.00 29 46 \w 83.00 115.00 1.00 12.00 -- 111.24 61.00 -60.00 32 47 \w 39.00 71.00 1.00 12.00 -- 111.24 -61.00 0.00 32 48 \w 79.00 156.00 1.00 12.00 -- 111.24 77.00 30.00 77 49 \w 85.00 112.00 1.00 12.00 -- 111.24 61.00 150.00 27 50 \w 83.00 158.00 1.00 12.00 -- 111.24 77.00 150.00 75 51 \w 79.00 157.00 1.00 12.00 -- 111.24 77.00 120.00 78 52 \w 83.00 136.00 1.00 12.00 -- 111.24 61.00 -30.00 53 53 \w 83.00 108.00 1.00 12.00 -- 111.24 61.00 0.00 25 54 \w 39.00 64.00 1.00 12.00 -- 111.24 -61.00 60.00 25 55 \w 82.00 157.00 1.00 12.00 -- 111.24 64.00-170.00 75 56 \w 85.00 110.00 1.00 12.00 -- 111.24 61.00-120.00 25 57 \w 118.00 157.00 1.00 12.00 -- 111.24 61.00 -90.00 39 58 \w 83.00 110.00 1.00 12.00 -- 111.24 61.00 -90.00 27 59 \w 117.00 144.00 1.00 12.00 -- 111.24 77.00 -60.00 27 60 \w 39.00 64.00 1.00 12.00 -- 111.24 -61.00 120.00 25 61 \w 115.00 157.00 1.00 12.00 -- 111.24 77.00 0.00 42 62 \w 80.00 114.00 1.00 12.00 -- 111.24 77.00 -60.00 34 63 \w 80.00 109.00 1.00 12.00 -- 111.24 77.00 0.00 29 64 \w 85.00 152.00 1.00 12.00 -- 111.24 61.00 60.00 67 65 \w 116.00 156.00 1.00 12.00 -- 111.24 61.00 90.00 40 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0954978000 _diffrn_orient_matrix_UB_12 -0.0330331000 _diffrn_orient_matrix_UB_13 0.0764003000 _diffrn_orient_matrix_UB_21 -0.0222524000 _diffrn_orient_matrix_UB_22 0.1116239000 _diffrn_orient_matrix_UB_23 0.0283621000 _diffrn_orient_matrix_UB_31 -0.2417265000 _diffrn_orient_matrix_UB_32 -0.0233115000 _diffrn_orient_matrix_UB_33 0.0276297000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_unetI/netI 0.0205 _diffrn_reflns_Laue_measured_fraction_full 0.778 _diffrn_reflns_Laue_measured_fraction_max 0.751 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 6081 _diffrn_reflns_point_group_measured_fraction_full 0.776 _diffrn_reflns_point_group_measured_fraction_max 0.749 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 69.579 _diffrn_reflns_theta_min 4.207 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 3.445 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.735 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'dull colourless' _exptl_crystal_colour_lustre dull _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.348 _exptl_crystal_description block _exptl_crystal_F_000 584 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.111 _exptl_crystal_size_min 0.043 _refine_diff_density_max 0.114 _refine_diff_density_min -0.183 _refine_diff_density_rms 0.032 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.30(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 219 _refine_ls_number_reflns 1807 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.037 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0281 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+0.0506P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.0757 _reflns_Friedel_coverage 0.693 _reflns_Friedel_fraction_full 