#------------------------------------------------------------------------------ #$Date: 2021-12-07 05:41:24 +0200 (Tue, 07 Dec 2021) $ #$Revision: 271198 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/10/7061040.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_7061040 loop_ _publ_author_name 'Bhuin, Shouvik' 'Bhattacharya, Suman' 'Chakravarty, Manab' _publ_section_title ; Acceptor--donor--acceptor-linked triphenylamine and phenothiazine motifs as cousin molecules: the methyl effect on stimuli-responsiveness, crystallochromism, and dual-state emission ; _journal_issue 45 _journal_name_full 'New Journal of Chemistry' _journal_page_first 21236 _journal_page_last 21247 _journal_paper_doi 10.1039/D1NJ04190H _journal_volume 45 _journal_year 2021 _chemical_formula_moiety 'C26 H24 N4 S' _chemical_formula_sum 'C26 H24 N4 S' _chemical_formula_weight 424.55 _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 direct _audit_block_doi 10.5517/ccdc.csd.cc26jlkx _audit_creation_date 2020-05-23 _audit_creation_method ; Olex2 1.3-alpha (compiled 2020.05.07 svn.rd67b107b for OlexSys, GUI svn.r6105) ; _audit_update_record ; 2020-10-31 deposited with the CCDC. 2021-10-22 downloaded from the CCDC. ; _cell_angle_alpha 91.003(3) _cell_angle_beta 95.825(4) _cell_angle_gamma 106.344(4) _cell_formula_units_Z 4 _cell_length_a 8.9131(4) _cell_length_b 11.8184(4) _cell_length_c 21.8914(9) _cell_measurement_reflns_used 6097 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 78.7250 _cell_measurement_theta_min 3.9070 _cell_volume 2198.83(16) _computing_cell_refinement 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3-alpha (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-alpha (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2014/7 (Sheldrick, 2015)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _diffrn_ambient_temperature 293 _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 5.8140 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.976 _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 -69.00 -42.00 0.50 2.45 -- 0.00 -57.00-180.00 54 2 \w -44.00 -16.00 0.50 2.45 -- 0.00 -37.00 -30.00 56 3 \w -89.00 -35.00 0.50 2.45 -- 0.00 -57.00 60.00 108 4 \w -10.00 16.00 0.50 2.45 -- 0.00 -57.00-180.00 52 5 \w -6.00 19.00 0.50 2.45 -- 0.00 -37.00 -30.00 50 6 \w -19.00 88.00 0.50 2.45 -- 0.00 37.00 -60.00 214 7 \w -31.00 22.00 0.50 2.45 -- 0.00 -57.00 60.00 106 8 \w -18.00 85.00 0.50 2.45 -- 0.00 37.00 150.00 206 9 \w -33.00 -6.00 0.50 2.45 -- 0.00 -77.00 -60.00 54 10 \w 55.00 139.00 0.50 9.80 -- 107.20 -82.00-180.00 168 11 \w 39.00 131.00 0.50 9.80 -- 107.20 -61.00 -30.00 184 12 \w 100.00 126.00 0.50 9.80 -- 107.20 -82.00 -60.00 52 13 \w 27.00 133.00 0.50 9.80 -- 107.20 -15.00-180.00 212 14 \w 96.00 123.00 0.50 9.80 -- 107.20 -82.00-120.00 54 15 \w 80.00 106.00 0.50 9.80 -- 107.20 -45.00 60.00 52 16 \w 87.00 188.00 0.50 9.80 -- 107.20 45.00 150.00 202 17 \w 26.00 126.00 0.50 9.80 -- 107.20 -30.00-150.00 200 18 \w 21.00 116.00 0.50 9.80 -- 107.20 -82.00 0.00 190 19 \w 50.00 112.00 0.50 9.80 -- 107.20 -82.00 -30.00 124 20 \w 50.00 130.00 0.50 9.80 -- 107.20 -61.00-180.00 160 21 \w 93.00 196.00 0.50 9.80 -- 107.20 45.00-180.00 206 22 \w 19.00 139.00 0.50 9.80 -- 107.20 -82.00 90.00 240 23 \w 94.00 185.00 0.50 9.80 -- 107.20 30.00-150.00 182 24 \w 19.00 110.00 0.50 9.80 -- 107.20 -61.00 90.00 182 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC12 (RINC): Kappa dual home/near' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0927098000 _diffrn_orient_matrix_UB_12 -0.0275431000 _diffrn_orient_matrix_UB_13 -0.0644160000 _diffrn_orient_matrix_UB_21 -0.1130728000 _diffrn_orient_matrix_UB_22 -0.1102448000 _diffrn_orient_matrix_UB_23 0.0237028000 _diffrn_orient_matrix_UB_31 -0.1070843000 _diffrn_orient_matrix_UB_32 0.0747238000 _diffrn_orient_matrix_UB_33 0.0174455000 _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 0.0321 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.976 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 10060 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.976 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 80.047 _diffrn_reflns_theta_min 3.902 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'Rigaku (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 1.458 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.81481 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear yellowish brown' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier yellowish _exptl_crystal_colour_primary brown _exptl_crystal_density_diffrn 1.282 _exptl_crystal_description block _exptl_crystal_F_000 896 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.785 _refine_diff_density_min -0.984 _refine_diff_density_rms 0.085 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 562 _refine_ls_number_reflns 10060 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.061 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0671 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1415P)^2^+0.4708P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1872 _refine_ls_wR_factor_ref 0.1933 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8733 _reflns_number_total 10060 _reflns_threshold_expression 'I > 2\s(I)' _twin_special_details ; Component 2 rotated by -179.9674\% around [-0.00 0.00 1.00] (reciprocal) or [0.27 0.09 0.96] (direct) ; _cod_data_source_file d1nj04190h2.cif _cod_data_source_block exp_530_ptz-cnc_twin1_hklf4 _cod_depositor_comments 'Adding full bibliography for 7061040--7061042.cif.' _cod_original_cell_volume 2198.84(16) _cod_database_code 7061040 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula 'C12 H12 N2 O2 S1' _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 0.868 _shelx_estimated_absorpt_t_min 0.759 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Others Sof(C49B)=Sof(H49A)=Sof(H49B)=Sof(C50B)=Sof(H50A)=Sof(H50B)=Sof(C48B)= Sof(H48A)=Sof(H48B)=Sof(C51B)=Sof(H51A)=Sof(H51B)=Sof(C52B)=Sof(H52A)= Sof(H52B)=Sof(H52C)=1-FVAR(1) Sof(C48A)=Sof(H48C)=Sof(H48D)=Sof(C49A)=Sof(H49C)=Sof(H49D)=Sof(C50A)= Sof(H50C)=Sof(H50D)=Sof(C51A)=Sof(H51C)=Sof(H51D)=Sof(C52A)=Sof(H52D)= Sof(H52E)=Sof(H52F)=FVAR(1) 3.a Rotating group: N5(H5A,H5B), N37(H37A,H37B) 3.b Secondary CH2 refined with riding coordinates: C22(H22A,H22B), C49B(H49A,H49B), C24(H24A,H24B), C50B(H50A,H50B), C48B(H48A, H48B), C23(H23A,H23B), C25(H25A,H25B), C51B(H51A,H51B), C48A(H48C,H48D), C49A(H49C,H49D), C50A(H50C,H50D), C51A(H51C,H51D) 3.c Aromatic/amide H refined with riding coordinates: C15(H15), C5(H5), C31(H31), C11(H11), C14(H14), C38(H38), C41(H41), C37(H37), C21(H21), C18(H18), C19(H19), C43(H43), C46(H46), C20(H20), C45(H45), C44(H44) 3.d Idealised Me refined as rotating group: C7(H7A,H7B,H7C), C33(H33A,H33B,H33C), C26(H26A,H26B,H26C), C52B(H52A,H52B, H52C), C52A(H52D,H52E,H52F) ; _shelx_res_file ; exp_530_ptz-cnc_twin1_hklf4.res created by SHELXL-2014/7 TITL exp_530_PTZ-CNC_twin1_hklf4 in P-1 #2 REM reset to P-1 #2 CELL 1.54184 8.913142 11.818425 21.891382 91.0025 95.8254 106.3444 ZERR 4 0.000368 0.000447 0.000922 0.0033 0.0035 0.0035 LATT 1 SFAC C H N S UNIT 104 96 16 4 L.S. 10 0 0 PLAN 4 SIZE 0.2 0.1 0.1 TEMP 19.85 CONF BOND MORE -1 BOND $H fmap 2 53 acta OMIT 3 -2 1 OMIT 4 -1 -27 OMIT -3 4 16 REM REM REM WGHT 0.141500 0.470800 FVAR 1.83875 0.54370 S1 4 0.278377 -0.178665 0.228515 11.00000 0.02359 0.03414 = 0.03500 -0.00855 0.00687 -0.00029 S2 4 1.034622 0.362413 0.057612 11.00000 0.05132 0.03050 = 0.03637 0.00886 -0.00299 -0.00381 N1 3 0.591934 -0.017018 0.272596 11.00000 0.01811 0.02082 = 0.03178 0.00163 0.00707 0.00158 N2 3 -0.050873 -0.254778 0.402376 11.00000 0.03052 0.02540 = 0.03307 0.00412 0.00610 0.00860 N3 3 -0.365321 0.155175 0.511811 11.00000 0.02485 0.02841 = 0.03618 -0.00044 0.00760 0.00620 C16 1 0.594000 -0.134147 0.261468 11.00000 0.02779 0.02170 = 0.02659 0.00503 0.00909 0.00692 N5 3 -0.287868 -0.094272 0.453265 11.00000 0.02396 0.02023 = 0.03788 0.00496 0.01263 0.00343 AFIX 7 H5A 2 -0.256530 -0.149546 0.470802 11.00000 -1.20000 H5B 2 -0.339459 -0.065985 0.477784 11.00000 -1.20000 AFIX 0 C15 1 0.376090 0.105164 0.381568 11.00000 0.02230 0.02204 = 0.02538 0.00259 0.00401 0.00503 AFIX 43 H15 2 0.396872 0.165250 0.411933 11.00000 -1.20000 AFIX 0 C5 1 0.096398 0.174910 0.408796 11.00000 0.02061 0.02254 = 0.02971 0.00435 0.00630 0.00412 AFIX 43 H5 2 0.179598 0.234925 0.397269 11.00000 -1.20000 AFIX 0 N8 3 0.924685 0.498610 0.278546 11.00000 0.03179 0.03226 = 0.04442 -0.00286 0.00116 0.01273 C32 1 1.487786 0.443386 0.362306 11.00000 0.02357 0.01959 = 0.03093 0.00545 0.00710 0.00298 C6 1 -0.020379 0.204570 0.437595 11.00000 0.02145 0.02252 = 0.02596 0.00340 0.00361 0.00494 C1 1 -0.148128 0.113458 0.452852 11.00000 0.01909 0.02224 = 0.02545 0.00211 0.00494 0.00528 C8 1 -0.266671 0.139130 0.485434 11.00000 0.02263 0.01814 = 0.02941 0.00196 0.00304 0.00464 C31 1 1.400647 0.373996 0.311999 11.00000 0.02600 0.01774 = 0.03291 0.00117 0.00652 0.00347 AFIX 43 H31 2 1.439745 0.317587 0.294314 11.00000 -1.20000 AFIX 0 C2 1 -0.161314 -0.007475 0.439821 11.00000 0.01957 0.02052 = 0.02414 0.00424 0.00529 0.00200 C13 1 0.472721 0.001302 0.304927 11.00000 0.02099 0.02164 = 0.02869 0.00641 0.00653 0.00585 C28 1 1.282161 0.544978 0.365461 11.00000 0.02669 0.01647 = 0.02802 0.00401 0.00813 0.00349 N17 3 1.582842 0.652260 0.485223 11.00000 0.03468 0.01982 = 0.03646 0.00252 0.00165 0.00404 C10 1 0.221985 0.032839 0.367060 11.00000 0.01949 0.02051 = 0.02538 0.00423 0.00500 0.00482 C4 1 0.092298 0.057124 0.396641 11.00000 0.01940 0.02275 = 0.02447 0.00352 0.00261 0.00499 C11 1 0.196336 -0.058569 0.321939 11.00000 0.01910 0.02013 = 0.03033 0.00131 0.00552 0.00242 AFIX 43 H11 2 0.096001 -0.110273 0.312829 11.00000 -1.20000 AFIX 0 C34 1 1.513527 0.597494 0.441789 11.00000 0.02371 0.01987 = 0.03475 0.00426 0.00646 0.00360 C9 1 -0.042165 -0.156071 0.406277 11.00000 0.02163 0.02305 = 0.02661 0.00268 0.00458 0.00510 C3 1 -0.036378 -0.033500 0.413101 11.00000 0.01854 0.01968 = 0.02559 0.00367 0.00555 0.00361 C36 1 1.171543 0.311937 0.232281 11.00000 0.02315 0.02211 = 0.03059 0.00351 0.00606 0.00471 C30 1 1.255930 0.386491 0.287190 11.00000 0.02807 0.01696 = 0.02699 0.00664 0.00856 0.00437 C12 1 0.318151 -0.073079 0.290704 11.00000 0.02095 0.02305 = 0.02971 0.00286 0.00396 0.00250 C22 1 0.736677 0.078961 0.270169 11.00000 0.01903 0.02352 = 0.03489 -0.00021 0.00795 -0.00022 AFIX 23 H22A 2 0.806496 0.051335 0.246316 11.00000 -1.20000 H22B 2 0.789161 0.099767 0.311538 11.00000 -1.20000 AFIX 0 C14 1 0.498421 0.088562 0.351311 11.00000 0.01981 0.01833 = 0.02667 0.00181 0.00310 0.00242 AFIX 43 H14 2 0.599985 0.137019 0.362363 11.00000 -1.20000 AFIX 0 C39 1 1.021074 0.166973 0.125460 11.00000 0.02746 0.02266 = 0.02885 0.00072 0.00391 0.00141 C38 1 1.076965 0.119479 0.178675 11.00000 0.02752 0.02050 = 0.03435 