#------------------------------------------------------------------------------ #$Date: 2021-09-04 00:23:46 +0300 (Sat, 04 Sep 2021) $ #$Revision: 268443 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/90/4519020.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_4519020 loop_ _publ_author_name 'Huke, Cameron D.' 'Taylor, Laurence J.' 'Argent, Stephen P.' 'Kays, Deborah L.' _publ_section_title ; Catalyst-free Hydrophosphinylation of Isocyanates and Isothiocyanates under Low-Added-Solvent Conditions ; _journal_issue 32 _journal_name_full 'ACS Sustainable Chemistry & Engineering' _journal_page_first 10704 _journal_page_last 10709 _journal_paper_doi 10.1021/acssuschemeng.1c02907 _journal_volume 9 _journal_year 2021 _chemical_formula_moiety 'C15 H16 N O2 P' _chemical_formula_sum 'C15 H16 N O2 P' _chemical_formula_weight 273.26 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2021-02-18 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257) ; _cell_angle_alpha 90.450(3) _cell_angle_beta 93.891(3) _cell_angle_gamma 117.301(4) _cell_formula_units_Z 4 _cell_length_a 8.7838(4) _cell_length_b 8.7951(4) _cell_length_c 20.4442(8) _cell_measurement_reflns_used 9535 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 72.4220 _cell_measurement_theta_min 4.3470 _cell_volume 1398.88(12) _computing_cell_refinement 'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_environment 'N2 gas' _diffrn_ambient_temperature 120(2) _diffrn_crystal_treatment 'flash frozen in gaseous N2' _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 5.2349 _diffrn_detector_type 'Agilent Diffraction Atlas S2 detector' _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.979 _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 -4.00 21.00 1.00 4.00 -- 34.00 91.00 178.08 25 2 \w -5.00 20.00 1.00 4.00 -- 34.00 94.00 87.64 25 3 \w -112.00 -13.00 1.00 4.00 -- -40.95 -57.00 150.00 99 4 \w 58.00 101.00 1.00 4.00 -- 40.95 38.00 -30.00 43 5 \w -29.00 69.00 1.00 4.00 -- 40.95 -57.00 30.00 98 6 \w 25.00 56.00 1.00 4.00 -- 40.95 38.00 -30.00 31 7 \w 28.00 97.00 1.00 4.00 -- 40.95-125.00 -60.00 69 8 \w 7.00 32.00 1.00 4.00 -- 42.00 84.00 -29.01 25 9 \w 16.00 41.00 1.00 4.00 -- 50.00 82.00-118.59 25 10 \w 16.00 41.00 1.00 4.00 -- 50.00 81.00-168.19 25 11 \w 16.00 41.00 1.00 4.00 -- 50.00 81.00 31.84 25 12 \w 16.00 41.00 1.00 4.00 -- 50.00 82.00 -38.62 25 13 \w 16.00 41.00 1.00 4.00 -- 50.00 82.00 41.65 25 14 \w 16.00 41.00 1.00 4.00 -- 50.00 81.00-133.72 25 15 \w 16.00 41.00 1.00 4.00 -- 50.00 82.00 128.30 25 16 \w 23.00 50.00 1.00 4.00 -- 54.00 71.00 17.80 27 17 \w 64.00 128.00 1.00 4.00 -- 54.00 71.00 17.80 64 18 \w 25.00 52.00 1.00 4.00 -- 54.00 74.00 102.46 27 19 \w 96.00 122.00 1.00 4.00 -- 54.00 74.00 102.46 26 20 \w 92.00 131.00 1.00 4.00 -- 58.00 74.00 54.49 39 21 \w 28.00 55.00 1.00 4.00 -- 58.00 74.00 54.49 27 22 \w 30.00 61.00 1.00 4.00 -- 62.00 74.00 108.47 31 23 \w 33.00 60.00 1.00 4.00 -- 62.00 71.00 159.17 27 24 \w 109.00 134.00 1.00 4.00 -- 62.00 74.00 108.47 25 25 \w 97.00 134.00 1.00 4.00 -- 62.00 71.00 159.17 37 26 \w 34.00 61.00 1.00 4.00 -- 66.00 74.00 -77.72 27 27 \w 36.00 64.00 1.00 4.00 -- 66.00 64.00-104.30 28 28 \w 37.00 76.00 1.00 4.00 -- 66.00 68.00 8.39 39 29 \w 39.00 73.00 1.00 4.00 -- 70.00 73.00 175.70 34 30 \w 43.00 69.00 1.00 4.00 -- 70.00 54.00 155.70 26 31 \w 44.00 76.00 1.00 16.00 -- 74.00 66.00 49.23 32 32 \w 101.00 149.00 1.00 16.00 -- 74.00 73.00 -61.02 48 33 \w 42.00 69.00 1.00 16.00 -- 74.00 73.00 -61.02 27 34 \w 121.00 148.00 1.00 16.00 -- 78.00 64.00 -39.95 27 35 \w 51.00 84.00 1.00 16.00 -- 78.00 64.00 -39.95 33 36 \w 52.00 91.00 1.00 16.00 -- 82.00 65.00-142.70 39 37 \w 58.00 86.00 1.00 16.00 -- 86.00 62.00 93.02 28 38 \w 75.00 171.00 1.00 16.00 -- 104.05 61.00 90.00 96 39 \w 129.00 173.00 1.00 16.00 -- 104.05 125.00 0.00 44 40 \w 31.00 112.00 1.00 16.00 -- 104.05-125.00 -30.00 81 41 \w 76.00 103.00 1.00 16.00 -- 104.05 61.00 30.00 27 42 \w 68.00 111.00 1.00 16.00 -- 104.05-125.00 30.00 43 43 \w 75.00 172.00 1.00 16.00 -- 104.05 61.00 0.00 97 44 \w 75.00 171.00 1.00 16.00 -- 104.05 61.00-150.00 96 45 \w 75.00 159.00 1.00 16.00 -- 104.05 61.00 120.00 84 46 \w 116.00 141.00 1.00 16.00 -- 104.05 61.00 60.00 25 47 \w 75.00 102.00 1.00 16.00 -- 104.05 61.00 60.00 27 48 \w 30.00 85.00 1.00 16.00 -- 104.05 -77.00 -30.00 55 49 \w 114.00 175.00 1.00 16.00 -- 104.05 61.00 150.00 61 50 \w 83.00 112.00 1.00 16.00 -- 104.05-125.00-120.00 29 51 \w 76.00 102.00 1.00 16.00 -- 104.05 61.00 150.00 26 52 \w 32.00 81.00 1.00 16.00 -- 104.05-125.00-120.00 49 53 \w 75.00 176.00 1.00 16.00 -- 104.05 61.00 -90.00 101 54 \w 117.00 144.00 1.00 16.00 -- 104.05 61.00 -30.00 27 55 \w 75.00 104.00 1.00 16.00 -- 104.05 61.00 -30.00 29 56 \w 129.00 156.00 1.00 16.00 -- 104.05 61.00-180.00 27 57 \w 112.00 175.00 1.00 16.00 -- 104.05 61.00 30.00 63 58 \w 28.00 117.00 1.00 16.00 -- 104.05 -77.00 90.00 89 59 \w 75.00 114.00 1.00 16.00 -- 104.05 61.00-180.00 39 60 \w 76.00 154.00 1.00 16.00 -- 104.05 61.00-120.00 78 61 \w 119.00 176.00 1.00 16.00 -- 104.05 61.00 -60.00 57 62 \w 75.00 107.00 1.00 16.00 -- 104.05 61.00 -60.00 32 63 \w 24.00 107.00 1.00 16.00 -- 104.05 -94.00 60.00 83 ; _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'SuperNova, Atlas S2' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'MiTeGen micromount' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0398021000 _diffrn_orient_matrix_UB_12 0.1501229000 _diffrn_orient_matrix_UB_13 0.0136117000 _diffrn_orient_matrix_UB_21 0.1900405000 _diffrn_orient_matrix_UB_22 0.1141018000 _diffrn_orient_matrix_UB_23 0.0236856000 _diffrn_orient_matrix_UB_31 0.0391497000 _diffrn_orient_matrix_UB_32 0.0580998000 _diffrn_orient_matrix_UB_33 -0.0704835000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_unetI/netI 0.0183 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.979 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 7807 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.979 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.753 _diffrn_reflns_theta_min 4.339 _diffrn_source 'microfocus sealed tube' _diffrn_source_type 'Agilent Diffraction microfocus tube' _exptl_absorpt_coefficient_mu 1.721 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.537 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020) 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 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.297 _exptl_crystal_description block _exptl_crystal_F_000 576 _exptl_crystal_recrystallization_method 'Recystallised from ethanol' _exptl_crystal_size_max 0.284 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.078 _refine_diff_density_max 0.449 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.048 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 352 _refine_ls_number_reflns 7807 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.058 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0356 _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^)+(0.0688P)^2^+0.2094P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1038 _refine_ls_wR_factor_ref 0.1059 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6791 _reflns_number_total 7807 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file sc1c02907_si_002.cif _cod_data_source_block ochdkb _cod_original_cell_volume 1398.88(11) _cod_database_code 4519020 _nottingham_internal_coll_name OCHDKB _nottingham_internal_coll_number 18736 _nottingham_internal_coll_client CH/DLK _nottingham_internal_coll_type custom _nottingham_internal_coll_frame_method '\w scans' _nottingham_internal_coll_frame_time '16.00, 4.00' _nottingham_internal_coll_frame_width 1.00 _nottingham_internal_coll_user pczlt _nottingham_internal_coll_date 20/07/2020 _nottingham_internal_coll_location NOTTS _nottingham_internal_coll_instrument 'GVB, PL13110001' _nottingham_internal_process_date 06/08/2020 _nottingham_internal_process_user pczlt _nottingham_internal_solution_date 06/08/2020 _nottingham_internal_solution_user pczlt _nottingham_internal_refinement_date 06/08/2020 _nottingham_internal_refinement_user pczlt _nottingham_internal_self_archive_date 16/02/2021 _nottingham_internal_self_validation_date 16/02/2021 _nottingham_internal_self_validation_user pcxch6 _nottingham_internal_validation_date 17/02/2021 _nottingham_internal_validation_user pczspa _nottingham_internal_archive_date 17/02/2021 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C15H16N1O2P _chemical_oxdiff_usercomment 'OCHDKB #18736 GVB-1803 CH/DLK fomblin micromount' _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 0.877 _shelx_estimated_absorpt_t_min 0.641 _reflns_odcompleteness_completeness 99.90 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.5320(9) 0.4680(9) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 3. Restrained distances N1-H1 0.88 with sigma of 0.02 N2-H2A 0.88 with sigma of 0.02 4.a Secondary CH2 refined with riding coordinates: C29(H29A,H29B), C14(H14A,H14B) 4.b Aromatic/amide H refined with riding coordinates: C2(H2), C8(H8), C4(H4), C23(H23), C18(H18), C9(H9), C24(H24), C3(H3), C21(H21), C27(H27), C12(H12), C6(H6), C17(H17), C25(H25), C10(H10), C26(H26), C19(H19), C20(H20), C11(H11), C5(H5) 4.c Idealised Me refined as rotating group: C30(H30A,H30B,H30C), C15(H15A,H15B,H15C) ; _shelx_res_file ; TITL ochdkb_a.res in P-1 ochdkb.res created by SHELXL-2018/3 at 10:08:00 on 18-Feb-2021 REM Old TITL OCHDKB in P-1 REM SHELXT solution in P-1: R1 0.126, Rweak 0.012, Alpha 0.051 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C30 N2 O4 P2 CELL 1.54184 8.7838 8.7951 20.4442 90.45 93.891 117.301 ZERR 4 0.0004 0.0004 0.0008 0.003 0.003 0.004 LATT 1 SFAC C H N O P UNIT 60 64 4 8 4 DFIX 0.88 N1 H1 DFIX 0.88 N2 H2a L.S. 20 PLAN 4 SIZE 0.078 0.1 0.284 TEMP -153(2) CONF HTAB N2 O1 HTAB N1 O3 BOND list 4 MORE -1 BOND $H fmap 2 53 acta OMIT -6 -1 0 OMIT 6 1 -2 OMIT 8 -9 -2 OMIT 1 6 -2 OMIT 9 -8 0 OMIT 1 6 0 OMIT -1 -1 -15 OMIT 2 -3 -10 REM REM REM WGHT 0.068800 0.209400 BASF 0.46796 FVAR 5.84333 P1 5 0.553606 0.526153 0.334860 11.00000 0.02424 0.02344 = 0.02091 0.00465 0.00453 0.00814 P2 5 0.984663 0.917126 0.165321 11.00000 0.02008 0.02775 = 0.02150 0.00436 0.00515 0.00943 O3 4 0.965522 0.871145 0.235205 11.00000 0.02692 0.03901 = 0.02332 0.00523 0.00472 0.01199 O4 4 0.795411 0.792598 0.050200 11.00000 0.02612 0.04124 = 0.02244 0.00701 0.00448 0.01176 O1 4 0.586461 0.549835 0.264515 11.00000 0.03439 0.03133 = 0.02290 0.00422 0.00625 0.00827 O2 4 0.689480 0.714382 0.447702 11.00000 0.03500 0.02836 = 0.02308 0.00374 0.00719 0.01074 N2 3 0.676681 0.640840 0.139151 11.00000 0.02462 0.02738 = 0.02253 0.00450 0.00425 0.00975 H2A 2 0.683991 0.637198 0.181500 11.00000 -1.20000 N1 3 0.839797 0.828135 0.358424 11.00000 0.02651 0.02594 = 0.02304 0.00210 0.00493 0.00943 H1 2 0.843610 0.812588 0.316659 11.00000 -1.20000 C13 1 0.711196 0.709530 0.388999 11.00000 0.02517 0.02128 = 0.02426 0.00382 0.00349 0.01006 C2 1 0.596513 0.324936 0.433411 11.00000 0.02406 0.02598 = 0.03034 0.00431 0.00527 0.00958 AFIX 43 H2 2 0.600081 0.407557 0.464514 11.00000 -1.20000 AFIX 0 C28 1 0.798477 0.767793 0.109459 11.00000 0.02120 0.02767 = 0.02386 0.00382 0.00514 0.01088 C1 1 0.570980 0.343938 0.366466 11.00000 0.02215 0.02174 = 0.02978 0.00488 0.00628 0.00875 C29 