0.774 _reflns_Friedel_fraction_max 0.745 _reflns_number_gt 1752 _reflns_number_total 1807 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file sc1c02240_si_001.cif _cod_data_source_block h3co_phssph_och3 _cod_database_code 4518722 _shelx_shelxl_version_number 2018/1 _chemical_oxdiff_formula S2C14O2H14 _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 0.866 _shelx_estimated_absorpt_t_min 0.480 _reflns_odcompleteness_completeness 75.11 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 69.95 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.70(3) 0.30(3) 2. Fixed Uiso At 1.2 times of: All C(H) groups ; _shelx_res_file ; TITL Metoxy_disulp in P212121 #19 h3co_phssph_och3.res created by SHELXL-2018/1 at 14:44:18 on 22-Sep-2020 REM Best SHELXD solution FINAL CC 83.48 REM Fragments: 21 REM reset to P212121 #19 CELL 1.54184 5.9037 12.98 17.9041 90 90 90 ZERR 4 0.0002 0.0004 0.0006 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,-Z SYMM -X,0.5+Y,0.5-Z SFAC C H O S UNIT 56 56 8 8 L.S. 44 PLAN 2 SIZE 0.043 0.111 0.25 TEMP 26.3(3) CONF MORE -1 BOND $H fmap 2 53 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT -1 12 1 OMIT -4 10 11 OMIT 5 1 1 OMIT -5 8 5 OMIT -3 10 14 OMIT 5 1 2 OMIT 3 0 7 REM REM REM WGHT 0.052500 0.050600 BASF 0.30476 FVAR 0.82629 S2 4 0.480367 0.022488 0.016761 11.00000 0.06026 0.06711 = 0.06577 -0.00244 -0.00342 0.00128 S1 4 0.155543 -0.028370 0.021820 11.00000 0.06467 0.07261 = 0.06363 -0.00284 0.01368 -0.00415 C8 1 0.136880 -0.125406 -0.048493 11.00000 0.05319 0.05880 = 0.05400 0.00927 0.00716 -0.00264 O2 3 0.030810 -0.358507 -0.202347 11.00000 0.07617 0.08704 = 0.07679 -0.01478 -0.01233 0.00679 C1 1 0.479522 0.120030 -0.053584 11.00000 0.04789 0.05811 = 0.05760 -0.01316 0.00333 0.00316 C11 1 0.075368 -0.283463 -0.150492 11.00000 0.05857 0.06796 = 0.05359 0.00628 0.00266 -0.00157 C4 1 0.510896 0.273724 -0.160412 11.00000 0.06653 0.06442 = 0.05960 -0.00358 0.00710 -0.00274 O1 3 0.507146 0.346896 -0.216132 11.00000 0.08956 0.08963 = 0.07526 0.01449 0.00118 -0.01435 C9 1 0.303391 -0.198627 -0.059177 11.00000 0.04968 0.05934 = 0.07112 0.01010 -0.00483 -0.00080 C10 1 0.274405 -0.276572 -0.110652 11.00000 0.05728 0.05404 = 0.07314 0.00619 0.00047 0.00775 C6 1 0.667195 0.182717 -0.056834 11.00000 0.05043 0.06652 = 0.07341 -0.00906 -0.00975 -0.00396 C5 1 0.683187 0.259445 -0.110439 11.00000 0.05483 0.06425 = 0.08076 -0.00769 0.00102 -0.01087 C2 1 0.307675 0.134807 -0.104275 11.00000 0.05420 0.08140 = 0.06705 0.00041 -0.00134 -0.01457 C13 1 -0.061038 -0.132109 -0.089656 11.00000 0.05047 0.07289 = 0.06365 0.00307 0.00879 0.01043 C3 1 0.319613 0.211541 -0.156753 11.00000 0.05425 0.09999 = 0.06498 0.00604 -0.00653 -0.01413 C14 1 0.200811 -0.430537 -0.218704 11.00000 0.09396 0.07676 = 0.08776 -0.01702 0.00700 -0.00059 C12 1 -0.093249 -0.210339 -0.139599 11.00000 0.04583 0.09360 = 0.05797 0.00088 -0.00334 0.00725 H12 2 -0.219642 -0.218732 -0.164949 11.00000 -1.20000 C7 1 0.699833 0.410216 -0.224666 11.00000 0.09982 0.07738 = 0.07803 0.00272 0.01874 -0.01232 H2 2 0.177432 0.095838 -0.102157 11.00000 0.06141 H7A 2 0.839816 0.372647 -0.230201 11.00000 0.09030 H6 2 0.800420 0.173266 -0.021675 11.00000 0.08695 H7B 2 0.670352 0.444231 -0.267371 11.00000 0.08975 H14A 2 0.235270 -0.474949 -0.176167 11.00000 0.11424 H14B 2 0.363044 -0.399021 -0.230731 11.00000 0.09228 H3 2 0.206817 0.222010 -0.188012 11.00000 0.08653 H7C 2 0.697793 0.456880 -0.182375 11.00000 0.10728 H9 2 0.438293 -0.195287 -0.034168 11.00000 0.06476 H5 2 0.817533 0.293355 -0.112897 11.00000 0.08164 H10 2 0.382320 -0.319133 -0.119574 11.00000 0.06296 H14C 2 0.150058 -0.465984 -0.257586 11.00000 0.10601 H13 2 -0.182060 -0.083155 -0.085582 11.00000 0.06473 HKLF 4 REM Metoxy_disulp in P212121 #19 REM R1 = 0.0281 for 1752 Fo > 4sig(Fo) and 0.0292 for all 1807 data REM 219 parameters refined using 0 restraints END WGHT 0.0524 0.0517 REM Highest difference peak 0.114, deepest hole -0.183, 1-sigma level 0.032 Q1 1 0.4839 0.0390 -0.0326 11.00000 0.05 0.11 Q2 1 0.6133 -0.3761 -0.1600 11.00000 0.05 0.11 ; _shelx_res_checksum 81907 _shelx_hkl_file ; 0 0 1 0.04 0.04 0 0 -1 1.02 0.13 0 0 2 3551.65 12.10 0 0 -2 3524.32 10.39 0 0 3 0.30 0.17 0 0 -3 0.08 0.09 0 0 -4 1476.37 9.51 0 0 -5 0.15 0.16 0 0 -5 0.05 0.21 0 0 -6 566.64 6.74 0 0 -6 544.25 7.23 0 0 7 -0.10 0.26 0 0 -7 0.08 0.12 0 0 -7 0.35 0.25 0 0 -8 218.42 4.97 0 0 -8 209.54 5.31 0 0 8 221.43 6.00 0 0 -9 -0.10 0.30 0 0 -9 -0.11 0.17 0 0 9 0.20 0.25 0 0 -10 48.17 2.90 0 0 10 53.13 3.41 0 0 11 0.15 0.42 0 0 -11 0.01 0.28 0 0 12 151.83 6.36 0 0 -12 147.27 5.86 0 0 -13 0.13 0.28 0 0 13 0.85 0.70 0 0 -13 -0.29 0.43 0 0 14 20.42 2.60 0 0 -14 20.76 2.15 0 0 -14 20.33 2.43 0 0 -15 1.17 0.73 0 0 -15 0.77 0.29 0 0 -16 266.40 7.78 0 0 -17 3.86 1.12 0 0 -18 7.25 1.23 0 0 -19 0.44 0.37 0 -1 0 0.07 0.06 0 1 -1 52.23 1.25 0 -1 1 52.61 1.13 0 1 -2 25.26 0.97 0 -1 -2 21.52 0.84 0 1 -3 35.20 1.19 0 -1 -3 32.42 1.23 0 1 -3 32.71 1.27 0 1 -4 2446.19 11.25 0 -1 4 2438.92 14.27 0 -1 -5 83.96 2.53 0 -1 5 94.37 3.18 0 1 -5 94.36 2.54 0 1 -5 85.87 2.75 0 1 -5 90.65 2.46 0 1 -6 4013.13 20.00 0 1 -6 4053.12 18.16 0 -1 6 4208.41 23.72 0 -1 6 3958.90 18.71 0 -1 -6 3929.67 19.28 0 1 -6 4155.41 18.36 0 1 -7 12.90 1.25 0 1 7 14.39 1.43 0 -1 7 13.20 1.17 0 -1 -7 12.72 1.21 0 1 -7 14.35 1.17 0 1 8 405.95 8.12 0 -1 8 416.53 8.27 0 1 -8 397.55 7.64 0 -1 -8 396.04 7.29 0 1 -8 411.15 6.80 0 -1 -9 12.19 1.41 0 -1 9 8.73 1.31 0 1 -9 8.92 1.22 0 1 9 9.58 1.34 0 -1 -9 8.70 1.17 0 -1 -10 3016.47 23.59 0 -1 -10 3385.75 23.48 0 -1 10 3051.18 25.94 0 1 -10 3111.66 21.90 0 1 -10 3343.58 26.75 0 1 10 3053.14 25.55 0 1 -10 2935.08 23.55 0 1 -11 5.53 1.10 0 -1 -11 4.12 0.80 0 -1 -11 4.24 0.97 0 1 11 4.87 1.11 0 -1 -11 4.82 0.91 0 1 -11 6.90 1.37 0 -1 11 4.38 1.11 0 1 -12 896.16 14.52 0 -1 -12 951.56 13.42 0 1 12 939.80 16.01 0 -1 -12 943.83 