0.00190 0.00723 0.00286 AFIX 43 H38 2 1.061815 0.038417 0.179606 11.00000 -1.20000 AFIX 0 C35 1 1.045213 0.484808 0.292485 11.00000 0.03088 0.02079 = 0.03261 0.00101 0.00553 0.00589 C29 1 1.197151 0.471805 0.314526 11.00000 0.02389 0.01913 = 0.02954 0.00246 0.00491 0.00278 N33 3 0.946112 0.097645 0.073102 11.00000 0.03374 0.02413 = 0.03224 -0.00028 0.00397 0.00180 C17 1 0.453437 -0.220785 0.241163 11.00000 0.02952 0.02428 = 0.03293 0.00126 0.01258 0.00369 C40 1 1.052529 0.291087 0.126663 11.00000 0.03590 0.02156 = 0.03317 0.00427 0.00118 0.00119 C41 1 1.119064 0.360504 0.179720 11.00000 0.03366 0.01667 = 0.03347 0.00285 0.00248 0.00343 AFIX 43 H41 2 1.128754 0.440956 0.180155 11.00000 -1.20000 AFIX 0 N37 3 1.224744 0.626868 0.391876 11.00000 0.02786 0.02425 = 0.03749 -0.00235 0.00365 0.00674 AFIX 7 H37A 2 1.136319 0.592514 0.405217 11.00000 -1.20000 H37B 2 1.290924 0.663107 0.422225 11.00000 -1.20000 AFIX 0 C27 1 1.427408 0.527807 0.389183 11.00000 0.02283 0.02115 = 0.02628 0.00359 0.00484 0.00169 C37 1 1.154086 0.191132 0.229678 11.00000 0.02867 0.02159 = 0.02868 0.00424 0.00525 0.00451 AFIX 43 H37 2 1.195312 0.157567 0.263086 11.00000 -1.20000 AFIX 0 PART 2 C49B 1 0.784033 -0.098020 0.104394 -21.00000 0.01723 AFIX 23 H49A 2 0.809926 -0.076517 0.147951 -21.00000 -1.20000 H49B 2 0.688728 -0.077173 0.090696 -21.00000 -1.20000 AFIX 0 PART 0 C21 1 0.731247 -0.168717 0.271361 11.00000 0.03666 0.03406 = 0.03338 0.00354 0.00647 0.01618 AFIX 43 H21 2 0.825061 -0.113164 0.286271 11.00000 -1.20000 AFIX 0 C7 1 -0.008604 0.331940 0.451731 11.00000 0.02747 0.02034 = 0.03683 0.00511 0.00874 0.00505 AFIX 137 H7A 2 0.099904 0.375752 0.461521 11.00000 -1.50000 H7B 2 -0.065304 0.337641 0.486129 11.00000 -1.50000 H7C 2 -0.052894 0.363746 0.416569 11.00000 -1.50000 AFIX 0 C24 1 0.608417 0.165571 0.179932 11.00000 0.03794 0.02384 = 0.03968 0.00658 0.00949 0.00037 AFIX 23 H24A 2 0.505795 0.112464 0.184795 11.00000 -1.20000 H24B 2 0.657988 0.126576 0.152007 11.00000 -1.20000 AFIX 0 C42 1 0.870913 0.256740 0.019177 11.00000 0.03811 0.03362 = 0.02853 0.00177 0.00433 0.00325 C18 1 0.453284 -0.337291 0.229618 11.00000 0.04866 0.02192 = 0.04086 0.00059 0.02290 -0.00014 AFIX 43 H18 2 0.359567 -0.394123 0.215946 11.00000 -1.20000 AFIX 0 C47 1 0.848020 0.136516 0.028440 11.00000 0.03189 0.03112 = 0.02899 -0.00071 0.00657 0.00582 C19 1 0.591573 -0.368547 0.238399 11.00000 0.07128 0.02486 = 0.04398 0.00946 0.02631 0.01753 AFIX 43 H19 2 0.590840 -0.446177 0.230163 11.00000 -1.20000 AFIX 0 C43 1 0.775429 0.295048 -0.025425 11.00000 0.03782 0.03721 = 0.03325 0.00459 0.00443 0.00689 AFIX 43 H43 2 0.789573 0.375454 -0.029539 11.00000 -1.20000 AFIX 0 C46 1 0.726672 0.056003 -0.009593 11.00000 0.03692 0.03797 = 0.03669 0.00001 0.00807 0.00332 AFIX 43 H46 2 0.706301 -0.024487 -0.003906 11.00000 -1.20000 AFIX 0 C33 1 1.644725 0.430241 0.387861 11.00000 0.02360 0.03050 = 0.03869 -0.00019 0.00115 0.00950 AFIX 137 H33A 2 1.638287 0.402204 0.428679 11.00000 -1.50000 H33B 2 1.722910 0.505358 0.389108 11.00000 -1.50000 H33C 2 1.673189 0.374766 0.362114 11.00000 -1.50000 AFIX 0 C20 1 0.730435 -0.285512 0.259262 11.00000 0.05741 0.03743 = 0.03847 0.00773 0.01485 0.02826 AFIX 43 H20 2 0.823417 -0.306886 0.265305 11.00000 -1.20000 AFIX 0 PART 2 C50B 1 0.753451 -0.231317 0.094725 -21.00000 0.02099 AFIX 23 H50A 2 0.664345 -0.268959 0.116483 -21.00000 -1.20000 H50B 2 0.720423 -0.250888 0.051304 -21.00000 -1.20000 AFIX 0 C48B 1 0.919358 -0.026748 0.069288 -21.00000 0.01840 AFIX 23 H48A 2 1.015535 -0.044339 0.085137 -21.00000 -1.20000 H48B 2 0.896558 -0.053491 0.026313 -21.00000 -1.20000 AFIX 0 PART 0 C23 1 0.707346 0.189273 0.241784 11.00000 0.03427 0.02280 = 0.03610 0.00383 0.01384 0.00096 AFIX 23 H23A 2 0.655283 0.225569 0.269968 11.00000 -1.20000 H23B 2 0.807972 0.245330 0.237053 11.00000 -1.20000 AFIX 0 C26 1 0.477792 0.252958 0.091766 11.00000 0.05847 0.05317 = 0.05223 0.01505 0.00969 0.01756 AFIX 137 H26A 2 0.511152 0.202441 0.064612 11.00000 -1.50000 H26B 2 0.481191 0.326064 0.072725 11.00000 -1.50000 H26C 2 0.372214 0.214972 0.100203 11.00000 -1.50000 AFIX 0 C45 1 0.637235 0.095139 -0.055374 11.00000 0.02895 0.04822 = 0.03931 -0.00419 0.00264 0.00017 AFIX 43 H45 2 0.560466 0.040328 -0.081118 11.00000 -1.20000 AFIX 0 C25 1 0.587410 0.277485 0.151912 11.00000 0.06484 0.03445 = 0.04545 0.00940 0.00884 0.01421 AFIX 23 H25A 2 0.689411 0.328080 0.144235 11.00000 -1.20000 H25B 2 0.545092 0.319483 0.181127 11.00000 -1.20000 AFIX 0 PART 2 C51B 1 0.878232 -0.287556 0.112767 -21.00000 0.04867 AFIX 23 H51A 2 0.919722 -0.264496 0.155260 -21.00000 -1.20000 H51B 2 0.963449 -0.259741 0.087542 -21.00000 -1.20000 AFIX 0 PART 0 C44 1 0.660064 0.214431 -0.063509 11.00000 0.03339 0.05350 = 0.03480 0.00583 0.00308 0.01046 AFIX 43 H44 2 0.598677 0.239897 -0.094141 11.00000 -1.20000 AFIX 0 PART 2 C52B 1 0.816437 -0.425210 0.105448 -21.00000 0.07194 AFIX 137 H52A 2 0.727751 -0.447571 0.074482 -21.00000 -1.50000 H52B 2 0.785175 -0.456469 0.143857 -21.00000 -1.50000 H52C 2 0.898441 -0.456114 0.093511 -21.00000 -1.50000 AFIX 0 PART 1 C48A 1 0.937289 -0.034062 0.078280 21.00000 0.03470 AFIX 23 H48C 2 0.926485 -0.069455 0.037165 21.00000 -1.20000 H48D 2 1.035906 -0.039632 0.099342 21.00000 -1.20000 AFIX 0 C49A 1 0.805312 -0.104501 0.111492 21.00000 0.04280 AFIX 23 H49C 2 0.709795 -0.083851 0.097907 21.00000 -1.20000 H49D 2 0.830092 -0.085137 0.155280 21.00000 -1.20000 AFIX 0 C50A 