1 0.520612 0.509328 0.103510 11.00000 0.02279 0.02880 = 0.02905 0.00391 0.00396 0.00713 AFIX 23 H29A 2 0.490845 0.559436 0.064545 11.00000 -1.20000 H29B 2 0.424383 0.471426 0.132147 11.00000 -1.20000 AFIX 0 C8 1 0.268841 0.438775 0.408339 11.00000 0.02715 0.02530 = 0.03003 0.00451 0.00359 0.01094 AFIX 43 H8 2 0.317101 0.386744 0.437927 11.00000 -1.20000 AFIX 0 C22 1 1.167409 0.908464 0.134076 11.00000 0.02132 0.02226 = 0.02926 0.00574 0.00478 0.00900 C4 1 0.609904 0.063396 0.409168 11.00000 0.03210 0.02596 = 0.05515 0.00949 0.01017 0.01597 AFIX 43 H4 2 0.623090 -0.032513 0.423732 11.00000 -1.20000 AFIX 0 C7 1 0.350794 0.513780 0.352481 11.00000 0.02321 0.02372 = 0.02736 0.00397 0.00283 0.00979 C23 1 1.182661 0.891788 0.067165 11.00000 0.02334 0.02617 = 0.02941 0.00460 0.00482 0.01009 AFIX 43 H23 2 1.097234 0.890526 0.035750 11.00000 -1.20000 AFIX 0 C14 1 0.976513 0.981745 0.393389 11.00000 0.02652 0.02430 = 0.03227 0.00082 0.00472 0.00617 AFIX 23 H14A 2 0.928889 1.014010 0.430511 11.00000 -1.20000 H14B 2 1.016839 1.077644 0.363255 11.00000 -1.20000 AFIX 0 C18 1 1.056045 1.364809 0.083724 11.00000 0.03177 0.02903 = 0.05068 0.00741 0.00093 0.01242 AFIX 43 H18 2 1.102347 1.426700 0.046003 11.00000 -1.20000 AFIX 0 C9 1 0.115966 0.440854 0.420313 11.00000 0.02829 0.03259 = 0.03820 0.00379 0.01008 0.01162 AFIX 43 H9 2 0.058873 0.388416 0.457963 11.00000 -1.20000 AFIX 0 C24 1 1.322747 0.877086 0.046720 11.00000 0.03268 0.02939 = 0.03543 0.00532 0.01217 0.01538 AFIX 43 H24 2 1.332188 0.864094 0.001226 11.00000 -1.20000 AFIX 0 C3 1 0.616683 0.185166 0.454473 11.00000 0.02505 0.03058 = 0.03771 0.00985 0.00529 0.01210 AFIX 43 H3 2 0.635178 0.172786 0.500017 11.00000 -1.20000 AFIX 0 C21 1 0.921842 1.186886 0.194497 11.00000 0.03379 0.04082 = 0.03618 -0.00426 0.00562 0.01770 AFIX 43 H21 2 0.877190 1.126805 0.232745 11.00000 -1.20000 AFIX 0 C27 1 1.293853 0.910836 0.179850 11.00000 0.02659 0.03468 = 0.03151 0.00809 0.00561 0.01451 AFIX 43 H27 2 1.283704 0.921462 0.225428 11.00000 -1.20000 AFIX 0 C16 1 0.993317 1.121466 0.150219 11.00000 0.02329 0.02680 = 0.02823 0.00045 0.00209 0.01085 C12 1 0.277986 0.588666 0.309298 11.00000 0.03419 0.03594 = 0.03133 0.00888 0.00204 0.01705 AFIX 43 H12 2 0.331992 0.637071 0.270620 11.00000 -1.20000 AFIX 0 C6 1 0.565215 0.221751 0.321033 11.00000 0.03151 0.03139 = 0.03274 0.00183 0.00819 0.01244 AFIX 43 H6 2 0.548539 0.234328 0.275386 11.00000 -1.20000 AFIX 0 C17 1 1.061200 1.211890 0.094593 11.00000 0.02658 0.03117 = 0.03268 0.00413 0.00416 0.01253 AFIX 43 H17 2 1.110757 1.168624 0.064307 11.00000 -1.20000 AFIX 0 C25 1 1.449068 0.881200 0.092146 11.00000 0.02863 0.03746 = 0.04923 0.01221 0.01464 0.02119 AFIX 43 H25 2 1.545578 0.872765 0.077713 11.00000 -1.20000 AFIX 0 C10 1 0.046236 0.518184 0.378151 11.00000 0.02611 0.03761 = 0.04951 -0.00152 0.00060 0.01606 AFIX 43 H10 2 -0.057436 0.520214 0.387298 11.00000 -1.20000 AFIX 0 C26 1 1.434838 0.897634 0.158736 11.00000 0.02943 0.04862 = 0.04237 0.01244 0.00424 0.02322 AFIX 43 H26 2 1.521261 0.899869 0.189877 11.00000 -1.20000 AFIX 0 C30 1 0.541637 0.356373 0.081717 11.00000 0.03746 0.03135 = 0.05181 -0.00371 -0.00497 0.01265 AFIX 137 H30A 2 0.639792 0.393900 0.054836 11.00000 -1.50000 H30B 2 0.437083 0.275107 0.055825 11.00000 -1.50000 H30C 2 0.561706 0.300665 0.120319 11.00000 -1.50000 AFIX 0 C15 1 1.127128 0.955584 0.419220 11.00000 0.02975 0.03513 = 0.05215 -0.00481 -0.00280 0.01053 AFIX 137 H15A 2 1.181464 0.934100 0.382369 11.00000 -1.50000 H15B 2 1.087133 0.857206 0.447399 11.00000 -1.50000 H15C 2 1.210790 1.058422 0.444701 11.00000 -1.50000 AFIX 0 C19 1 0.983440 1.427344 0.127823 11.00000 0.03715 0.02842 = 0.06668 -0.00291 -0.00423 0.01880 AFIX 43 H19 2 0.980164 1.532211 0.120093 11.00000 -1.20000 AFIX 0 C20 1 0.915618 1.339079 0.182990 11.00000 0.04478 0.04442 = 0.05682 -0.01452 0.00075 0.02628 AFIX 43 H20 2 0.865087 1.382440 0.212812 11.00000 -1.20000 AFIX 0 C11 1 0.126595 0.592982 0.322489 11.00000 0.03962 0.04060 = 0.04533 0.00382 -0.00686 0.02329 AFIX 43 H11 2 0.078750 0.646747 0.293580 11.00000 -1.20000 AFIX 0 C5 1 0.583975 0.081696 0.342882 11.00000 0.04142 0.03103 = 0.04757 -0.00042 0.01274 0.01744 AFIX 43 H5 2 0.578943 -0.002140 0.312029 11.00000 -1.20000 AFIX 0 HKLF 5 REM ochdkb_a.res in P-1 REM wR2 = 0.1059, GooF = S = 1.058, Restrained GooF = 1.058 for all data REM R1 = 0.0356 for 6791 Fo > 4sig(Fo) and 0.0404 for all 7807 data REM 352 parameters refined using 2 restraints END WGHT 0.0689 0.2074 REM Highest 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147.554 2 -2 4 15 4727.33 139.438 2 -2 4 14 338.792 97.5061 2 -2 4 13 96.8975 78.0085 2 -2 4 12 1379.65 74.3784 2 -2 4 11 1617.02 73.0406 2 -2 4 10 1288.43 81.3291 2 -2 4 9 159.535 78.4014 2 -2 4 8 3229.87 94.7789 2 2 -4 -7 4905.95 109.723 2 2 -4 -6 3287.42 97.1254 2 -2 4 5 2158.99 109.515 2 -2 4 4 1974.21 130.524 2 -2 4 -2 51947.0 548.592 2 2 -4 3 72717.8 335.708 2 -2 4 -4 662.842 89.8573 2 -2 4 -5 30.4803 85.9280 2 -2 4 -6 9918.56 145.941 2 -2 4 -7 13184.6 133.052 2 -2 4 -8 2355.68 84.0905 2 -2 4 -9 1261.26 79.2577 2 -2 4 -10 4917.22 99.9931 2 -2 4 -11 746.807 62.2447 2 -2 4 -12 3108.19 77.4102 2 -2 4 -13 24982.9 163.349 2 -2 4 -14 12833.4 126.889 2 -2 4 -15 18843.1 171.198 2 -2 4 -16 6793.48 123.984 2 2 -4 17 522.621 95.2659 2 2 -4 18 6022.43 151.565 2 2 -4 19 506.217 110.082 2 2 -4 20 6036.64 196.622 2 2 -4 21 442.534 90.2686 2 2 -4 22 316.413 75.7817 2 2 -4 23 611.150 64.8980 2 -2 3 24 689.024 94.0980 2 -2 3 23 1284.69 130.265 2 -2 3 22 133.570 133.466 2 -2 3 21 764.142 88.2061 2 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187.128 92.4686 2 2 -3 19 51.7349 90.2633 2 2 -3 20 78.9797 71.8317 2 2 -3 21 7611.20 140.650 2 2 -3 22 712.297 88.4232 2 2 -3 23 695.099 75.9890 2 2 -3 24 418.428 83.1221 2 -2 2 24 1053.31 111.923 2 -2 2 23 1030.96 131.639 2 -2 2 22 489.344 146.756 2 -2 2 21 70.8726 68.6618 2 -2 2 20 1954.58 75.7535 2 -2 2 19 1017.14 80.7055 2 -2 2 18 22961.1 173.713 2 -2 2 17 227.572 72.4546 2 -2 2 16 10294.1 119.754 2 -2 2 15 1519.82 76.0420 2 -2 2 14 11021.7 128.504 2 -2 2 13 3890.74 121.140 2 2 -2 -12 294.910 111.708 2 2 -2 -11 2017.95 131.071 2 2 -2 -10 20949.9 257.565 2 2 -2 -9 1268.08 118.550 2 2 -2 -8 8451.15 122.285 2 -2 2 7 2083.42 98.0802 2 -2 2 6 21240.6 141.646 2 -2 2 5 1794.44 84.4576 2 -2 2 4 38502.1 179.755 2 -2 2 3 392.482 73.8542 2 -2 2 2 85.5679 67.3077 2 -2 2 1 27817.1 141.599 2 -2 2 0 216081. 