15.10 0 1 -13 26.23 2.60 0 1 -13 19.64 2.27 0 -1 13 21.90 2.60 0 -1 -13 21.13 2.09 0 -1 -13 23.22 2.50 0 1 -14 791.72 15.24 0 1 -14 809.21 13.37 0 -1 -14 772.68 15.22 0 -1 14 794.48 16.24 0 -1 -14 769.43 12.87 0 -1 -15 60.30 4.38 0 -1 15 64.05 4.71 0 -1 -15 61.74 3.78 0 1 -15 65.63 3.89 0 1 -15 61.46 4.39 0 -1 -16 461.43 10.30 0 1 -16 473.19 10.33 0 -1 -17 37.83 2.99 0 1 -17 40.15 2.95 0 1 -18 134.33 5.11 0 -1 -18 129.56 5.22 0 -1 -19 14.76 1.64 0 2 0 832.38 5.72 0 -2 0 797.48 5.79 0 -2 -1 27.48 0.63 0 2 -1 26.79 1.16 0 2 -2 4271.91 15.23 0 -2 2 4540.59 14.57 0 -2 -3 141.77 1.60 0 -2 -3 141.56 2.65 0 -2 -3 131.03 2.75 0 -2 3 139.30 2.82 0 2 -3 134.41 2.91 0 2 -5 178.44 3.96 0 -2 -5 172.96 3.80 0 2 -5 185.48 3.86 0 -2 5 177.62 4.41 0 2 -5 180.06 3.55 0 -2 5 177.35 3.93 0 -2 -5 180.26 3.53 0 -2 6 835.49 9.16 0 2 -6 867.03 8.99 0 -2 6 867.13 10.77 0 -2 -6 858.01 8.33 0 2 -6 856.88 8.85 0 -2 -6 834.84 9.07 0 2 -6 838.28 8.32 0 2 -7 98.59 3.13 0 2 -7 88.98 3.09 0 -2 -7 94.01 3.14 0 2 -7 93.61 3.06 0 2 7 91.17 3.56 0 -2 -7 103.30 3.49 0 -2 7 89.64 3.21 0 -2 7 91.19 3.86 0 2 -7 93.81 3.53 0 -2 -7 85.36 2.86 0 -2 8 601.22 10.78 0 -2 -8 546.07 7.80 0 -2 8 569.12 8.68 0 -2 -8 562.29 8.83 0 2 -8 589.17 8.22 0 -2 -8 579.26 8.27 0 2 8 592.82 9.83 0 2 -8 562.17 9.26 0 2 9 3.66 0.87 0 2 -9 2.97 0.65 0 2 -9 3.14 0.77 0 -2 9 3.62 0.88 0 -2 -9 3.27 0.65 0 -2 -9 4.26 0.79 0 -2 -9 2.75 0.70 0 2 -10 788.29 10.98 0 -2 10 770.79 13.18 0 -2 -10 749.76 11.80 0 -2 -10 742.45 10.37 0 -2 -10 774.02 11.01 0 2 -11 48.60 3.27 0 -2 -11 48.74 3.26 0 -2 11 51.27 3.62 0 -2 -11 53.28 2.87 0 -2 -11 51.62 2.98 0 2 -11 57.00 3.15 0 2 -12 14.29 1.89 0 -2 -12 15.49 1.94 0 -2 -12 14.61 1.67 0 -2 12 14.39 2.00 0 -2 -13 2.61 0.83 0 -2 -13 2.11 0.77 0 -2 13 2.12 0.87 0 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43.60 4.16 4 5 -6 42.85 3.40 4 -5 5 253.85 9.13 4 -5 5 260.11 10.27 4 5 -5 239.87 8.02 4 -5 4 116.30 6.11 4 5 -4 104.58 5.33 4 5 -4 103.03 5.85 -4 -5 -3 131.94 3.94 4 -5 3 158.58 7.32 4 -5 3 154.11 7.70 -4 -5 -3 111.01 5.32 4 5 -3 138.59 6.91 4 5 -3 91.18 5.39 4 -5 2 32.61 3.38 4 -5 2 24.12 3.02 -4 -5 -2 18.29 2.15 4 5 -2 26.42 3.04 4 5 -1 113.68 6.44 4 -5 1 128.81 5.70 -4 -5 0 3.38 1.00 4 -5 0 6.80 1.54 4 -5 0 7.22 1.66 4 5 0 5.40 1.51 4 -5 0 7.26 1.39 4 -5 -1 134.20 6.87 -4 -5 1 108.09 5.05 4 -5 -1 99.29 7.23 4 5 1 137.72 6.91 4 5 1 121.05 6.89 4 -5 -1 128.74 5.88 -4 -5 2 19.45 2.14 4 5 2 27.38 3.21 4 5 2 23.91 3.12 4 -5 -2 24.66 2.65 -4 -5 3 142.61 6.43 4 5 3 149.81 7.63 4 5 3 147.33 7.79 4 -5 -3 145.97 6.52 -4 -5 4 97.90 3.16 4 5 4 116.76 6.92 4 5 4 112.53 6.89 4 -5 -4 115.77 5.91 4 5 5 244.47 10.15 4 5 5 243.89 10.29 4 -5 -5 265.87 9.21 4 5 6 45.56 4.43 4 5 6 42.42 4.32 4 5 6 46.64 4.45 4 -5 -6 51.80 4.18 4 5 7 279.38 11.18 4 5 7 286.58 10.88 4 -5 -7 289.80 10.15 4 -5 -8 49.70 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46.94 4.23 4 -6 -1 49.84 3.79 -4 -6 2 4.28 1.10 4 -6 -2 4.14 1.10 4 -6 -2 2.80 1.04 4 -6 -2 1.23 0.77 -4 6 -2 2.38 1.23 4 6 2 5.10 1.45 4 6 2 3.55 1.28 4 6 3 153.21 7.51 4 6 3 141.60 7.57 4 -6 -3 154.58 6.93 -4 -6 4 92.30 3.18 4 6 4 104.84 6.36 4 6 4 100.44 6.49 4 -6 -4 99.30 5.67 4 6 5 130.95 7.23 4 6 5 133.73 7.52 4 -6 -5 143.66 6.93 4 6 6 104.20 6.64 4 6 6 104.28 6.68 4 -6 -6 109.27 6.07 4 6 7 323.95 11.77 4 -6 -7 349.57 10.97 4 6 8 33.32 3.77 4 -6 -8 41.72 3.87 4 6 9 78.17 5.73 4 -6 -9 86.41 5.50 4 6 10 8.88 1.90 4 -6 -10 10.70 1.93 4 6 11 12.80 2.16 4 -6 -11 16.05 2.34 4 7 -10 4.29 0.97 4 7 -9 152.85 5.97 4 7 -9 157.97 6.04 4 7 -8 9.80 1.51 4 7 -8 12.61 1.81 4 7 -7 89.18 4.90 4 7 -6 44.43 3.64 4 7 -6 45.06 3.67 4 -7 5 110.66 6.26 4 7 -5 110.71 5.80 4 -7 4 0.84 0.52 4 -7 4 2.13 0.80 4 7 -4 0.34 0.50 4 -7 3 133.59 7.03 4 7 -3 118.82 6.02 -4 -7 -2 8.34 1.08 4 -7 2 8.68 1.77 4 -7 2 7.31 1.69 4 7 -2 8.11 1.56 4 7 -2 9.14 1.74 -4 -7 -1 98.72 3.76 -4 -7 -1 87.06 3.42 4 -7 1 110.41 7.01 4 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8.92 1.68 5 5 -2 9.54 1.81 -5 -5 -1 25.92 1.87 5 -5 1 25.70 3.03 5 -5 1 27.99 3.68 5 5 -1 24.57 3.10 5 -5 0 2.02 0.95 5 -5 0 0.37 0.56 5 5 0 1.30 0.61 5 -5 -1 27.58 3.62 5 -5 -1 28.12 2.89 5 -5 -2 13.83 2.39 5 -5 -2 14.10 2.80 5 5 2 11.49 2.19 5 -5 -2 13.47 2.05 5 -5 -3 127.38 7.21 5 -5 -3 134.82 8.76 5 5 3 128.72 7.35 5 -5 -3 135.00 6.58 5 -5 -4 19.54 2.85 5 5 4 15.34 2.58 5 5 4 17.29 2.84 5 -5 -4 20.30 2.61 5 -5 -5 52.03 4.62 5 5 5 61.48 5.15 5 5 5 55.68 5.04 5 -5 -5 71.28 4.93 5 5 6 31.65 3.69 5 5 6 33.73 3.84 5 -5 -6 33.35 3.39 5 5 7 57.47 4.96 5 5 7 66.25 5.25 5 -5 -7 71.28 4.96 5 5 8 9.92 1.98 5 -5 -8 12.27 2.03 5 5 9 44.51 4.10 5 6 -5 44.11 3.58 5 -6 4 34.22 3.93 -5 -6 -3 51.27 2.68 5 -6 3 46.60 4.07 5 -6 3 51.67 4.93 -5 -6 -2 8.00 1.07 5 -6 2 10.69 2.01 5 -6 2 9.06 2.25 5 -6 1 59.75 4.70 5 6 -1 52.86 4.42 5 -6 0 22.12 2.91 5 6 0 21.93 2.94 5 -6 -1 62.62 5.11 5 6 1 50.97 4.51 -5 -6 2 11.08 1.10 5 -6 -2 11.69 2.32 5 6 2 10.40 2.09 5 -6 -2 10.79 1.84 5 -6 -3 50.84 4.71 5 6 3 49.94 4.55 5 -6 -3 55.81 4.20 5 -6 -4 28.25 3.49 5 6 4 35.65 3.89 5 -6 -4 38.64 3.54 5 6 5 38.27 4.04 5 -6 -5 46.02 3.90 5 6 6 29.67 3.54 5 -6 -6 40.36 3.65 5 6 7 74.31 5.47 5 -6 -7 81.17 5.17 5 6 8 5.74 1.52 5 7 -5 31.95 3.01 5 7 -4 15.74 2.18 -5 -7 -4 19.74 1.68 -5 -7 -3 12.85 1.41 5 -7 3 18.92 2.55 5 -7 2 17.50 2.50 5 -7 1 36.34 3.58 5 7 -1 33.60 3.40 5 -7 0 -0.84 0.66 5 7 0 -1.22 0.73 5 -7 -1 43.10 4.22 5 7 1 36.61 3.75 -5 -7 2 15.78 1.29 5 -7 -2 19.10 3.03 5 7 2 15.12 2.46 5 -7 -3 18.43 2.79 5 7 3 17.47 2.67 5 -7 -3 19.84 2.48 5 -7 -4 15.86 2.52 5 7 4 19.12 2.80 5 -7 -4 21.45 2.60 5 7 5 41.74 4.09 5 -7 -5 47.65 3.87 5 -7 -6 8.76 1.77 5 7 6 12.22 2.21 5 -7 -7 27.06 3.23 5 7 7 40.13 3.85 -5 -8 -11 3.17 0.50 -5 -8 -10 0.25 0.23 -5 -8 -9 15.53 1.25 -5 -8 -8 5.40 0.78 -5 -8 -7 27.49 1.78 -5 -8 -6 8.12 1.03 -5 -8 -5 25.90 1.82 5 -8 3 75.55 4.98 5 -8 2 41.31 3.73 5 -8 1 72.24 4.97 5 -8 0 34.93 3.52 5 8 