1 0.778274 -0.235784 0.099663 21.00000 0.05376 AFIX 23 H50C 2 0.687227 -0.279460 0.118782 21.00000 -1.20000 H50D 2 0.757991 -0.255100 0.055795 21.00000 -1.20000 AFIX 0 C51A 1 0.915083 -0.268594 0.124549 21.00000 0.04057 AFIX 23 H51C 2 0.944063 -0.239077 0.166992 21.00000 -1.20000 H51D 2 1.002576 -0.233280 0.101504 21.00000 -1.20000 AFIX 0 C52A 1 0.881718 -0.403001 0.121228 21.00000 0.04743 AFIX 137 H52D 2 0.859954 -0.431513 0.079002 21.00000 -1.50000 H52E 2 0.792430 -0.437986 0.142651 21.00000 -1.50000 H52F 2 0.971845 -0.423806 0.139950 21.00000 -1.50000 AFIX 0 HKLF 5 REM exp_530_PTZ-CNC_twin1_hklf4 in P-1 #2 REM R1 = 0.0671 for 8733 Fo > 4sig(Fo) and 0.0738 for all 10060 data REM 562 parameters refined using 0 restraints END WGHT 0.1418 0.4643 REM Highest difference peak 0.785, deepest hole -0.984, 1-sigma level 0.085 Q1 1 1.1760 0.3955 0.0371 11.00000 0.05 0.79 Q2 1 0.9139 0.3554 0.0784 11.00000 0.05 0.66 Q3 1 0.7168 -0.2986 0.0409 11.00000 0.05 0.62 Q4 1 1.1182 0.0019 0.1649 11.00000 0.05 0.56 ; _shelx_res_checksum 54408 _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 2.248 _oxdiff_exptl_absorpt_empirical_full_min 0.655 _oxdiff_twin_integration_method simultaneous _oxdiff_twin_items 2 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 S1 S 0.27838(9) -0.17867(7) 0.22851(4) 0.03252(19) Uani 1 1 d . . . . . S2 S 1.03462(12) 0.36241(8) 0.05761(4) 0.0430(2) Uani 1 1 d . . . . . N1 N 0.5919(3) -0.0170(2) 0.27260(12) 0.0241(5) Uani 1 1 d . . . . . N2 N -0.0509(3) -0.2548(2) 0.40238(13) 0.0293(5) Uani 1 1 d . . . . . N3 N -0.3653(3) 0.1552(2) 0.51181(13) 0.0298(5) Uani 1 1 d . . . . . C16 C 0.5940(4) -0.1341(3) 0.26147(13) 0.0249(6) Uani 1 1 d . . . . . N5 N -0.2879(3) -0.0943(2) 0.45326(13) 0.0272(5) Uani 1 1 d . . . . . H5A H -0.2565 -0.1495 0.4708 0.033 Uiso 1 1 d R U . . . H5B H -0.3395 -0.0660 0.4778 0.033 Uiso 1 1 d R U . . . C15 C 0.3761(3) 0.1052(3) 0.38157(13) 0.0234(5) Uani 1 1 d . . . . . H15 H 0.3969 0.1652 0.4119 0.028 Uiso 1 1 calc R U . . . C5 C 0.0964(3) 0.1749(3) 0.40880(14) 0.0244(6) Uani 1 1 d . . . . . H5 H 0.1796 0.2349 0.3973 0.029 Uiso 1 1 calc R U . . . N8 N 0.9247(3) 0.4986(3) 0.27855(14) 0.0357(6) Uani 1 1 d . . . . . C32 C 1.4878(3) 0.4434(2) 0.36231(14) 0.0250(6) Uani 1 1 d . . . . . C6 C -0.0204(3) 0.2046(3) 0.43760(13) 0.0235(6) Uani 1 1 d . . . . . C1 C -0.1481(3) 0.1135(2) 0.45285(13) 0.0222(5) Uani 1 1 d . . . . . C8 C -0.2667(3) 0.1391(2) 0.48543(14) 0.0236(6) Uani 1 1 d . . . . . C31 C 1.4006(4) 0.3740(2) 0.31200(14) 0.0259(6) Uani 1 1 d . . . . . H31 H 1.4397 0.3176 0.2943 0.031 Uiso 1 1 calc R U . . . C2 C -0.1613(3) -0.0075(2) 0.43982(13) 0.0219(5) Uani 1 1 d . . . . . C13 C 0.4727(3) 0.0013(3) 0.30493(14) 0.0235(6) Uani 1 1 d . . . . . C28 C 1.2822(3) 0.5450(2) 0.36546(14) 0.0239(6) Uani 1 1 d . . . . . N17 N 1.5828(3) 0.6523(2) 0.48522(13) 0.0312(6) Uani 1 1 d . . . . . C10 C 0.2220(3) 0.0328(2) 0.36706(13) 0.0218(5) Uani 1 1 d . . . . . C4 C 0.0923(3) 0.0571(3) 0.39664(13) 0.0224(5) Uani 1 1 d . . . . . C11 C 0.1963(3) -0.0586(3) 0.32194(14) 0.0236(5) Uani 1 1 d . . . . . H11 H 0.0960 -0.1103 0.3128 0.028 Uiso 1 1 calc R U . . . C34 C 1.5135(3) 0.5975(3) 0.44179(15) 0.0264(6) Uani 1 1 d . . . . . C9 C -0.0422(3) -0.1561(3) 0.40628(13) 0.0239(6) Uani 1 1 d . . . . . C3 C -0.0364(3) -0.0335(2) 0.41310(13) 0.0214(5) Uani 1 1 d . . . . . C36 C 1.1715(3) 0.3119(3) 0.23228(14) 0.0254(6) Uani 1 1 d . . . . . C30 C 1.2559(4) 0.3865(2) 0.28719(13) 0.0240(6) Uani 1 1 d . . . . . C12 C 0.3182(3) -0.0731(3) 0.29070(14) 0.0252(6) Uani 1 1 d . . . . . C22 C 0.7367(3) 0.0790(3) 0.27017(15) 0.0268(6) Uani 1 1 d . . . . . H22A H 0.8065 0.0513 0.2463 0.032 Uiso 1 1 calc R U . . . H22B H 0.7892 0.0998 0.3115 0.032 Uiso 1 1 calc R U . . . C14 C 0.4984(3) 0.0886(2) 0.35131(13) 0.0222(5) Uani 1 1 d . . . . . H14 H 0.6000 0.1370 0.3624 0.027 Uiso 1 1 calc R U . . . C39 C 1.0211(4) 0.1670(3) 0.12546(14) 0.0275(6) Uani 1 1 d . . . . . C38 C 1.0770(4) 0.1195(3) 0.17868(15) 0.0280(6) Uani 1 1 d . . . . . H38 H 1.0618 0.0384 0.1796 0.034 Uiso 1 1 calc R U . . . C35 C 1.0452(4) 0.4848(3) 0.29249(15) 0.0283(6) Uani 1 1 d . . . . . C29 C 1.1972(3) 0.4718(2) 0.31453(14) 0.0247(6) Uani 1 1 d . . . . . N33 N 0.9461(3) 0.0976(2) 0.07310(13) 0.0314(6) Uani 1 1 d . . . . . C17 C 0.4534(4) -0.2208(3) 0.24116(15) 0.0291(6) Uani 1 1 d . . . . . C40 C 1.0525(4) 0.2911(3) 0.12666(15) 0.0318(7) Uani 1 1 d . . . . . C41 C 1.1191(4) 0.3605(3) 0.17972(15) 0.0288(6) Uani 1 1 d . . . . . H41 H 1.1288 0.4410 0.1802 0.035 Uiso 1 1 calc R U . . . N37 N 1.2247(3) 0.6269(2) 0.39188(13) 0.0301(6) Uani 1 1 d . . . . . H37A H 1.1363 0.5925 0.4052 0.036 Uiso 1 1 d R U . . . H37B H 1.2909 0.6631 0.4222 0.036 Uiso 1 1 d R U . . . C27 C 1.4274(3) 0.5278(3) 0.38918(13) 0.0242(6) Uani 1 1 d . . . . . C37 C 1.1541(4) 0.1911(3) 0.22968(14) 0.0267(6) Uani 1 1 d . . . . . H37 H 1.1953 0.1576 0.2631 0.032 Uiso 1 1 calc R U . . . C49B C 0.7840(12) -0.0980(8) 0.1044(4) 0.017(2) Uiso 0.46(3) 1 d . . P A 2 H49A H 0.8099 -0.0765 0.1480 0.021 Uiso 0.46(3) 1 calc R U P A 2 H49B H 0.6887 -0.0772 0.0907 0.021 Uiso 0.46(3) 1 calc R U P A 2 C21 C 0.7312(4) -0.1687(3) 0.27136(16) 0.0332(7) Uani 1 1 d . . . . . H21 H 0.8251 -0.1132 0.2863 0.040 Uiso 1 1 calc R U . . . C7 C -0.0086(4) 0.3319(3) 0.45173(15) 0.0282(6) Uani 1 1 d . . . . . H7A H 0.0999 0.3758 0.4615 0.042 Uiso 1 1 calc R U . . . H7B H -0.0653 0.3376 0.4861 0.042 Uiso 1 1 