485.554 2 -2 2 -1 40935.7 182.367 2 2 -2 2 16309.5 102.438 2 -2 2 -3 3783.67 79.9296 2 -2 2 -4 17502.5 138.946 2 -2 2 -5 670.851 59.2745 2 -2 2 -6 25573.3 143.872 2 -2 2 -7 2420.58 77.5709 2 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162.667 2 3 -4 22 2443.36 89.0485 2 3 -4 23 98.7662 77.2323 2 -3 3 24 100.485 80.5355 2 -3 3 23 323.824 111.625 2 -3 3 22 416.121 138.731 2 -3 3 21 298.962 148.821 2 -3 3 20 84.9789 70.1595 2 -3 3 19 315.671 75.1946 2 -3 3 18 7559.79 119.561 2 -3 3 17 11961.2 118.544 2 -3 3 16 54.9557 65.3966 2 -3 3 15 284.537 63.8709 2 -3 3 14 3695.34 80.1995 2 -3 3 13 3654.44 82.9286 2 -3 3 12 46.9251 74.3453 2 3 -3 -11 1642.61 93.6846 2 3 -3 -10 2411.95 97.2714 2 3 -3 -9 2051.47 90.9899 2 -3 3 8 5612.24 106.468 2 -3 3 7 9157.00 123.977 2 -3 3 6 1939.86 86.7223 2 -3 3 5 3897.85 94.3112 2 -3 3 4 306.632 92.0557 2 -3 3 3 20727.7 196.364 2 -3 3 2 91.4534 192.781 2 3 -3 0 36362.4 387.546 2 3 -3 1 4195.08 118.439 2 3 -3 2 6886.00 141.375 2 -3 3 -3 52805.3 285.079 2 -3 3 -4 136.755 75.3902 2 -3 3 -5 5039.92 116.204 2 -3 3 -6 492.838 91.8537 2 -3 3 -7 5661.14 103.825 2 -3 3 -8 5762.00 107.861 2 -3 3 -9 91.5167 75.5735 2 -3 3 -10 522.263 102.422 2 3 -3 11 1860.69 72.7876 2 3 -3 12 90.2766 72.4574 2 3 -3 13 12158.0 138.462 2 3 -3 14 3283.20 92.9140 2 -3 3 -15 4037.62 106.434 2 -3 3 -16 5506.13 120.520 2 3 -3 17 2295.56 109.082 2 3 -3 18 3433.87 117.850 2 3 -3 19 990.334 82.5464 2 3 -3 20 337.872 72.8579 2 3 -3 21-2.53177 71.4046 2 3 -3 22 371.174 119.926 2 3 -3 23 1286.42 106.770 2 -3 2 24 2383.98 119.587 2 -3 2 23 166.057 112.745 2 -3 2 22-25.0597 80.5424 2 -3 2 21 6955.21 146.460 2 -3 2 20 27.5735 102.778 2 -3 2 19 4656.88 104.716 2 -3 2 18 13.4066 69.8673 2 -3 2 17 12263.1 125.169 2 -3 2 16 2470.79 72.3973 2 -3 2 15 17179.7 129.760 2 -3 2 14 6556.66 100.380 2 -3 2 13 6982.33 94.9227 2 3 -2 -12 1654.46 137.117 2 3 -2 -11 506.503 117.902 2 3 -2 -10 51.2820 94.4125 2 3 -2 -9 41497.5 214.072 2 3 -2 -8 11689.4 124.005 2 3 -2 -7 1588.75 73.2846 2 3 -2 -6 14720.8 118.484 2 -3 2 5 28972.7 242.305 2 -3 2 4 56544.7 267.995 2 -3 2 3 55987.7 304.641 2 -3 2 2 2770.35 109.925 2 -3 2 1 3784.84 109.602 2 -3 2 0 973.948 61.4120 2 -3 2 -1 41441.0 195.510 2 -3 2 -2 8212.56 131.070 2 -3 2 -3 38323.7 171.174 2 3 -2 4 3184.52 79.0073 2 3 -2 5 18140.5 121.609 2 -3 2 -6 368.377 65.1331 2 3 -2 7 28872.4 164.179 2 3 -2 8 3629.77 88.5049 2 3 -2 9 13635.2 157.071 2 -3 2 -10 29.7214 110.954 2 -3 2 -11 414.621 116.655 2 -3 2 -12 1828.51 77.6921 2 -3 2 -13 38.7219 70.9192 2 -3 2 -14 5590.53 111.701 2 -3 2 -15 4001.27 112.242 2 -3 2 -16 13474.8 142.863 2 -3 2 -17 3238.00 98.8944 2 3 -2 18 33.6419 81.2681 2 3 -2 19 650.594 80.3758 2 3 -2 20 1744.12 85.3168 2 3 -2 21 161.638 79.2125 2 3 -2 22 304.487 115.380 2 3 -2 23 1819.24 80.1819 2 -3 1 24 3044.70 124.792 2 -3 1 23 238.931 72.7231 2 -3 1 22 2946.36 109.085 2 -3 1 21 34.3196 93.7130 2 -3 1 20 2242.54 103.579 2 -3 1 19 2237.40 105.704 2 -3 1 18 3177.53 106.434 2 -3 1 17 149.548 69.0226 2 -3 1 16 3455.88 83.4077 2 -3 1 15 5044.07 89.3934 2 -3 1 14 5249.44 94.3370 2 -3 1 13 10854.5 113.083 2 3 -1 -12 37028.3 434.260 2 3 -1 -11 3401.91 166.256 2 3 -1 -10 298.927 119.770 2 3 -1 -9 1043.70 110.689 2 -3 1 8 848.898 89.6302 2 -3 1 7-18.2605 84.2617 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4194.80 126.162 2 -6 0 20 1112.21 97.1619 2 -6 0 19 294.026 104.167 2 -6 0 18 643.405 89.1436 2 -6 0 17 1987.42 85.5183 2 -6 0 16 8999.06 114.350 2 -6 0 15 629.507 74.1436 2 -6 0 14 129.006 70.9567 2 -6 0 13 960.233 80.2975 2 -6 0 12 113.602 73.9229 2 -6 0 11 260.695 78.0212 2 -6 0 10 7472.14 121.797 2 -6 0 9 633.034 86.8428 2 -6 0 8 6684.50 113.570 2 -6 0 7 359.459 121.340 2 6 0 -6 2467.69 159.008 2 6 0 -5 3615.99 371.015 2 -6 0 -5 2899.09 417.652 2 6 0 6 656.289 280.250 2 6 0 7 1538.51 443.493 2 6 0 8 21874.4 259.449 2 -6 0 -9 4579.98 114.448 2 -6 0 -10 1450.30 96.7332 2 -6 0 -11 332.079 90.8631 2 -6 0 -12 2967.76 103.963 2 -6 0 -13 2658.51 99.1087 2 -6 0 -14 742.092 82.5977 2 -6 0 -15 2735.24 102.468 2 -6 0 -16 6621.16 113.059 2 6 0 17 745.471 71.4927 2 6 0 18 134.700 68.7210 2 -6 -1 18 112.861 64.5011 2 -6 -1 17 1650.32 85.6661 2 -6 -1 16 498.688 82.9189 2 -6 -1 15 3048.59 113.525 2 -6 -1 14 6.52692 82.9905 2 -6 -1 13 920.697 92.3217 2 6 1 -12 327.426 84.4320 2 -6 -1 11 4475.96 121.667 2 6 1 -10 737.633 80.9694 2 6 1 -9 3437.13 99.5493 2 6 1 -8 719.644 146.936 2 -6 -1 5 17518.7 730.866 2 6 1 -3 10023.8 509.261 2 -6 -1 -3 6284.37 554.954 2 6 1 5 7.74093 152.738 2 -6 -1 -6 4670.03 100.555 2 -6 -1 -7 7263.78 112.393 2 -6 -1 -8 1476.61 84.7686 2 -6 -1 -9 937.498 96.7912 2 -6 -1 -10 4947.32 119.421 2 -6 -1 -11 3438.98 107.292 2 -6 -1 -12 1473.09 92.5609 2 -6 -1 -13 1634.91 89.2329 2 -6 -1 -14 663.953 75.7752 2 -6 -1 -15 1052.97 69.7473 2 -6 -1 -16 180.885 112.246 2 6 1 17 2468.73 81.6834 2 -6 -2 18 2479.04 100.035 2 -6 -2 17 111.995 