0 32.40 3.28 -5 -8 1 67.80 2.66 5 -8 -1 76.80 5.32 5 8 1 65.09 4.71 5 -8 -2 41.72 4.03 5 8 2 34.89 3.59 5 -8 -3 76.66 5.79 5 8 3 64.88 4.91 5 -8 -4 28.40 3.41 5 8 4 26.59 3.07 5 -8 -5 49.16 4.35 5 -8 -6 5.90 1.58 5 -9 2 5.18 1.22 -5 -9 -1 3.39 0.59 5 -9 1 3.51 1.05 -5 -9 0 8.03 0.90 5 -9 0 8.63 1.60 5 -9 -1 3.29 1.11 5 -9 -2 4.42 1.23 -5 -10 -3 32.11 1.61 -5 -10 -2 12.04 1.00 6 0 4 159.29 8.76 6 0 5 -0.04 0.72 6 0 6 35.55 4.07 6 0 7 10.72 2.17 6 -1 7 15.58 2.58 6 -1 6 49.95 4.73 6 -1 5 10.08 2.17 6 1 3 48.37 4.86 6 1 4 3.92 1.46 6 1 5 8.76 2.10 6 1 6 42.73 4.42 6 1 7 15.69 2.62 6 -2 7 40.30 4.07 6 -2 6 66.78 5.41 6 -2 5 25.39 3.56 6 2 0 73.86 5.78 6 2 1 35.82 4.02 6 2 2 87.76 6.42 6 2 3 55.91 5.10 6 2 4 65.05 5.45 6 2 5 39.50 4.27 6 2 6 68.05 5.42 6 2 7 38.84 3.98 6 -3 6 54.21 4.69 6 3 1 33.16 3.69 6 3 2 15.48 2.58 6 3 3 51.18 4.71 6 3 4 68.33 5.41 6 3 5 32.25 3.64 6 3 6 56.87 4.79 6 4 0 21.03 2.81 6 4 1 2.12 0.95 6 4 2 45.87 4.30 6 4 3 13.97 2.36 0 0 0 0.00 0.00 TITL Metoxy_disulp in P2(1)2(1)2(1) REM P2(1)2(1)2(1) (#19 in standard setting) CELL 1.54184 5.903725 12.979953 17.904119 90.0000 90.0000 90.0000 ZERR 4.00 0.000220 0.000417 0.000562 0.0000 0.0000 0.0000 LATT -1 SYMM -x+1/2,-y, z+1/2 SYMM -x, y+1/2,-z+1/2 SYMM x+1/2,-y+1/2,-z SFAC C H O S UNIT 56.00 56.00 8.00 8.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 96604 _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 ; _oxdiff_exptl_absorpt_empirical_full_max 1.998 _oxdiff_exptl_absorpt_empirical_full_min 0.530 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-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 S2 S 0.48037(14) 0.02249(5) 0.01676(4) 0.0644(3) Uani 1 1 d . . . . . S1 S 0.15554(14) -0.02837(6) 0.02182(4) 0.0670(3) Uani 1 1 d . . . . . C8 C 0.1369(5) -0.1254(2) -0.04849(15) 0.0553(7) Uani 1 1 d . . . . . O2 O 0.0308(4) -0.35851(18) -0.20235(12) 0.0800(7) Uani 1 1 d . . . . . C1 C 0.4795(5) 0.1200(2) -0.05358(14) 0.0545(7) Uani 1 1 d . . . . . C11 C 0.0754(6) -0.2835(2) -0.15049(16) 0.0600(8) Uani 1 1 d . . . . . C4 C 0.5109(6) 0.2737(2) -0.16041(16) 0.0635(8) Uani 1 1 d . . . . . O1 O 0.5071(5) 0.34690(19) -0.21613(12) 0.0848(7) Uani 1 1 d . . . . . C9 C 0.3034(6) -0.1986(2) -0.05918(17) 0.0600(7) Uani 1 1 d . . . . . C10 C 0.2744(6) -0.2766(2) -0.11065(18) 0.0615(8) Uani 1 1 d . . . . . C6 C 0.6672(6) 0.1827(2) -0.05683(18) 0.0635(8) Uani 1 1 d . . . . . C5 C 0.6832(7) 0.2594(2) -0.11044(19) 0.0666(8) Uani 1 1 d . . . . . C2 C 0.3077(6) 0.1348(2) -0.10428(18) 0.0676(8) Uani 1 1 d . . . . . C13 C -0.0610(6) -0.1321(2) -0.08966(17) 0.0623(8) Uani 1 1 d . . . . . C3 C 0.3196(7) 0.2115(3) -0.15675(19) 0.0731(9) Uani 1 1 d . . . . . C14 C 0.2008(9) -0.4305(3) -0.2187(3) 0.0862(11) Uani 1 1 d . . . . . C12 C -0.0932(6) -0.2103(3) -0.13960(17) 0.0658(9) Uani 1 1 d . . . . . H12 H -0.220(7) -0.219(3) -0.1649(17) 0.079 Uiso 1 1 d . U . . . C7 C 0.6998(9) 0.4102(3) -0.2247(3) 