calc R U . . . H7C H -0.0529 0.3637 0.4166 0.042 Uiso 1 1 calc R U . . . C24 C 0.6084(4) 0.1656(3) 0.17993(17) 0.0351(7) Uani 1 1 d . . . . . H24A H 0.5058 0.1125 0.1848 0.042 Uiso 1 1 calc R U . . . H24B H 0.6580 0.1266 0.1520 0.042 Uiso 1 1 calc R U . . . C42 C 0.8709(4) 0.2567(3) 0.01918(15) 0.0348(7) Uani 1 1 d . . . . . C18 C 0.4533(5) -0.3373(3) 0.22962(17) 0.0380(8) Uani 1 1 d . . . . . H18 H 0.3596 -0.3941 0.2159 0.046 Uiso 1 1 calc R U . . . C47 C 0.8480(4) 0.1365(3) 0.02844(15) 0.0311(6) Uani 1 1 d . . . . . C19 C 0.5916(5) -0.3685(3) 0.23840(18) 0.0444(9) Uani 1 1 d . . . . . H19 H 0.5908 -0.4462 0.2302 0.053 Uiso 1 1 calc R U . . . C43 C 0.7754(4) 0.2950(3) -0.02543(16) 0.0368(7) Uani 1 1 d . . . . . H43 H 0.7896 0.3755 -0.0295 0.044 Uiso 1 1 calc R U . . . C46 C 0.7267(4) 0.0560(3) -0.00959(17) 0.0384(8) Uani 1 1 d . . . . . H46 H 0.7063 -0.0245 -0.0039 0.046 Uiso 1 1 calc R U . . . C33 C 1.6447(4) 0.4302(3) 0.38786(16) 0.0307(7) Uani 1 1 d . . . . . H33A H 1.6383 0.4022 0.4287 0.046 Uiso 1 1 calc R U . . . H33B H 1.7229 0.5054 0.3891 0.046 Uiso 1 1 calc R U . . . H33C H 1.6732 0.3748 0.3621 0.046 Uiso 1 1 calc R U . . . C20 C 0.7304(5) -0.2855(3) 0.25926(17) 0.0407(8) Uani 1 1 d . . . . . H20 H 0.8234 -0.3069 0.2653 0.049 Uiso 1 1 calc R U . . . C50B C 0.7535(13) -0.2313(8) 0.0947(4) 0.021(2) Uiso 0.46(3) 1 d . . P A 2 H50A H 0.6643 -0.2690 0.1165 0.025 Uiso 0.46(3) 1 calc R U P A 2 H50B H 0.7204 -0.2509 0.0513 0.025 Uiso 0.46(3) 1 calc R U P A 2 C48B C 0.9194(11) -0.0267(8) 0.0693(5) 0.018(2) Uiso 0.46(3) 1 d . . P A 2 H48A H 1.0155 -0.0443 0.0851 0.022 Uiso 0.46(3) 1 calc R U P A 2 H48B H 0.8966 -0.0535 0.0263 0.022 Uiso 0.46(3) 1 calc R U P A 2 C23 C 0.7073(4) 0.1893(3) 0.24178(15) 0.0318(7) Uani 1 1 d . . . . . H23A H 0.6553 0.2256 0.2700 0.038 Uiso 1 1 calc R U . . . H23B H 0.8080 0.2453 0.2371 0.038 Uiso 1 1 calc R U . . . C26 C 0.4778(6) 0.2530(4) 0.0918(2) 0.0539(10) Uani 1 1 d . . . . . H26A H 0.5112 0.2024 0.0646 0.081 Uiso 1 1 calc R U . . . H26B H 0.4812 0.3261 0.0727 0.081 Uiso 1 1 calc R U . . . H26C H 0.3722 0.2150 0.1002 0.081 Uiso 1 1 calc R U . . . C45 C 0.6372(4) 0.0951(4) -0.05537(17) 0.0412(8) Uani 1 1 d . . . . . H45 H 0.5605 0.0403 -0.0811 0.049 Uiso 1 1 calc R U . . . C25 C 0.5874(6) 0.2775(3) 0.15191(19) 0.0479(9) Uani 1 1 d . . . . . H25A H 0.6894 0.3281 0.1442 0.058 Uiso 1 1 calc R U . . . H25B H 0.5451 0.3195 0.1811 0.058 Uiso 1 1 calc R U . . . C51B C 0.8782(19) -0.2876(12) 0.1128(7) 0.049(3) Uiso 0.46(3) 1 d . . P A 2 H51A H 0.9197 -0.2645 0.1553 0.058 Uiso 0.46(3) 1 calc R U P A 2 H51B H 0.9634 -0.2597 0.0875 0.058 Uiso 0.46(3) 1 calc R U P A 2 C44 C 0.6601(4) 0.2144(4) -0.06351(17) 0.0410(8) Uani 1 1 d . . . . . H44 H 0.5987 0.2399 -0.0941 0.049 Uiso 1 1 calc R U . . . C52B C 0.816(3) -0.4252(14) 0.1054(8) 0.072(4) Uiso 0.46(3) 1 d . . P A 2 H52A H 0.7278 -0.4476 0.0745 0.108 Uiso 0.46(3) 1 calc R U P A 2 H52B H 0.7852 -0.4565 0.1439 0.108 Uiso 0.46(3) 1 calc R U P A 2 H52C H 0.8984 -0.4561 0.0935 0.108 Uiso 0.46(3) 1 calc R U P A 2 C48A C 0.9373(13) -0.0341(9) 0.0783(5) 0.035(3) Uiso 0.54(3) 1 d . . P A 1 H48C H 0.9265 -0.0695 0.0372 0.042 Uiso 0.54(3) 1 calc R U P A 1 H48D H 1.0359 -0.0396 0.0993 0.042 Uiso 0.54(3) 1 calc R U P A 1 C49A C 0.8053(15) -0.1045(10) 0.1115(6) 0.043(3) Uiso 0.54(3) 1 d . . P A 1 H49C H 0.7098 -0.0839 0.0979 0.051 Uiso 0.54(3) 1 calc R U P A 1 H49D H 0.8301 -0.0851 0.1553 0.051 Uiso 0.54(3) 1 calc R U P A 1 C50A C 0.7783(18) -0.2358(12) 0.0997(6) 0.054(4) Uiso 0.54(3) 1 d . . P A 1 H50C H 0.6872 -0.2795 0.1188 0.065 Uiso 0.54(3) 1 calc R U P A 1 H50D H 0.7580 -0.2551 0.0558 0.065 Uiso 0.54(3) 1 calc R U P A 1 C51A C 0.9151(14) -0.2686(9) 0.1245(5) 0.041(2) Uiso 0.54(3) 1 d . . P A 1 H51C H 0.9441 -0.2391 0.1670 0.049 Uiso 0.54(3) 1 calc R U P A 1 H51D H 1.0026 -0.2333 0.1015 0.049 Uiso 0.54(3) 1 calc R U P A 1 C52A C 0.8817(14) -0.4030(8) 0.1212(5) 0.047(3) Uiso 0.54(3) 1 d . . P A 1 H52D H 0.8600 -0.4315 0.0790 0.071 Uiso 0.54(3) 1 calc R U P A 1 H52E H 0.7924 -0.4380 0.1427 0.071 Uiso 0.54(3) 1 calc R U P A 1 H52F H 0.9718 -0.4238 0.1399 0.071 Uiso 0.54(3) 1 calc R U P A 1 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 S1 0.0236(3) 0.0341(4) 0.0350(4) -0.0085(3) 0.0069(3) -0.0003(3) S2 0.0513(5) 0.0305(4) 0.0364(4) 0.0089(3) -0.0030(4) -0.0038(4) N1 0.0181(11) 0.0208(11) 0.0318(13) 0.0016(9) 0.0071(9) 0.0016(9) N2 0.0305(13) 0.0254(13) 0.0331(13) 0.0041(10) 0.0061(10) 0.0086(11) N3 0.0249(12) 0.0284(13) 0.0362(14) -0.0004(10) 0.0076(11) 0.0062(10) C16 0.0278(14) 0.0217(13) 0.0266(14) 0.0050(11) 0.0091(11) 0.0069(11) N5 0.0240(12) 0.0202(12) 0.0379(14) 0.0050(10) 0.0126(10) 0.0034(10) C15 0.0223(13) 0.0220(13) 0.0254(13) 0.0026(10) 0.0040(10) 0.0050(11) C5 0.0206(13) 0.0225(14) 0.0297(14) 0.0043(11) 0.0063(11) 0.0041(11) N8 0.0318(15) 0.0323(15) 0.0444(16) -0.0029(12) 0.0012(12) 0.0127(12) C32 0.0236(14) 0.0196(13) 0.0309(15) 0.0054(11) 0.0071(11) 0.0030(11) C6 0.0214(13) 0.0225(13) 0.0260(14) 0.0034(10) 0.0036(10) 0.0049(11) C1 0.0191(13) 0.0222(13) 0.0255(13) 0.0021(10) 0.0049(10) 0.0053(11) C8 0.0226(13) 0.0181(13) 0.0294(14) 0.0020(10) 0.0030(11) 0.0046(11) C31 0.0260(14) 0.0177(13) 0.0329(15) 0.0012(11) 0.0065(12) 0.0035(11) C2 0.0196(13) 0.0205(13) 0.0241(13) 0.0042(10) 0.0053(10) 0.0020(10) C13 0.0210(13) 0.0216(13) 0.0287(14) 0.0064(11) 0.0065(11) 0.0059(11) C28 0.0267(14) 0.0165(12) 0.0280(14) 0.0040(10) 0.0081(11) 