97.2523 2 -6 -2 16 2140.85 136.948 2 -6 -2 15-8.46592 128.015 2 -6 -2 14 34.2388 129.761 2 -6 -2 13 35.9469 143.301 2 -6 -2 12 211.858 100.795 2 -6 -2 -8 3077.60 143.634 2 -6 -2 -9 1221.00 93.6439 2 -6 -2 -10 75.6138 81.2547 2 -6 -2 -11 626.721 81.2295 2 -6 -2 -12 2479.25 88.1942 2 -6 -2 -13 3180.50 84.8799 2 -6 -2 -14 881.648 73.4375 2 -6 -2 -15 98.5752 96.3934 2 -6 -3 16 52.3040 77.1976 2 -6 -3 15 3279.45 130.504 2 6 3 -13 6278.07 188.577 2 6 3 8 177.388 141.179 2 -6 -3 -10 392.240 136.304 2 -6 -3 -11 4645.37 125.092 2 -6 -3 -12-1.37726 79.3237 2 -6 -3 -13 27.5936 65.0460 2 7 -10 6-13.8008 94.4313 2 7 -10 7 3013.43 116.952 2 7 -9 -12 738.583 73.1368 2 7 -9 -11 3538.90 103.723 2 7 -9 -10 543.666 63.8219 2 7 -9 -9 464.509 68.1988 2 7 -9 -8 19.1413 68.8876 2 -7 9 7 466.028 87.2618 2 7 -9 8 5646.63 132.833 2 7 -9 9 706.458 93.9388 2 7 -9 10 779.955 82.9896 2 7 -9 11 43.7394 66.6587 2 7 -8 -15 56.0077 64.7292 2 7 -8 -14 200.828 78.2166 2 7 -8 -13 174.348 88.4285 2 7 -8 -12 2865.85 117.911 2 -7 8 11 472.210 89.0029 2 -7 8 10 202.616 92.4904 2 -7 8 9 122.616 94.7646 2 -7 8 8-31.8545 169.214 2 7 -8 8 130.524 151.244 2 -7 8 -9 38.1824 151.413 2 7 -8 10 472.386 107.808 2 7 -8 11 1595.08 108.412 2 7 -8 12 571.346 92.0398 2 -7 8 -13 6794.75 175.868 2 -7 8 -14 105.838 102.408 2 7 -7 -16 854.282 84.2429 2 7 -7 -15 1217.64 100.816 2 7 -7 -14 1647.54 112.467 2 7 -7 -13 68.6964 105.590 2 -7 7 12 354.990 164.755 2 -7 7 11 560.240 181.433 2 -7 7 -11 91.5462 103.494 2 7 -7 12 2337.51 97.3807 2 7 -7 13 1126.98 83.0519 2 -7 7 -14 1809.71 97.1773 2 -7 7 -15 939.524 82.1063 2 -7 6 18 1148.37 106.833 2 -7 6 17 403.840 68.5132 2 -7 6 16 1067.75 151.059 2 -7 6 15 776.085 158.670 2 -7 6 -13 482.300 144.040 2 -7 6 -14 430.316 101.914 2 -7 6 -15 92.5277 89.5311 2 -7 6 -16 1554.59 69.5750 2 -7 6 -17 672.454 89.4055 2 7 -5 -14 2027.59 383.071 2 7 -5 -11 5964.49 464.565 2 -7 1 19 449.102 83.4041 2 -7 1 18 2367.78 90.0774 2 -7 1 17 169.181 81.9228 2 7 -1 -15 6048.94 194.508 2 7 -1 15 5642.25 126.443 2 7 -1 16 4255.70 83.8680 2 -7 0 17 379.555 90.1313 2 -7 0 16 21.5306 68.5563 2 -7 0 15 11.6156 85.1990 2 -7 0 14 439.730 96.5477 2 7 0 -13 279.158 71.0123 2 7 0 -12 11555.4 150.986 2 -7 0 11 209.514 110.841 2 7 0 -10 10993.5 242.649 2 7 0 -9 977.886 303.258 2 7 0 11 3440.96 114.150 2 -7 0 -12 1807.30 82.9809 2 -7 0 -13 4175.98 87.2675 2 -7 0 -14 18.9530 72.9564 2 7 0 15 147.420 54.6921 2 -7 -1 16-3.38707 92.0909 2 -7 -1 15 526.029 116.023 2 -7 -1 14 4275.47 172.159 2 -7 -1 13 1.43567 129.498 2 -7 -1 12 101.349 141.105 2 -7 -1 11 540.213 109.101 2 7 1 -10 12658.8 156.218 2 7 1 -9 6673.91 133.831 2 7 1 -8 273.439 150.072 2 7 1 5 216.167 151.202 2 7 1 8 2658.32 102.118 2 -7 -1 -9 4590.79 103.336 2 -7 -1 -10 4338.73 96.9173 2 -7 -1 -11 460.758 73.8723 2 -7 -1 -12 607.527 68.9611 2 -7 -1 -13 1678.07 66.5831 2 -7 -2 15 267.885 81.8166 2 -7 -2 14 1005.29 105.312 2 -7 -2 13 5560.35 113.784 2 -7 -2 12 40.9827 88.4354 2 -7 -2 11 21.4083 95.3204 2 -7 -2 10 70.1835 99.0973 2 7 2 -9 1430.07 171.047 2 -7 -2 -6 903.762 92.0956 2 -7 -2 -7 657.669 72.7264 2 -7 -2 -8 573.156 72.5278 2 -7 -2 -9 37.5863 64.8197 2 -7 -2 -10 116.204 61.1878 2 -7 -2 -11 2614.63 77.5183 2 -7 -3 12 3333.15 112.160 2 7 3 7 388.396 125.790 2 7 3 8 2078.77 90.5904 2 8 -10 4 150.854 88.0452 2 8 -9 4 2205.81 139.971 2 8 -9 5 535.334 115.427 2 8 -9 6 1525.06 140.690 2 8 -9 7 1505.24 76.6256 2 8 -9 8 22.4385 72.8799 2 8 -9 9 175.209 88.2248 2 -8 8 13 188.119 67.0625 2 8 -8 -12 1651.11 74.2221 2 8 -8 -11 804.225 73.2991 2 8 -8 -10 840.881 78.4674 2 8 -8 -9 894.690 73.9013 2 8 -8 -8 1552.72 82.1169 2 -8 8 -7 1063.48 113.768 2 8 -8 8 1484.53 90.8077 2 8 -8 9 187.293 75.0941 2 8 -8 10 1174.13 77.5645 2 8 -8 11 328.434 78.3302 2 -8 8 -12 1291.16 109.203 2 -8 7 15 5147.74 80.5545 2 8 -7 -14 1101.88 72.8283 2 8 -7 -13 1511.69 105.549 2 8 -7 -12 155.525 96.0541 2 8 -7 -11 316.543 105.458 2 8 -7 -10 48.4222 105.672 2 -8 7 9-0.05488 154.892 2 -8 7 -7 499.374 163.624 2 -8 7 -8 166.819 85.9449 2 8 -7 9 348.782 62.9544 2 8 -7 10 2742.66 71.7003 2 8 -7 11 280.211 63.3018 2 -8 7 -12 326.431 63.0776 2 -8 7 -13 27.9447 53.5161 2 -8 6 16 1901.92 71.0399 2 -8 6 15 630.687 88.2357 2 8 -6 -14 251.029 96.9016 2 8 -6 -13 3827.03 127.200 2 -8 6 12 367.154 162.658 2 -8 6 -9 3269.50 134.535 2 -8 6 -10 638.172 79.1081 2 -8 6 -11 7408.69 122.652 2 -8 6 -12 244.773 78.5097 2 -8 6 -13 4539.79 94.2826 2 -8 6 -14 104.019 63.4159 2 -8 5 17 2044.66 66.9471 2 -8 5 16 698.828 87.1769 2 -8 5 -11 325.861 172.930 2 -8 5 -12 542.024 109.637 2 -8 5 -13 189.200 76.7577 2 -8 5 -14 2456.79 83.0575 2 8 -5 15 876.055 76.2413 2 -8 0 14 913.415 106.369 2 -8 -1 13 5003.40 135.667 2 -8 -1 12 740.971 79.0725 2 -8 -1 11 34.8172 108.457 2 -8 -1 -9 551.671 114.364 2 -8 -1 -10 1904.75 113.495 2 -8 -2 10 1230.00 96.5805 2 -8 -2 9 518.689 72.2295 2 8 2 -8 1468.38 124.445 2 -8 -2 -6 2273.24 129.548 2 9 -9 4 1363.74 109.904 2 9 -8 -10 24.0323 84.1923 2 9 -8 4 125.592 122.130 2 9 -8 5 205.546 118.985 2 9 -8 6 222.295 115.871 2 9 -8 7 15.0579 99.4089 2 -9 8 -8 801.342 112.571 2 9 -7 -13 4.14310 80.3809 2 -9 7 12 1070.23 78.4865 2 -9 7 11 376.496 80.6308 2 -9 7 10 4178.26 118.231 2 -9 7 9 45.1776 88.9378 2 -9 7 8 54.4715 125.693 2 -9 7 7 1164.72 106.115 2 -9 7 6 6738.13 192.813 2 -9 7 -5 248.742 105.271 2 -9 7 -6 100.425 98.2522 2 9 -7 7 1049.74 71.2104 2 -9 7 -8 161.474 75.0205 2 -9 7 -9 5381.59 117.968 2 -9 7 -10 973.304 80.1241 2 -9 6 14 879.606 58.4436 2 -9 6 13 1376.46 85.7076 2 -9 6 12 851.066 89.5023 2 -9 6 11 28.2098 88.0803 2 -9 6 10 1215.01 146.548 2 -9 6 -6-2.51453 163.069 2 -9 6 -7 28.7581 78.7065 2 -9 6 -8 1437.92 89.0162 2 -9 6 -9-7.46561 91.7398 