0.0851(11) Uani 1 1 d . . . . . H2 H 0.177(6) 0.096(2) -0.1022(16) 0.061(8) Uiso 1 1 d . . . . . H7A H 0.840(7) 0.373(3) -0.230(2) 0.090(13) Uiso 1 1 d . . . . . H6 H 0.800(6) 0.173(2) -0.0217(18) 0.087(10) Uiso 1 1 d . . . . . H7B H 0.670(7) 0.444(3) -0.267(2) 0.090(12) Uiso 1 1 d . . . . . H14A H 0.235(8) -0.475(3) -0.176(3) 0.114(15) Uiso 1 1 d . . . . . H14B H 0.363(7) -0.399(3) -0.231(2) 0.092(12) Uiso 1 1 d . . . . . H3 H 0.207(7) 0.222(3) -0.1880(18) 0.087(11) Uiso 1 1 d . . . . . H7C H 0.698(7) 0.457(3) -0.182(2) 0.107(13) Uiso 1 1 d . . . . . H9 H 0.438(6) -0.195(2) -0.0342(15) 0.065(9) Uiso 1 1 d . . . . . H5 H 0.818(7) 0.293(3) -0.1129(17) 0.082(10) Uiso 1 1 d . . . . . H10 H 0.382(6) -0.319(2) -0.1196(16) 0.063(9) Uiso 1 1 d . . . . . H14C H 0.150(7) -0.466(4) -0.258(2) 0.106(14) Uiso 1 1 d . . . . . H13 H -0.182(6) -0.083(2) -0.0856(16) 0.065(8) 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 S2 0.0603(5) 0.0671(4) 0.0658(5) -0.0024(4) -0.0034(4) 0.0013(3) S1 0.0647(5) 0.0726(5) 0.0636(5) -0.0028(4) 0.0137(4) -0.0041(4) C8 0.0532(19) 0.0588(15) 0.0540(15) 0.0093(13) 0.0072(14) -0.0026(13) O2 0.0762(17) 0.0870(13) 0.0768(13) -0.0148(12) -0.0123(13) 0.0068(15) C1 0.0479(18) 0.0581(14) 0.0576(15) -0.0132(13) 0.0033(14) 0.0032(13) C11 0.059(2) 0.0680(17) 0.0536(15) 0.0063(15) 0.0027(16) -0.0016(15) C4 0.067(2) 0.0644(16) 0.0596(17) -0.0036(15) 0.0071(17) -0.0027(17) O1 0.0896(19) 0.0896(14) 0.0753(13) 0.0145(12) 0.0012(14) -0.0144(16) C9 0.0497(19) 0.0593(16) 0.0711(18) 0.0101(16) -0.0048(17) -0.0008(14) C10 0.057(2) 0.0540(16) 0.0731(19) 0.0062(16) 0.0005(18) 0.0078(15) C6 0.0504(19) 0.0665(17) 0.0734(19) -0.0091(16) -0.0097(16) -0.0040(15) C5 0.055(2) 0.0642(18) 0.081(2) -0.0077(17) 0.001(2) -0.0109(15) C2 0.054(2) 0.081(2) 0.0671(18) 0.0004(18) -0.0013(17) -0.0146(18) C13 0.0505(19) 0.0729(19) 0.0636(18) 0.0031(16) 0.0088(15) 0.0104(15) C3 0.054(2) 0.100(2) 0.065(2) 0.006(2) -0.0065(18) -0.014(2) C14 0.094(3) 0.077(2) 0.088(3) -0.017(2) 0.007(3) -0.001(2) C12 0.0458(19) 0.094(2) 0.0580(18) 0.0009(18) -0.0033(16) 0.0072(17) C7 0.100(3) 0.077(2) 0.078(3) 0.003(2) 0.019(3) -0.012(2) 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' S S 0.3331 0.5567 '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 8 3 0.0475 0 -8 -4 0.0550 -4 -1 0 0.1030 0 3 -11 0.0207 4 1 1 0.1165 0 -3 11 0.0223 -2 4 8 0.0872 -3 -6 1 0.0795 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 C1 S2 S1 105.03(10) . . ? C8 S1 S2 104.86(10) . . ? C9 C8 S1 122.7(2) . . ? C9 C8 C13 118.9(3) . . ? C13 C8 S1 118.2(2) . . ? C11 O2 C14 118.5(3) . . ? C6 C1 S2 116.5(2) . . ? C2 C1 S2 124.5(2) . . ? C2 C1 C6 118.9(3) . . ? O2 C11 C10 124.1(3) . . ? O2 C11 C12 116.3(3) . . ? C10 C11 C12 119.6(3) . . ? O1 C4 C3 114.9(3) . . ? C5 C4 O1 125.4(3) . . ? C5 C4 C3 119.7(3) . . ? C4 O1 C7 117.8(3) . . ? C8 C9 H9 121.3(18) . . ? C10 C9 C8 120.6(3) . . ? C10 C9 H9 118.0(17) . . ? C11 C10 C9 