0.0035(11) N17 0.0347(14) 0.0198(12) 0.0365(14) 0.0025(10) 0.0016(11) 0.0040(10) C10 0.0195(13) 0.0205(12) 0.0254(13) 0.0042(10) 0.0050(10) 0.0048(10) C4 0.0194(13) 0.0228(14) 0.0245(13) 0.0035(10) 0.0026(10) 0.0050(11) C11 0.0191(13) 0.0201(13) 0.0303(14) 0.0013(11) 0.0055(10) 0.0024(10) C34 0.0237(14) 0.0199(13) 0.0347(16) 0.0043(11) 0.0065(12) 0.0036(11) C9 0.0216(13) 0.0230(15) 0.0266(13) 0.0027(11) 0.0046(10) 0.0051(11) C3 0.0185(12) 0.0197(13) 0.0256(13) 0.0037(10) 0.0056(10) 0.0036(10) C36 0.0232(13) 0.0221(13) 0.0306(15) 0.0035(11) 0.0061(11) 0.0047(11) C30 0.0281(14) 0.0170(12) 0.0270(14) 0.0066(10) 0.0086(11) 0.0044(11) C12 0.0210(13) 0.0231(13) 0.0297(14) 0.0029(11) 0.0040(11) 0.0025(11) C22 0.0190(13) 0.0235(14) 0.0349(15) -0.0002(11) 0.0079(11) -0.0002(11) C14 0.0198(13) 0.0183(12) 0.0267(13) 0.0018(10) 0.0031(10) 0.0024(10) C39 0.0275(14) 0.0227(14) 0.0289(15) 0.0007(11) 0.0039(11) 0.0014(11) C38 0.0275(15) 0.0205(13) 0.0344(16) 0.0019(11) 0.0072(12) 0.0029(11) C35 0.0309(16) 0.0208(14) 0.0326(15) 0.0010(11) 0.0055(12) 0.0059(12) C29 0.0239(14) 0.0191(13) 0.0295(14) 0.0025(11) 0.0049(11) 0.0028(11) N33 0.0337(14) 0.0241(13) 0.0322(14) -0.0003(10) 0.0040(11) 0.0018(11) C17 0.0295(15) 0.0243(14) 0.0329(15) 0.0013(12) 0.0126(12) 0.0037(12) C40 0.0359(17) 0.0216(14) 0.0332(16) 0.0043(12) 0.0012(13) 0.0012(13) C41 0.0337(16) 0.0167(13) 0.0335(16) 0.0028(11) 0.0025(12) 0.0034(12) N37 0.0279(13) 0.0242(13) 0.0375(14) -0.0023(10) 0.0036(11) 0.0067(11) C27 0.0228(13) 0.0212(13) 0.0263(13) 0.0036(11) 0.0048(11) 0.0017(11) C37 0.0287(14) 0.0216(13) 0.0287(14) 0.0042(11) 0.0052(11) 0.0045(11) C21 0.0367(17) 0.0341(17) 0.0334(16) 0.0035(13) 0.0065(13) 0.0162(14) C7 0.0275(15) 0.0203(13) 0.0368(16) 0.0051(11) 0.0087(12) 0.0051(11) C24 0.0379(17) 0.0238(15) 0.0397(18) 0.0066(13) 0.0095(14) 0.0004(13) C42 0.0381(18) 0.0336(17) 0.0285(15) 0.0018(13) 0.0043(13) 0.0032(14) C18 0.049(2) 0.0219(15) 0.0409(18) 0.0006(13) 0.0229(16) -0.0001(14) C47 0.0319(16) 0.0311(16) 0.0290(15) -0.0007(12) 0.0066(12) 0.0058(13) C19 0.071(3) 0.0249(16) 0.044(2) 0.0095(14) 0.0263(19) 0.0175(17) C43 0.0378(18) 0.0372(18) 0.0333(17) 0.0046(13) 0.0044(14) 0.0069(15) C46 0.0369(18) 0.0380(18) 0.0367(18) 0.0000(14) 0.0081(14) 0.0033(15) C33 0.0236(15) 0.0305(16) 0.0387(17) -0.0002(13) 0.0011(12) 0.0095(12) C20 0.057(2) 0.0374(19) 0.0385(18) 0.0077(14) 0.0148(16) 0.0283(18) C23 0.0343(16) 0.0228(14) 0.0361(16) 0.0038(12) 0.0138(13) 0.0010(12) C26 0.058(3) 0.053(2) 0.052(2) 0.0151(19) 0.010(2) 0.018(2) C45 0.0289(17) 0.048(2) 0.0393(19) -0.0042(16) 0.0026(14) 0.0002(15) C25 0.065(3) 0.0344(19) 0.045(2) 0.0094(16) 0.0088(19) 0.0142(18) C44 0.0334(18) 0.054(2) 0.0348(18) 0.0058(16) 0.0031(14) 0.0105(16) 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' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _citation_id _citation_doi _citation_year 1 10.1039/D0RA09580J 2021 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 C17 S1 C12 97.53(15) . . ? C42 S2 C40 99.01(16) . . ? C16 N1 C22 119.1(2) . . ? C13 N1 C16 117.8(2) . . ? C13 N1 C22 119.7(2) . . ? C17 C16 N1 119.6(3) . . ? C21 C16 N1 122.3(3) . . ? C21 C16 C17 118.1(3) . . ? H5A N5 H5B 109.3 . . ? C2 N5 H5A 109.4 . . ? C2 N5 H5B 109.5 . . ? C10 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C14 C15 C10 121.0(3) . . ? C6 C5 H5 119.1 . . ? C6 C5 C4 121.9(3) . . ? C4 C5 H5 119.1 . . ? C31 C32 C27 118.8(3) . . ? C31 C32 C33 121.2(3) . . ? C27 C32 C33 120.0(3) . . ? C5 C6 C1 118.6(3) . . ? C5 C6 C7 120.2(3) . . ? C1 C6 C7 121.2(3) . . ? C6 C1 C8 120.6(3) . . ? C6 C1 C2 122.0(2) . . ? C2 C1 C8 117.2(2) . . ? N3 C8 C1 177.3(3) . . ? C32 C31 H31 119.1 . . ? C32 C31 C30 121.8(3) . . ? C30 C31 H31 119.1 . . ? N5 C2 C1 121.3(2) . . ? N5 C2 C3 121.4(3) . . ? C3 C2 C1 117.3(2) . . ? N1 C13 C12 118.9(3) . . ? C14 C13 N1 123.4(3) . . ? C14 C13 C12 117.7(3) . . ? C29 C28 C27 117.5(3) . . ? N37 C28 C29 121.3(3) . . ? N37 C28 C27 121.2(3) . . ? C15 C10 C4 120.1(3) . . ? C15 C10 C11 117.7(2) . . ? C11 C10 C4 122.2(3) . . ? C5 C4 C10 118.7(3) . . ? C5 C4 C3 118.7(3) . . ? C3 C4 C10 122.7(3) . . ? C10 C11 H11 119.4 . . ? C12 C11 C10 121.1(3) . . ? C12 C11 H11 119.4 . . ? N17 C34 C27 178.7(3) . . ? N2 C9 C3 177.4(3) . . ? C2 C3 C4 121.4(2) . . ? C2 C3 C9 117.0(2) . . ? C4 C3 C9 121.5(2) . . ? C41 C36 C30 121.7(3) . . ? C37 C36 C30 120.6(3) . . ? C37 C36 C41 117.5(3) . . ? C31 C30 C36 118.9(3) . . ? C31 C30 C29 118.7(3) . . ? C29 C30 C36 122.4(3) . . ? C13 C12 S1 119.0(2) . . ? C11 C12 S1 120.1(2) . . ? C11 C12 C13 120.8(3) . . ? N1 C22 H22A 109.0 . . ? N1 C22 H22B 109.0 . . ? N1 C22 C23 113.1(3) . . ? H22A C22 H22B 107.8 . . ? C23 C22 H22A 109.0 . . ? C23 C22 H22B 109.0 . . ? C15 C14 C13 121.6(3) . . ? C15 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? C38 C39 C40 116.2(3) . . ? N33 C39 C38 122.6(3) . . ? N33 C39 C40 121.1(3) . . ? C39 C38 H38 119.3 . . ? C37 C38 C39 121.3(3) . . ? C37 C38 H38 119.3 . . ? N8 C35 C29 175.6(3) . . ? C28 C29 C35 117.5(3) . . ? C30 C29 C28 121.5(3) . . ? C30 C29 C35 121.0(3) . . ? C39 N33 C47 121.9(3) . . ? C39 N33 C48B 122.6(5) . . ? C39 N33 C48A 113.5(5) . . ? C47 N33 C48B 112.6(5) . . ? C47 N33 C48A 122.0(5) . . ? C16 C17 S1 118.7(2) . . ? C18 C17 S1 120.8(3) . . ? C18 C17 C16 120.4(3) . . ? C39 C40 S2 119.8(2) . . ? C41 C40 S2 118.1(2) . . ? C41 C40 C39 121.5(3) . . ? C36 C41 H41 119.4 . . ? C40 C41 C36 121.2(3) . . ? C40 C41 H41 119.4 . . ? C28 N37 