2 -9 6 -10 4791.60 120.099 2 9 -6 11-5.45042 102.416 2 9 -6 12 18.7334 84.9443 2 -9 5 15 1196.70 69.5668 2 -9 5 14 148.854 60.1120 2 -9 5 13 5066.34 167.335 2 -9 5 -8-12.4295 90.3250 2 9 -5 9 198.553 70.3654 2 9 -5 10 1211.97 72.7378 2 9 -5 11 213.346 76.0748 2 9 -5 12-7.65201 64.6559 2 9 -4 10 119.931 131.730 2 9 -4 11 1435.80 73.2446 2 9 -4 12 749.948 74.5346 2 10 -7 -9 2203.08 106.383 2 10 -6 -10 577.967 98.0040 2 10 -6 -9 609.845 71.5289 2 -10 6 8 418.740 114.200 2 -10 6 -4 54.3636 82.1697 2 -10 6 -5 3281.65 104.313 2 10 -6 6 102.584 104.274 2 10 -6 7 38.9456 89.4309 2 10 -5 -11 1112.71 94.8749 2 -10 5 -5 175.392 85.8005 2 10 -5 6 1371.23 120.909 2 10 -5 7 3068.14 92.1718 2 10 -5 8 19.0063 94.2890 2 -10 4 -6 1153.24 89.2431 2 -10 4 -7-21.5648 57.2207 2 -10 4 -8 424.512 98.0193 2 0 0 0 0.00000 0.00000 0 TITL OCHDKB_twin1_hklf4 in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 8.783773 8.795085 20.444177 90.4500 93.8907 117.3013 ZERR 4.00 0.000368 0.000357 0.000799 0.0034 0.0033 0.0042 LATT 1 SFAC C H N O P UNIT 60.00 64.00 4.00 8.00 4.00 TREF HKLF 5 BASF 0.45788 END ; _shelx_hkl_checksum 21242 _olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount' _olex2_submission_original_sample_id OCHDKB _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 1.365 _oxdiff_exptl_absorpt_empirical_full_min 0.763 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.55361(7) 0.52615(7) 0.33486(2) 0.02380(13) Uani 1 1 d . . . . . P2 P 0.98466(7) 0.91713(7) 0.16532(2) 0.02353(13) Uani 1 1 d . . . . . O3 O 0.9655(2) 0.8711(2) 0.23520(7) 0.0308(3) Uani 1 1 d . . . . . O4 O 0.7954(2) 0.7926(2) 0.05020(7) 0.0312(3) Uani 1 1 d . . . . . O1 O 0.5865(2) 0.5498(2) 0.26452(7) 0.0320(4) Uani 1 1 d . . . . . O2 O 0.6895(2) 0.7144(2) 0.44770(6) 0.0300(3) Uani 1 1 d . . . . . N2 N 0.6767(2) 0.6408(2) 0.13915(8) 0.0256(4) Uani 1 1 d D . . . . H2A H 0.684(3) 0.637(3) 0.1815(9) 0.031 Uiso 1 1 d D U . . . N1 N 0.8398(2) 0.8281(2) 0.35842(8) 0.0260(4) Uani 1 1 d D . . . . H1 H 0.844(3) 0.813(3) 0.3167(9) 0.031 Uiso 1 1 d D U . . . C13 C 0.7112(3) 0.7095(3) 0.38900(9) 0.0237(4) Uani 1 1 d . . . . . C2 C 0.5965(3) 0.3249(3) 0.43341(10) 0.0274(4) Uani 1 1 d . . . . . H2 H 0.600081 0.407557 0.464514 0.033 Uiso 1 1 calc R U . . . C28 C 0.7985(3) 0.7678(3) 0.10946(9) 0.0242(4) Uani 1 1 d . . . . . C1 C 0.5710(3) 0.3439(3) 0.36647(10) 0.0248(4) Uani 1 1 d . . . . . C29 C 0.5206(3) 0.5093(3) 0.10351(10) 0.0286(4) Uani 1 1 d . . . . . H29A H 0.490845 0.559436 0.064545 0.034 Uiso 1 1 calc R U . . . H29B H 0.424383 0.471426 0.132147 0.034 Uiso 1 1 calc R U . . . C8 C 0.2688(3) 0.4388(3) 0.40834(10) 0.0278(4) Uani 1 1 d . . . . . H8 H 0.317101 0.386744 0.437927 0.033 Uiso 1 1 calc R U . . . C22 C 1.1674(3) 0.9085(3) 0.13408(9) 0.0245(4) Uani 1 1 d . . . . . C4 C 0.6099(3) 0.0634(3) 0.40917(12) 0.0363(5) Uani 1 1 d . . . . . H4 H 0.623090 -0.032513 0.423732 0.044 Uiso 1 1 calc R U . . . C7 C 0.3508(3) 0.5138(3) 0.35248(10) 0.0251(4) Uani 1 1 d . . . . . C23 C 1.1827(3) 0.8918(3) 0.06716(10) 0.0267(4) Uani 1 1 d . . . . . H23 H 1.097234 0.890526 0.035750 0.032 Uiso 1 1 calc R U . . . C14 C 0.9765(3) 0.9817(3) 0.39339(10) 0.0297(5) Uani 1 1 d . . . . . H14A H 0.928889 1.014010 0.430511 0.036 Uiso 1 1 calc R U . . . H14B H 1.016839 1.077644 0.363255 0.036 Uiso 1 1 calc R U . . . C18 C 1.0560(3) 1.3648(3) 0.08372(13) 0.0379(5) Uani 1 1 d . . . . . H18 H 1.102347 1.426700 0.046003 0.045 Uiso 1 1 calc R U . . . C9 C 0.1160(3) 0.4409(3) 0.42031(11) 0.0336(5) Uani 1 1 d . . . . . H9 H 0.058873 0.388416 0.457963 0.040 Uiso 1 1 calc R U . . . C24 C 1.3227(3) 0.8771(3) 0.04672(11) 0.0316(5) Uani 1 1 d . . . . . H24 H 1.332188 0.864094 0.001226 0.038 Uiso 1 1 calc R U . . . C3 C 0.6167(3) 0.1852(3) 0.45447(11) 0.0312(5) Uani 1 1 d . . . . . H3 H 0.635178 0.172786 0.500017 0.037 Uiso 1 1 calc R U . . . C21 C 0.9218(3) 1.1869(3) 0.19450(11) 0.0366(5) Uani 1 1 d . . . . . H21 H 0.877190 1.126805 0.232745 0.044 Uiso 1 1 calc R U . . . C27 C 1.2939(3) 0.9108(3) 0.17985(11) 0.0306(5) Uani 1 1 d . . . . . H27 H 1.283704 0.921462 0.225428 0.037 Uiso 1 1 calc R U . . . C16 C 0.9933(3) 1.1215(3) 0.15022(10) 0.0264(4) Uani 1 1 d . . . . . C12 C 0.2780(3) 0.5887(3) 0.30930(11) 0.0335(5) Uani 1 1 d . . . . . H12 H 0.331992 0.637071 0.270620 0.040 Uiso 1 1 calc R U . . . C6 C 0.5652(3) 0.2218(3) 0.32103(11) 0.0324(5) Uani 1 1 d . . . . . H6 H 0.548539 0.234328 0.275386 0.039 Uiso 1 1 calc R U . . . C17 C 1.0612(3) 1.2119(3) 0.09459(10) 0.0303(5) Uani 1 1 d . . . . . H17 H 1.110757 1.168624 0.064307 0.036 Uiso 1 1 calc R U . . . C25 C 1.4491(3) 0.8812(3) 0.09215(12) 0.0355(5) Uani 1 1 d . . . . . H25 H 1.545578 0.872765 0.077713 0.043 Uiso 1 1 calc R U . . . C10 C 0.0462(3) 0.5182(3) 0.37815(12) 0.0373(5) Uani 1 1 d . . . . . H10 H -0.057436 0.520214 0.387298 0.045 Uiso 1 1 calc R U . . . C26 C 1.4348(3) 0.8976(4) 0.15874(12) 0.0380(6) Uani 1 1 d . . . . . H26 H 1.521261 0.899869 0.189877 0.046 Uiso 1 1 calc R U . . . C30 C 0.5416(4) 0.3564(3) 0.08172(13) 0.0419(6) Uani 1 1 d . . . . . H30A H 0.639792 0.393900 0.054836 0.063 Uiso 1 1 calc R U . . . H30B H 0.437083 0.275107 0.055825 0.063 Uiso 1 1 calc R U . . . H30C H 0.561706 0.300665 0.120319 0.063 Uiso 1 1 calc R U . . . C15 C 1.1271(3) 0.9556(3) 0.41922(13) 0.0411(6) Uani 1 1 d . . . . . H15A H 1.181464 0.934100 0.382369 0.062 Uiso 1 1 calc R U . . . H15B H 1.087133 0.857206 0.447399 0.062 Uiso 1 1 calc R U . . . H15C H 1.210790 1.058422 0.444701 0.062 Uiso 1 1 calc R U . . . C19 C 0.9834(4) 1.4273(3) 0.12782(14) 0.0431(6) Uani 1 1 d . . . . . H19 H 0.980164 1.532211 0.120093 0.052 Uiso 1 1 calc R U . . . C20 C 0.9156(4) 