120.0(3) . . ? C11 C10 H10 120(2) . . ? C9 C10 H10 120(2) . . ? C1 C6 C5 120.6(3) . . ? C1 C6 H6 121.8(18) . . ? C5 C6 H6 117.6(18) . . ? C4 C5 C6 120.0(3) . . ? C4 C5 H5 124(2) . . ? C6 C5 H5 116(2) . . ? C1 C2 H2 120.8(18) . . ? C3 C2 C1 121.1(3) . . ? C3 C2 H2 118.0(18) . . ? C8 C13 H13 123.1(17) . . ? C12 C13 C8 120.8(3) . . ? C12 C13 H13 116.0(17) . . ? C4 C3 H3 120(2) . . ? C2 C3 C4 119.7(3) . . ? C2 C3 H3 121(2) . . ? O2 C14 H14A 112(3) . . ? O2 C14 H14B 115(2) . . ? O2 C14 H14C 106(3) . . ? H14A C14 H14B 101(3) . . ? H14A C14 H14C 112(4) . . ? H14B C14 H14C 110(3) . . ? C11 C12 H12 117(2) . . ? C13 C12 C11 120.0(3) . . ? C13 C12 H12 123(2) . . ? O1 C7 H7A 114(2) . . ? O1 C7 H7B 103(3) . . ? O1 C7 H7C 106(3) . . ? H7A C7 H7B 109(3) . . ? H7A C7 H7C 114(4) . . ? H7B C7 H7C 111(3) . . ? 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 S2 S1 2.0301(12) . ? S2 C1 1.786(3) . ? S1 C8 1.784(3) . ? C8 C9 1.381(4) . ? C8 C13 1.384(4) . ? O2 C11 1.371(4) . ? O2 C14 1.403(5) . ? C1 C6 1.376(4) . ? C1 C2 1.375(4) . ? C11 C10 1.378(5) . ? C11 C12 1.389(5) . ? C4 O1 1.378(3) . ? C4 C5 1.367(5) . ? C4 C3 1.390(5) . ? O1 C7 1.412(5) . ? C9 C10 1.379(4) . ? C9 H9 0.91(3) . ? C10 H10 0.86(3) . ? C6 C5 1.386(4) . ? C6 H6 1.01(3) . ? C5 H5 0.91(4) . ? C2 C3 1.371(4) . ? C2 H2 0.92(3) . ? C13 C12 1.366(5) . ? C13 H13 0.96(3) . ? C3 H3 0.88(4) . ? C14 H14A 0.98(5) . ? C14 H14B 1.06(4) . ? C14 H14C 0.89(5) . ? C12 H12 0.88(4) . ? C7 H7A 0.96(4) . ? C7 H7B 0.90(4) . ? C7 H7C 0.97(5) . ? 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 S2 S1 C8 C9 43.2(2) . . . . ? S2 S1 C8 C13 -142.2(2) . . . . ? S2 C1 C6 C5 178.9(2) . . . . ? S2 C1 C2 C3 -180.0(3) . . . . ? S1 S2 C1 C6 166.17(19) . . . . ? S1 S2 C1 C2 -14.8(3) . . . . ? S1 C8 C9 C10 175.4(2) . . . . ? S1 C8 C13 C12 -174.2(2) . . . . ? C8 C9 C10 C11 -1.8(4) . . . . ? C8 C13 C12 C11 -1.1(5) . . . . ? O2 C11 C10 C9 -179.6(3) . . . . ? O2 C11 C12 C13 -179.1(3) . . . . ? C1 C6 C5 C4 0.4(5) . . . . ? C1 C2 C3 C4 1.9(5) . . . . ? O1 C4 C5 C6 -179.8(3) . . . . ? O1 C4 C3 C2 178.7(3) . . . . ? C9 C8 C13 C12 0.7(4) . . . . ? C10 C11 C12 C13 0.1(5) . . . . ? C6 C1 C2 C3 -1.0(5) . . . . ? C5 C4 O1 C7 2.6(5) . . . . ? C5 C4 C3 C2 -1.6(5) . . . . ? C2 C1 C6 C5 -0.1(4) . . . . ? C13 C8 C9 C10 0.8(4) . . . . ? C3 C4 O1 C7 -177.8(3) . . . . ? C3 C4 C5 C6 0.5(5) . . . . ? C14 O2 C11 C10 -2.9(4) . . . . ? C14 O2 C11 C12 176.2(3) . . . . ? C12 C11 C10 C9 1.3(5) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.70(3) 2 0.30(3) 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 0.7754 7.9963 2.8000 0.0238 0.9547 -0.2965 -0.1859 -8.0101 -3.5527 -0.0246 -0.9907 0.1335 -3.8218 -0.6121 -0.3441 -0.3710 0.0070 0.9286 -0.4796 2.8747 -10.8262 -0.9679 0.0245 -0.2502 3.8210 0.5542 0.5553 0.3890 -0.0074 -0.9212 0.4796 -2.8747 10.8262 0.9679 -0.0245 0.2502 -2.0106 3.9796 8.0022 0.2879 0.7159 0.6143 -3.0002 -6.0121 0.9975 -0.0117 -0.5760 0.8929