H37A 109.7 . . ? C28 N37 H37B 109.0 . . ? H37A N37 H37B 109.2 . . ? C32 C27 C28 121.6(3) . . ? C32 C27 C34 119.5(3) . . ? C28 C27 C34 118.9(3) . . ? C36 C37 H37 119.1 . . ? C38 C37 C36 121.8(3) . . ? C38 C37 H37 119.1 . . ? H49A C49B H49B 107.8 . . ? C50B C49B H49A 109.1 . . ? C50B C49B H49B 109.1 . . ? C50B C49B C48B 112.6(7) . . ? C48B C49B H49A 109.1 . . ? C48B C49B H49B 109.1 . . ? C16 C21 H21 119.4 . . ? C16 C21 C20 121.2(3) . . ? C20 C21 H21 119.4 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? H24A C24 H24B 107.8 . . ? C23 C24 H24A 109.1 . . ? C23 C24 H24B 109.1 . . ? C23 C24 C25 112.7(3) . . ? C25 C24 H24A 109.1 . . ? C25 C24 H24B 109.1 . . ? C47 C42 S2 120.4(3) . . ? C43 C42 S2 118.1(3) . . ? C43 C42 C47 121.2(3) . . ? C17 C18 H18 119.9 . . ? C19 C18 C17 120.3(3) . . ? C19 C18 H18 119.9 . . ? C42 C47 N33 121.2(3) . . ? C42 C47 C46 117.4(3) . . ? C46 C47 N33 121.4(3) . . ? C18 C19 H19 119.8 . . ? C20 C19 C18 120.3(3) . . ? C20 C19 H19 119.8 . . ? C42 C43 H43 119.8 . . ? C44 C43 C42 120.5(3) . . ? C44 C43 H43 119.8 . . ? C47 C46 H46 119.6 . . ? C45 C46 C47 120.8(4) . . ? C45 C46 H46 119.6 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C21 C20 H20 120.2 . . ? C19 C20 C21 119.7(3) . . ? C19 C20 H20 120.2 . . ? C49B C50B H50A 107.2 . . ? C49B C50B H50B 107.2 . . ? H50A C50B H50B 106.8 . . ? C51B C50B C49B 120.6(10) . . ? C51B C50B H50A 107.2 . . ? C51B C50B H50B 107.2 . . ? N33 C48B C49B 115.1(6) . . ? N33 C48B H48A 108.5 . . ? N33 C48B H48B 108.5 . . ? C49B C48B H48A 108.5 . . ? C49B C48B H48B 108.5 . . ? H48A C48B H48B 107.5 . . ? C22 C23 H23A 108.7 . . ? C22 C23 H23B 108.7 . . ? C24 C23 C22 114.1(3) . . ? C24 C23 H23A 108.7 . . ? C24 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? C46 C45 H45 119.4 . . ? C44 C45 C46 121.1(4) . . ? C44 C45 H45 119.4 . . ? C24 C25 C26 112.7(4) . . ? C24 C25 H25A 109.0 . . ? C24 C25 H25B 109.0 . . ? C26 C25 H25A 109.0 . . ? C26 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C50B C51B H51A 109.2 . . ? C50B C51B H51B 109.2 . . ? C50B C51B C52B 112.0(10) . . ? H51A C51B H51B 107.9 . . ? C52B C51B H51A 109.2 . . ? C52B C51B H51B 109.2 . . ? C43 C44 C45 119.0(3) . . ? C43 C44 H44 120.5 . . ? C45 C44 H44 120.5 . . ? C51B C52B H52A 109.5 . . ? C51B C52B H52B 109.5 . . ? C51B C52B H52C 109.5 . . ? H52A C52B H52B 109.5 . . ? H52A C52B H52C 109.5 . . ? H52B C52B H52C 109.5 . . ? N33 C48A H48C 108.5 . . ? N33 C48A H48D 108.5 . . ? H48C C48A H48D 107.5 . . ? C49A C48A N33 115.0(7) . . ? C49A C48A H48C 108.5 . . ? C49A C48A H48D 108.5 . . ? C48A C49A H49C 109.4 . . ? C48A C49A H49D 109.4 . . ? C48A C49A C50A 111.1(9) . . ? H49C C49A H49D 108.0 . . ? C50A C49A H49C 109.4 . . ? C50A C49A H49D 109.4 . . ? C49A C50A H50C 109.8 . . ? C49A C50A H50D 109.8 . . ? H50C C50A H50D 108.2 . . ? C51A C50A C49A 109.6(10) . . ? C51A C50A H50C 109.8 . . ? C51A C50A H50D 109.8 . . ? C50A C51A H51C 109.6 . . ? C50A C51A H51D 109.6 . . ? C50A C51A C52A 110.4(9) . . ? H51C C51A H51D 108.1 . . ? C52A C51A H51C 109.6 . . ? C52A C51A H51D 109.6 . . ? C51A C52A H52D 109.5 . . ? C51A C52A H52E 109.5 . . ? C51A C52A H52F 109.5 . . ? H52D C52A H52E 109.5 . . ? H52D C52A H52F 109.5 . . ? H52E C52A H52F 109.5 . . ? 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 S1 C12 1.769(3) . ? S1 C17 1.764(3) . ? S2 C40 1.759(3) . ? S2 C42 1.756(4) . ? N1 C16 1.407(4) . ? N1 C13 1.398(4) . ? N1 C22 1.465(4) . ? N2 C9 1.148(4) . ? N3 C8 1.156(4) . ? C16 C17 1.402(4) . ? C16 C21 1.393(4) . ? N5 H5A 0.8613 . ? N5 H5B 0.8612 . ? N5 C2 1.356(4) . ? C15 H15 0.9300 . ? C15 C10 1.400(4) . ? C15 C14 1.389(4) . ? C5 H5 0.9300 . ? C5 C6 1.391(4) . ? C5 C4 1.402(4) . ? N8 C35 1.144(4) . ? C32 C31 1.387(4) . ? C32 C27 1.406(4) . ? C32 C33 1.503(4) . ? C6 C1 1.403(4) . ? C6 C7 1.504(4) . ? C1 C8 1.429(4) . ? C1 C2 1.422(4) . ? C31 H31 0.9300 . ? C31 C30 1.396(4) . ? C2 C3 1.413(4) . ? C13 C12 1.410(4) . ? C13 C14 1.389(4) . ? C28 C29 1.411(4) . ? C28 N37 1.361(4) . ? C28 C27 1.415(4) . ? N17 C34 1.157(4) . ? C10 C4 1.473(4) . ? C10 C11 1.405(4) . ? C4 C3 1.414(4) . ? C11 H11 0.9300 . ? C11 C12 1.388(4) . ? C34 C27 1.423(4) . ? C9 C3 1.440(4) . ? C36 C30 1.481(4) . ? C36 C41 1.392(4) . ? C36 C37 1.391(4) . ? C30 C29 1.410(4) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 C23 1.530(4) . ? C14 H14 0.9300 . ? C39 C38 1.408(4) . ? C39 N33 1.391(4) . ? C39 C40 1.413(4) . ? C38 H38 0.9300 . ? C38 C37 1.386(4) . ? C35 C29 1.441(4) . ? N33 C47 1.414(4) . ? N33 C48B 1.421(9) . ? N33 C48A 1.543(11) . ? C17 C18 1.395(4) . ? C40 C41 1.388(5) . ? C41 H41 0.9300 . ? N37 H37A 0.8614 . ? N37 H37B 0.8608 . ? C37 H37 0.9300 . ? C49B H49A 0.9700 . ? C49B H49B 0.9700 . ? C49B C50B 1.528(13) . ? C49B C48B 1.547(12) . ? C21 H21 0.9300 . ? C21 C20 1.399(5) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 C23 1.515(5) . ? C24 C25 1.518(5) . ? C42 C47 1.399(5) . ? C42 C43 1.395(5) . ? C18 H18 0.9300 . ? C18 C19 1.380(6) . ? C47 C46 1.407(5) . ? C19 H19 0.9300 . ? C19 C20 1.375(6) . ? C43 H43 0.9300 . ? C43 C44 1.381(5) . ? C46 H46 0.9300 . ? C46 C45 1.384(5) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C20 H20 0.9300 . ? C50B H50A 0.9700 . ? C50B H50B 0.9700 . ? C50B C51B 1.473(15) . ? C48B H48A 0.9700 . ? C48B H48B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C26 C25 1.529(6) . ? C45 H45 0.9300 . ? C45 C44 1.384(6) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C51B H51A 0.9700 . ? C51B H51B 0.9700 . ? C51B C52B 1.563(18) . ? C44 H44 0.9300 . ? C52B H52A 0.9600 . ? C52B H52B 0.9600 . ? C52B H52C 0.9600 . ? C48A H48C 0.9700 . ? C48A H48D 0.9700 . ? C48A C49A 1.500(15) . ? C49A H49C 0.9700 . ? C49A H49D 0.9700 . ? C49A C50A 1.515(17) . ? C50A H50C 0.9700 . ? C50A H50D 0.9700 . ? C50A C51A 1.440(16) . ? C51A H51C 0.9700 . ? C51A H51D 0.9700 . ? C51A C52A 1.531(12) . ? C52A H52D 0.9600 . ? C52A H52E 0.9600 . ? C52A H52F 0.9600 . ? 