1.3391(4) 0.18299(14) 0.0467(7) Uani 1 1 d . . . . . H20 H 0.865087 1.382440 0.212812 0.056 Uiso 1 1 calc R U . . . C11 C 0.1266(4) 0.5930(4) 0.32249(12) 0.0405(6) Uani 1 1 d . . . . . H11 H 0.078750 0.646747 0.293580 0.049 Uiso 1 1 calc R U . . . C5 C 0.5840(4) 0.0817(3) 0.34288(12) 0.0393(6) Uani 1 1 d . . . . . H5 H 0.578943 -0.002140 0.312029 0.047 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0242(3) 0.0234(3) 0.0209(2) 0.00465(18) 0.00453(19) 0.0081(2) P2 0.0201(3) 0.0278(3) 0.0215(2) 0.00436(18) 0.00515(18) 0.0094(2) O3 0.0269(8) 0.0390(9) 0.0233(7) 0.0052(6) 0.0047(6) 0.0120(7) O4 0.0261(8) 0.0412(10) 0.0224(7) 0.0070(6) 0.0045(5) 0.0118(7) O1 0.0344(9) 0.0313(8) 0.0229(7) 0.0042(6) 0.0062(6) 0.0083(7) O2 0.0350(9) 0.0284(8) 0.0231(7) 0.0037(6) 0.0072(6) 0.0107(7) N2 0.0246(9) 0.0274(9) 0.0225(8) 0.0045(6) 0.0043(6) 0.0097(8) N1 0.0265(9) 0.0259(9) 0.0230(8) 0.0021(7) 0.0049(7) 0.0094(8) C13 0.0252(10) 0.0213(10) 0.0243(9) 0.0038(7) 0.0035(7) 0.0101(8) C2 0.0241(11) 0.0260(11) 0.0303(10) 0.0043(8) 0.0053(8) 0.0096(9) C28 0.0212(10) 0.0277(11) 0.0239(9) 0.0038(7) 0.0051(7) 0.0109(9) C1 0.0222(10) 0.0217(10) 0.0298(10) 0.0049(8) 0.0063(8) 0.0087(9) C29 0.0228(11) 0.0288(12) 0.0291(10) 0.0039(8) 0.0040(8) 0.0071(9) C8 0.0272(11) 0.0253(11) 0.0300(10) 0.0045(8) 0.0036(8) 0.0109(9) C22 0.0213(10) 0.0223(10) 0.0293(10) 0.0057(8) 0.0048(8) 0.0090(9) C4 0.0321(13) 0.0260(12) 0.0552(14) 0.0095(10) 0.0102(10) 0.0160(11) C7 0.0232(10) 0.0237(11) 0.0274(10) 0.0040(8) 0.0028(8) 0.0098(9) C23 0.0233(11) 0.0262(11) 0.0294(10) 0.0046(8) 0.0048(8) 0.0101(9) C14 0.0265(11) 0.0243(11) 0.0323(10) 0.0008(8) 0.0047(8) 0.0062(9) C18 0.0318(13) 0.0290(13) 0.0507(13) 0.0074(10) 0.0009(10) 0.0124(11) C9 0.0283(12) 0.0326(13) 0.0382(11) 0.0038(9) 0.0101(9) 0.0116(10) C24 0.0327(12) 0.0294(12) 0.0354(11) 0.0053(9) 0.0122(9) 0.0154(10) C3 0.0250(11) 0.0306(12) 0.0377(11) 0.0098(9) 0.0053(9) 0.0121(10) C21 0.0338(13) 0.0408(14) 0.0362(12) -0.0043(10) 0.0056(9) 0.0177(12) C27 0.0266(12) 0.0347(12) 0.0315(10) 0.0081(9) 0.0056(8) 0.0145(10) C16 0.0233(11) 0.0268(11) 0.0282(10) 0.0004(8) 0.0021(8) 0.0109(9) C12 0.0342(13) 0.0359(13) 0.0313(11) 0.0089(9) 0.0020(9) 0.0170(11) C6 0.0315(12) 0.0314(12) 0.0327(11) 0.0018(9) 0.0082(9) 0.0124(10) C17 0.0266(11) 0.0312(12) 0.0327(11) 0.0041(9) 0.0042(8) 0.0125(10) C25 0.0286(12) 0.0375(13) 0.0492(13) 0.0122(10) 0.0146(10) 0.0212(11) C10 0.0261(12) 0.0376(14) 0.0495(13) -0.0015(10) 0.0006(10) 0.0161(11) C26 0.0294(13) 0.0486(15) 0.0424(12) 0.0124(11) 0.0042(10) 0.0232(12) C30 0.0375(14) 0.0314(13) 0.0518(14) -0.0037(10) -0.0050(11) 0.0126(12) C15 0.0298(13) 0.0351(14) 0.0521(14) -0.0048(10) -0.0028(10) 0.0105(11) C19 0.0372(14) 0.0284(13) 0.0667(17) -0.0029(11) -0.0042(12) 0.0188(11) C20 0.0448(16) 0.0444(16) 0.0568(16) -0.0145(12) 0.0008(12) 0.0263(14) C11 0.0396(14) 0.0406(15) 0.0453(13) 0.0038(11) -0.0069(10) 0.0233(12) C5 0.0414(15) 0.0310(13) 0.0476(13) -0.0004(10) 0.0127(11) 0.0174(12) 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' N N 0.0311 0.0180 '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' P P 0.2955 0.4335 '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 4 0 5 0.0415 1 1 -5 0.1409 -1 -1 5 0.1409 -4 -1 -4 0.0525 -1 1 5 0.1046 -2 -2 -5 0.0399 0 0 1 0.1315 1 -1 -1 0.0791 3 -5 -1 0.0525 -3 5 1 0.0362 2 3 5 0.0297 1 0 -5 0.1352 -4 0 -5 0.0415 5 -3 3 0.0485 0 1 -5 0.1340 1 -5 -4 0.0394 -3 0 -5 0.0306 -4 5 2 0.0377 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 O1 P1 C13 112.87(9) . . ? O1 P1 C1 112.90(9) . . ? O1 P1 C7 113.28(10) . . ? C1 P1 C13 104.19(9) . . ? C7 P1 C13 103.14(10) . . ? C7 P1 C1 109.66(10) . . ? O3 P2 C28 112.84(9) . . ? O3 P2 C22 112.48(9) . . ? O3 P2 C16 113.41(10) . . ? C22 P2 C28 104.53(9) . . ? C16 P2 C28 103.06(10) . . ? C16 P2 C22 109.77(10) . . ? C28 N2 H2A 120.2(18) . . ? C28 N2 C29 122.65(17) . . ? C29 N2 H2A 117.0(18) . . ? C13 N1 H1 118.7(18) . . ? C13 N1 C14 122.09(17) . . ? C14 N1 H1 119.2(18) . . ? O2 C13 P1 119.66(16) . . ? O2 C13 N1 125.83(19) . . ? N1 C13 P1 114.50(14) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C3 C2 C1 119.9(2) . . ? O4 C28 P2 119.85(16) . . ? O4 C28 N2 125.7(2) . . ? N2 C28 P2 114.45(14) . . ? C2 C1 P1 122.72(16) . . ? C2 C1 C6 119.8(2) . . ? C6 C1 P1 117.46(16) . . ? N2 C29 H29A 109.2 . . ? N2 C29 H29B 109.2 . . ? N2 C29 C30 112.24(19) . . ? H29A C29 H29B 107.9 . . ? C30 C29 H29A 109.2 . . ? C30 C29 H29B 109.2 . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C9 C8 C7 119.4(2) . . ? C23 C22 P2 122.91(16) . . ? C27 C22 P2 117.34(15) . . ? C27 C22 C23 119.7(2) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C5 C4 C3 120.0(2) . . ? C8 C7 P1 122.59(17) . . ? C12 C7 P1 117.68(17) . . ? C12 C7 C8 119.7(2) . . ? C22 C23 H23 120.1 . . ? C24 C23 C22 119.8(2) . . ? C24 C23 H23 120.1 . . ? N1 C14 H14A 109.1 . . ? N1 C14 H14B 109.1 . . ? N1 C14 C15 112.61(19) . . ? H14A C14 H14B 107.8 . . ? C15 C14 H14A 109.1 . . ? C15 C14 H14B 109.1 . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C19 C18 C17 120.0(2) . . ? C8 C9 H9 119.6 . . ? C10 C9 C8 120.7(2) . . ? C10 C9 H9 119.6 . . ? C23 C24 H24 119.8 . . ? C25 C24 C23 120.5(2) . . ? C25 C24 H24 119.8 . . ? C2 C3 C4 120.2(2) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C16 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C20 C21 C16 120.3(2) . . ? C22 C27 H27 120.0 . . ? C26 C27 C22 120.0(2) . . ? C26 C27 H27 120.0 . . ? C21 C16 P2 118.02(18) . . ? C21 C16 C17 119.5(2) . . ? C17 C16 P2 122.39(17) . . ? C7 C12 H12 119.8 . . ? C11 C12 C7 120.4(2) . . ? C11 C12 H12 119.8 . . ? C1 C6 H6 120.2 . . ? C5 C6 C1 119.7(2) . . ? C5 C6 H6 120.2 . . ? C18 C17 C16 119.8(2) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C24 C25 H25 120.0 . . ? C24 C25 C26 120.1(2) . . ? C26 C25 H25 120.0 . . ? C9 C10 H10 119.8 . . ? C9 C10 C11 120.3(2) . . ? C11 C10 H10 119.8 . . ? C27 C26 H26 120.0 . . ? C25 C26 C27 119.9(2) . . ? C25 C26 H26 120.0 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 C19 H19 119.6 . . ? C20 C19 C18 120.8(2) . . ? C20 C19 H19 119.6 . . ? C21 C20 H20 120.2 . . ? C19 C20 C21 119.5(2) . . ? C19 C20 H20 120.2 . . ? C12 C11 H11 120.3 . . ? C10 C11 C12 119.4(2) . . ? C10 C11 H11 120.3 . . ? C4 C5 C6 120.5(2) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? 