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 S1 C17 C18 C19 178.6(3) . . . . ? S2 C40 C41 C36 -164.5(3) . . . . ? S2 C42 C47 N33 6.3(4) . . . . ? S2 C42 C47 C46 -171.9(3) . . . . ? S2 C42 C43 C44 170.0(3) . . . . ? N1 C16 C17 S1 1.5(4) . . . . ? N1 C16 C17 C18 179.7(3) . . . . ? N1 C16 C21 C20 -179.3(3) . . . . ? N1 C13 C12 S1 -5.0(4) . . . . ? N1 C13 C12 C11 179.6(3) . . . . ? N1 C13 C14 C15 178.8(3) . . . . ? N1 C22 C23 C24 -51.7(4) . . . . ? C16 N1 C13 C12 -42.3(4) . . . . ? C16 N1 C13 C14 136.8(3) . . . . ? C16 N1 C22 C23 142.4(3) . . . . ? C16 C17 C18 C19 0.3(5) . . . . ? C16 C21 C20 C19 -1.3(5) . . . . ? N5 C2 C3 C4 177.2(3) . . . . ? N5 C2 C3 C9 -5.8(4) . . . . ? C15 C10 C4 C5 36.4(4) . . . . ? C15 C10 C4 C3 -143.8(3) . . . . ? C15 C10 C11 C12 -3.1(4) . . . . ? C5 C6 C1 C8 176.6(3) . . . . ? C5 C6 C1 C2 0.1(4) . . . . ? C5 C4 C3 C2 1.6(4) . . . . ? C5 C4 C3 C9 -175.2(3) . . . . ? C32 C31 C30 C36 178.2(3) . . . . ? C32 C31 C30 C29 -0.4(4) . . . . ? C6 C5 C4 C10 -178.8(3) . . . . ? C6 C5 C4 C3 1.4(4) . . . . ? C6 C1 C2 N5 -178.1(3) . . . . ? C6 C1 C2 C3 2.8(4) . . . . ? C1 C2 C3 C4 -3.6(4) . . . . ? C1 C2 C3 C9 173.3(3) . . . . ? C8 C1 C2 N5 5.3(4) . . . . ? C8 C1 C2 C3 -173.9(3) . . . . ? C31 C32 C27 C28 -1.2(4) . . . . ? C31 C32 C27 C34 178.4(3) . . . . ? C31 C30 C29 C28 0.8(4) . . . . ? C31 C30 C29 C35 -177.2(3) . . . . ? C13 N1 C16 C17 44.6(4) . . . . ? C13 N1 C16 C21 -133.8(3) . . . . ? C13 N1 C22 C23 -59.0(4) . . . . ? C10 C15 C14 C13 1.1(4) . . . . ? C10 C4 C3 C2 -178.2(3) . . . . ? C10 C4 C3 C9 5.0(4) . . . . ? C10 C11 C12 S1 -173.2(2) . . . . ? C10 C11 C12 C13 2.2(4) . . . . ? C4 C5 C6 C1 -2.2(4) . . . . ? C4 C5 C6 C7 177.9(3) . . . . ? C4 C10 C11 C12 174.1(3) . . . . ? C11 C10 C4 C5 -140.7(3) . . . . ? C11 C10 C4 C3 39.1(4) . . . . ? C36 C30 C29 C28 -177.6(3) . . . . ? C36 C30 C29 C35 4.3(4) . . . . ? C30 C36 C41 C40 174.3(3) . . . . ? C30 C36 C37 C38 -179.4(3) . . . . ? C12 S1 C17 C16 -37.2(3) . . . . ? C12 S1 C17 C18 144.6(3) . . . . ? C12 C13 C14 C15 -2.0(4) . . . . ? C22 N1 C16 C17 -156.4(3) . . . . ? C22 N1 C16 C21 25.2(4) . . . . ? C22 N1 C13 C12 158.9(3) . . . . ? C22 N1 C13 C14 -22.0(4) . . . . ? C14 C15 C10 C4 -175.8(3) . . . . ? C14 C15 C10 C11 1.4(4) . . . . ? C14 C13 C12 S1 175.8(2) . . . . ? C14 C13 C12 C11 0.4(4) . . . . ? C39 C38 C37 C36 4.0(5) . . . . ? C39 N33 C47 C42 27.7(5) . . . . ? C39 N33 C47 C46 -154.2(3) . . . . ? C39 N33 C48B C49B 75.6(9) . . . . ? C39 N33 C48A C49A 82.1(9) . . . . ? C39 C40 C41 C36 6.3(5) . . . . ? C38 C39 N33 C47 159.5(3) . . . . ? C38 C39 N33 C48B 0.3(6) . . . . ? C38 C39 N33 C48A -2.5(6) . . . . ? C38 C39 C40 S2 163.7(2) . . . . ? C38 C39 C40 C41 -6.9(5) . . . . ? C29 C28 C27 C32 1.7(4) . . . . ? C29 C28 C27 C34 -177.9(3) . . . . ? N33 C39 C38 C37 178.6(3) . . . . ? N33 C39 C40 S2 -13.2(4) . . . . ? N33 C39 C40 C41 176.3(3) . . . . ? N33 C47 C46 C45 -176.4(3) . . . . ? N33 C48A C49A C50A 164.6(9) . . . . ? C17 S1 C12 C13 39.2(3) . . . . ? C17 S1 C12 C11 -145.4(3) . . . . ? C17 C16 C21 C20 2.3(5) . . . . ? C17 C18 C19 C20 0.7(5) . . . . ? C40 S2 C42 C47 -33.4(3) . . . . ? C40 S2 C42 C43 153.6(3) . . . . ? C40 C39 C38 C37 1.9(5) . . . . ? C40 C39 N33 C47 -23.9(5) . . . . ? C40 C39 N33 C48B 176.9(5) . . . . ? C40 C39 N33 C48A 174.1(5) . . . . ? C41 C36 C30 C31 -127.4(3) . . . . ? C41 C36 C30 C29 51.0(4) . . . . ? C41 C36 C37 C38 -4.8(4) . . . . ? N37 C28 C29 C30 -179.7(3) . . . . ? N37 C28 C29 C35 -1.6(4) . . . . ? N37 C28 C27 C32 179.9(3) . . . . ? N37 C28 C27 C34 0.3(4) . . . . ? C27 C32 C31 C30 0.6(4) . . . . ? C27 C28 C29 C30 -1.5(4) . . . . ? C27 C28 C29 C35 176.6(3) . . . . ? C37 C36 C30 C31 47.0(4) . . . . ? C37 C36 C30 C29 -134.6(3) . . . . ? C37 C36 C41 C40 -0.3(5) . . . . ? C49B C50B C51B C52B 173.8(9) . . . . ? C21 C16 C17 S1 179.9(2) . . . . ? C21 C16 C17 C18 -1.9(5) . . . . ? C7 C6 C1 C8 -3.5(4) . . . . ? C7 C6 C1 C2 180.0(3) . . . . ? C42 S2 C40 C39 36.7(3) . . . . ? C42 S2 C40 C41 -152.3(3) . . . . ? C42 C47 C46 C45 1.8(5) . . . . ? C42 C43 C44 C45 2.1(5) . . . . ? C18 C19 C20 C21 -0.3(5) . . . . ? C47 N33 C48B C49B -85.3(8) . . . . ? C47 N33 C48A C49A -79.9(9) . . . . ? C47 C42 C43 C44 -3.0(5) . . . . ? C47 C46 C45 C44 -2.6(5) . . . . ? C43 C42 C47 N33 179.2(3) . . . . ? C43 C42 C47 C46 1.0(5) . . . . ? C46 C45 C44 C43 0.6(6) . . . . ? C33 C32 C31 C30 -179.0(3) . . . . ? C33 C32 C27 C28 178.3(3) . . . . ? C33 C32 C27 C34 -2.1(4) . . . . ? C50B C49B C48B N33 175.9(8) . . . . ? C48B N33 C47 C42 -171.2(4) . . . . ? C48B N33 C47 C46 6.9(5) . . . . ? C48B C49B C50B C51B 59.9(12) . . . . ? C23 C24 C25 C26 -175.8(3) . . . . ? C25 C24 C23 C22 -177.6(3) . . . . ? C48A N33 C47 C42 -171.8(5) . . . . ? C48A N33 C47 C46 6.4(6) . . . . ? C48A C49A C50A C51A 64.0(13) . . . . ? C49A C50A C51A C52A 172.0(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 0.5140 8934 16909 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 2 0.4860 0 16909 nmt -0.9994 0.0004 -0.0008 -0.0005 -0.9999 0.0009 0.5579 0.1860 1.0007