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 P1 O1 1.4835(14) . ? P1 C13 1.860(2) . ? P1 C1 1.799(2) . ? P1 C7 1.796(2) . ? P2 O3 1.4874(14) . ? P2 C28 1.859(2) . ? P2 C22 1.800(2) . ? P2 C16 1.794(2) . ? O4 C28 1.233(2) . ? O2 C13 1.231(2) . ? N2 H2A 0.866(18) . ? N2 C28 1.328(3) . ? N2 C29 1.464(3) . ? N1 H1 0.869(18) . ? N1 C13 1.334(3) . ? N1 C14 1.469(3) . ? C2 H2 0.9500 . ? C2 C1 1.396(3) . ? C2 C3 1.388(3) . ? C1 C6 1.396(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C29 C30 1.507(3) . ? C8 H8 0.9500 . ? C8 C7 1.395(3) . ? C8 C9 1.389(3) . ? C22 C23 1.397(3) . ? C22 C27 1.395(3) . ? C4 H4 0.9500 . ? C4 C3 1.388(3) . ? C4 C5 1.382(4) . ? C7 C12 1.393(3) . ? C23 H23 0.9500 . ? C23 C24 1.386(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C14 C15 1.506(3) . ? C18 H18 0.9500 . ? C18 C17 1.385(3) . ? C18 C19 1.383(4) . ? C9 H9 0.9500 . ? C9 C10 1.379(4) . ? C24 H24 0.9500 . ? C24 C25 1.385(3) . ? C3 H3 0.9500 . ? C21 H21 0.9500 . ? C21 C16 1.395(3) . ? C21 C20 1.386(4) . ? C27 H27 0.9500 . ? C27 C26 1.392(3) . ? C16 C17 1.397(3) . ? C12 H12 0.9500 . ? C12 C11 1.392(4) . ? C6 H6 0.9500 . ? C6 C5 1.389(4) . ? C17 H17 0.9500 . ? C25 H25 0.9500 . ? C25 C26 1.388(3) . ? C10 H10 0.9500 . ? C10 C11 1.386(4) . ? C26 H26 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C19 H19 0.9500 . ? C19 C20 1.382(4) . ? C20 H20 0.9500 . ? C11 H11 0.9500 . ? C5 H5 0.9500 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N2 H2A O1 0.866(18) 1.95(2) 2.750(2) 152(3) . yes N1 H1 O3 0.869(18) 1.98(2) 2.778(2) 151(2) . yes 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 P1 C1 C6 C5 177.81(19) . . . . ? P1 C7 C12 C11 -175.88(19) . . . . ? P2 C22 C23 C24 -176.68(17) . . . . ? P2 C22 C27 C26 177.5(2) . . . . ? P2 C16 C17 C18 176.51(18) . . . . ? O3 P2 C28 O4 178.49(17) . . . . ? O3 P2 C28 N2 -0.9(2) . . . . ? O3 P2 C22 C23 158.94(18) . . . . ? O3 P2 C22 C27 -18.0(2) . . . . ? O3 P2 C16 C21 -22.8(2) . . . . ? O3 P2 C16 C17 160.24(18) . . . . ? O1 P1 C13 O2 173.04(17) . . . . ? O1 P1 C13 N1 -5.93(19) . . . . ? O1 P1 C1 C2 160.36(17) . . . . ? O1 P1 C1 C6 -17.0(2) . . . . ? O1 P1 C7 C8 158.78(18) . . . . ? O1 P1 C7 C12 -23.7(2) . . . . ? C13 P1 C1 C2 37.5(2) . . . . ? C13 P1 C1 C6 -139.82(18) . . . . ? C13 P1 C7 C8 -78.9(2) . . . . ? C13 P1 C7 C12 98.63(19) . . . . ? C13 N1 C14 C15 90.4(3) . . . . ? C2 C1 C6 C5 0.4(3) . . . . ? C28 P2 C22 C23 36.2(2) . . . . ? C28 P2 C22 C27 -140.82(18) . . . . ? C28 P2 C16 C21 99.49(19) . . . . ? C28 P2 C16 C17 -77.4(2) . . . . ? C28 N2 C29 C30 90.8(2) . . . . ? C1 P1 C13 O2 -64.13(19) . . . . ? C1 P1 C13 N1 116.91(16) . . . . ? C1 P1 C7 C8 31.7(2) . . . . ? C1 P1 C7 C12 -150.84(19) . . . . ? C1 C2 C3 C4 -0.6(3) . . . . ? C1 C6 C5 C4 -0.6(4) . . . . ? C29 N2 C28 P2 -179.50(15) . . . . ? C29 N2 C28 O4 1.2(3) . . . . ? C8 C7 C12 C11 1.7(4) . . . . ? C8 C9 C10 C11 1.0(4) . . . . ? C22 P2 C28 O4 -59.0(2) . . . . ? C22 P2 C28 N2 121.64(16) . . . . ? C22 P2 C16 C21 -149.59(18) . . . . ? C22 P2 C16 C17 33.5(2) . . . . ? C22 C23 C24 C25 -0.9(3) . . . . ? C22 C27 C26 C25 -0.3(4) . . . . ? C7 P1 C13 O2 50.42(19) . . . . ? C7 P1 C13 N1 -128.55(16) . . . . ? C7 P1 C1 C2 -72.3(2) . . . . ? C7 P1 C1 C6 110.34(18) . . . . ? C7 C8 C9 C10 -0.9(4) . . . . ? C7 C12 C11 C10 -1.7(4) . . . . ? C23 C22 C27 C26 0.4(3) . . . . ? C23 C24 C25 C26 0.9(4) . . . . ? C14 N1 C13 P1 -179.83(16) . . . . ? C14 N1 C13 O2 1.3(3) . . . . ? C18 C19 C20 C21 0.6(4) . . . . ? C9 C8 C7 P1 177.04(17) . . . . ? C9 C8 C7 C12 -0.4(3) . . . . ? C9 C10 C11 C12 0.3(4) . . . . ? C24 C25 C26 C27 -0.3(4) . . . . ? C3 C2 C1 P1 -177.06(17) . . . . ? C3 C2 C1 C6 0.2(3) . . . . ? C3 C4 C5 C6 0.3(4) . . . . ? C21 C16 C17 C18 -0.4(3) . . . . ? C27 C22 C23 C24 0.2(3) . . . . ? C16 P2 C28 O4 55.8(2) . . . . ? C16 P2 C28 N2 -123.60(17) . . . . ? C16 P2 C22 C23 -73.8(2) . . . . ? C16 P2 C22 C27 109.23(18) . . . . ? C16 C21 C20 C19 -1.1(4) . . . . ? C17 C18 C19 C20 0.1(4) . . . . ? C19 C18 C17 C16 -0.2(4) . . . . ? C20 C21 C16 P2 -176.0(2) . . . . ? C20 C21 C16 C17 1.0(4) . . . . ? C5 C4 C3 C2 0.4(4) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.5320(9) 2 0.4680(9) 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 3.9986 0.0021 5.0009 -0.0908 0.8786 -0.1958 0.9991 0.9988 -5.0012 0.0421 0.1854 0.4496 -0.9991 -0.9988 5.0012 -0.0421 -0.1854 -0.4496 -3.9985 -1.0019 -4.0009 -0.0457 -0.9690 0.0673 -0.9992 1.0014 5.0018 0.2582 0.0428 -0.3335 -1.9994 -2.0019 -5.0018 -0.2890 -0.7269 0.1580 0.0001 0.0003 1.0003 0.0137 0.0237 -0.0705 0.9995 -1.0002 -1.0007 -0.2036 0.0521 0.0516 2.9988 -5.0002 -1.0022 -0.8836 -0.0244 -0.1025 -2.9988 5.0002 1.0022 0.8836 0.0244 0.1025 1.9994 3.0020 5.0021 0.4392 0.8410 -0.0999 0.9991 -0.0013 -5.0015 -0.1080 0.0713 0.3916 -3.9986 -0.0021 -5.0009 0.0908 -0.8786 0.1958 4.9982 -2.9986 2.9993 -0.6083 0.6788 -0.1899 -0.0005 0.9986 -5.0011 0.0819 -0.0046 0.4105 0.9995 -5.0014 -4.0028 -0.8451 -0.4755 0.0307 -2.9991 -0.0019 -5.0010 0.0510 -0.6886 0.2350 -3.9983 5.0003 2.0026 0.9371 -0.1419 -0.0072