#------------------------------------------------------------------------------ #$Date: 2024-11-07 03:51:14 +0200 (Thu, 07 Nov 2024) $ #$Revision: 295817 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/16/02/7160213.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_7160213 loop_ _publ_author_name 'Cheruthu, Nusaiba Madappuram' 'Hashim, P. K.' 'Sahu, Saugata' 'Takahashi, Kiyonori' 'Nakamura, Takayoshi' 'Mitomo, Hideyuki' 'Ijiro, Kuniharu' 'Tamaoki, Nobuyuki' _publ_section_title ; Azophotoswitches containing thiazole, isothiazole, thiadiazole, and isothiadiazole ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D4OB01573H _journal_year 2024 _chemical_formula_moiety 'C8 H6 N4 S' _chemical_formula_sum 'C8 H6 N4 S' _chemical_formula_weight 190.23 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2024-07-16 _audit_creation_method ; Olex2 1.3-ac4 (compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214) ; _audit_update_record ; 2024-07-16 deposited with the CCDC. 2024-11-06 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 97.039(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.1698(4) _cell_length_b 5.5451(3) _cell_length_c 19.2296(9) _cell_measurement_reflns_used 7106 _cell_measurement_temperature 200.00(14) _cell_measurement_theta_max 71.9670 _cell_measurement_theta_min 2.3440 _cell_volume 864.58(8) _computing_cell_refinement 'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)' _computing_molecular_graphics 'Olex2 1.3-ac4 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-ac4 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 200.00(14) _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 0.991 _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 -89.00 89.00 0.50 1.37 -- 0.00 46.00 -90.00 356 2 \w -84.00 94.00 0.50 5.48 -- 5.00 37.00-180.00 356 3 \w -185.00 -6.00 0.50 5.48 -- -95.70 49.00 -17.48 358 4 \w -185.00 -6.00 0.50 5.48 -- -95.70 46.00 150.00 358 5 \w -185.00 -6.00 0.50 5.48 -- -95.70 55.00-104.90 358 6 \w -185.00 -6.00 0.50 5.48 -- -95.70 55.00-104.90 358 7 \w -185.00 -6.00 0.50 5.48 -- -95.70 54.00 89.06 358 8 \w -185.00 -6.00 0.50 5.48 -- -95.70 38.00-140.93 358 9 \w -185.00 -6.00 0.50 5.48 -- -95.70 55.00 41.60 358 10 \w -185.00 -6.00 0.50 5.48 -- -95.70 46.00 150.00 358 11 \w -185.00 -6.00 0.50 5.48 -- -95.70 52.00 140.44 358 12 \w -185.00 -6.00 0.50 5.48 -- -95.70 55.00 -37.38 358 13 \w -89.00 89.00 0.50 1.37 -- 0.00 18.00 60.00 356 14 \w -89.00 89.00 0.50 1.37 -- 0.00 46.00-180.00 356 15 \w -185.00 -6.00 0.50 5.48 -- -95.70 0.00 -90.00 358 16 \w -185.00 -74.00 0.50 5.48 -- -95.70 46.00 60.00 222 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC11 (RCD3): quarter-chi single' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0180777000 _diffrn_orient_matrix_UB_12 0.0364390000 _diffrn_orient_matrix_UB_13 0.0800177000 _diffrn_orient_matrix_UB_21 0.1837785000 _diffrn_orient_matrix_UB_22 -0.0682352000 _diffrn_orient_matrix_UB_23 0.0047537000 _diffrn_orient_matrix_UB_31 0.0445926000 _diffrn_orient_matrix_UB_32 0.2667297000 _diffrn_orient_matrix_UB_33 -0.0098369000 _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 0.0085 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 5133 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.627 _diffrn_reflns_theta_min 4.634 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 2.954 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.85321 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.99a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.461 _exptl_crystal_description plate _exptl_crystal_F_000 392 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.135 _refine_diff_density_min -0.158 _refine_diff_density_rms 0.040 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 159 _refine_ls_number_reflns 5133 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.059 _refine_ls_R_factor_all 0.0527 _refine_ls_R_factor_gt 0.0475 _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^)+(0.0808P)^2^+0.2122P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1371 _refine_ls_wR_factor_ref 0.1412 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4535 _reflns_number_total 5133 _reflns_threshold_expression 'I > 2\s(I)' _twin_special_details ; Component 2 rotated by 179.9170\% around [-0.00 0.00 1.00] (reciprocal) or [0.27 -0.00 0.96] (direct) ; _cod_data_source_file d4ob01573h2.cif _cod_data_source_block exp_867_twin1_hklf4 _cod_database_code 7160213 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C4H2N6S2 _chemical_oxdiff_usercomment 200K _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. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.620(2) 0.380(2) 2. Fixed Uiso At 1.2 times of: All C(H) groups 3. Restrained distances C7-C8 \\sim C7A-C8A with sigma of 0.02 4. Rigid bond restraints C8A, C7A with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 5. Uiso/Uaniso restraints and constraints Uanis(C8A) = Uanis(S1) 6. Others Sof(N1A)=Sof(N2A)=Sof(C7A)=Sof(S1A)=Sof(C8A)=Sof(H8A)=1-FVAR(1) Sof(S1)=Sof(C8)=Sof(H8)=Sof(N1)=Sof(N2)=Sof(C7)=FVAR(1) 7.a Aromatic/amide H refined with riding coordinates: C8(H8), C5(H5), C6(H6), C4(H4), C3(H3), C2(H2), C8A(H8A) ; _shelx_res_file ; TITL exp_867_twin1_hklf4_a.res in P2(1)/n exp_867_twin1_hklf4.res created by SHELXL-2018/3 at 16:53:36 on 26-Mar-2024 REM Old TITL exp_867_twin1_hklf4 in P2 REM SHELXT solution in P2(1)/n: R1 0.226, Rweak 0.209, Alpha 0.035 REM 1.838 for 167 systematic absences, Orientation as input REM Formula found by SHELXT: C2 N1 S CELL 1.54184 8.1698 5.5451 19.2296 90 97.039 90 ZERR 4 0.0004 0.0003 0.0009 0 0.004 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N S UNIT 32 24 16 4 DELU 0.001 0.001 C8A C7A EADP C8A S1 SADI C7 C8 C7A C8A L.S. 50 PLAN 5 TEMP -73 fmap 2 ACTA OMIT -2 -2 1 REM REM REM WGHT 0.080800 0.212200 BASF 0.38018 FVAR 6.63366 0.72575 PART 1 S1 4 0.083765 0.880893 0.585891 21.00000 0.06825 0.05452 = 0.04044 -0.00210 0.01454 -0.00086 C8 1 0.171823 0.508578 0.660178 21.00000 0.17743 0.14101 = 0.12265 -0.02602 0.02907 -0.05465 AFIX 43 H8 2 0.210254 0.353538 0.675569 21.00000 -1.20000 AFIX 0 N1 3 0.221201 0.570191 0.484853 21.00000 0.04976 0.05135 = 0.03552 -0.00349 0.01072 -0.00620 N2 3 0.234919 0.466323 0.544798 21.00000 0.05517 0.05496 = 0.02975 -0.00149 0.01015 -0.00741 PART 0 C1 1 0.294929 0.439340 0.433346 11.00000 0.04593 0.06164 = 0.04546 -0.00995 0.01161 -0.00997 PART 1 C7 1 0.169623 0.597429 0.595578 21.00000 0.04629 0.04406 = 0.04129 -0.00019 0.00762 -0.00537 PART 0 C5 1 0.446251 0.127342 0.384719 11.00000 0.05638 0.06182 = 0.09143 -0.01598 0.01585 0.00077 AFIX 43 H5 2 0.502751 -0.022626 0.389376 11.00000 -1.20000 AFIX 0 C6 1 0.376376 0.221542 0.440500 11.00000 0.05647 0.07157 = 0.05959 0.00796 0.01149 -0.00382 AFIX 43 H6 2 0.384340 0.136654 0.483696 11.00000 -1.20000 AFIX 0 C4 1 0.433896 0.251878 0.321838 11.00000 0.05424 0.10221 = 0.05843 -0.02978 0.01832 -0.01045 AFIX 43 H4 2 0.482946 0.187773 0.283511 11.00000 -1.20000 AFIX 0 C3 1 0.351376 0.466711 0.314726 11.00000 0.06548 0.09984 = 0.04799 0.00733 0.01698 -0.00455 AFIX 43 H3 2 0.342757 0.551039 0.271427 11.00000 -1.20000 AFIX 0 C2 1 0.280816 0.560937 0.370166 11.00000 0.05859 0.06108 = 0.05987 0.00130 0.01470 -0.00435 AFIX 43 H2 2 0.222489 0.709342 0.365027 11.00000 -1.20000 AFIX 0 PART 2 N1A 3 0.246644 0.452019 0.508528 -21.00000 0.06191 0.06130 = 0.07395 0.00098 -0.00505 -0.01318 N2A 3 0.187361 0.645978 0.508965 -21.00000 0.07687 0.07243 = 0.06467 0.00243 0.00374 -0.01899 C7A 1 0.144488 0.681377 0.581567 -21.00000 0.05386 0.05501 = 0.05043 -0.00609 0.01919 -0.00729 S1A 4 0.171665 0.515550 0.654617 -21.00000 0.05746 0.06409 = 0.06291 0.02476 0.01108 -0.00228 PART 0 N4 3 0.103167 0.696324 0.703768 11.00000 0.08374 0.07359 = 0.04455 -0.00876 0.02150 -0.01365 N3 3 0.052222 0.891527 0.670655 11.00000 0.08466 0.07015 = 0.05169 -0.01246 0.02158 -0.00874 PART 2 C8A 1 0.081511 0.886358 0.602116 -21.00000 0.06825 0.05452 = 0.04044 -0.00210 0.01454 -0.00086 AFIX 43 H8A 2 0.058462 1.019728 0.571469 -21.00000 -1.20000 AFIX 0 HKLF 5 REM exp_867_twin1_hklf4_a.res in P2(1)/n REM wR2 = 0.1412, GooF = S = 1.059, Restrained GooF = 1.059 for all data REM R1 = 0.0475 for 4535 Fo > 4sig(Fo) and 0.0527 for all 5133 data REM 159 parameters refined using 2 restraints END WGHT 0.0812 0.2093 REM Highest difference peak 0.135, deepest hole -0.158, 1-sigma level 0.040 Q1 1 0.0457 0.6208 0.5974 11.00000 0.05 0.13 Q2 1 0.1081 0.6157 0.5864 11.00000 0.05 0.13 Q3 1 0.5000 0.0000 0.5000 10.50000 0.05 0.13 Q4 1 0.3925 0.5558 0.3477 11.00000 0.05 0.13 Q5 1 0.4939 0.0435 0.2984 11.00000 0.05 0.12 ; _shelx_res_checksum 30557 _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 1.561 _oxdiff_exptl_absorpt_empirical_full_min 0.812 _oxdiff_twin_integration_method simultaneous _oxdiff_twin_items 2 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.0838(2) 0.8809(3) 0.58589(5) 0.0537(4) Uani 0.726(5) 1 d . . P A 1 C8 C 0.1718(17) 0.509(3) 0.6602(8) 0.146(8) Uani 0.726(5) 1 d D . P A 1 H8 H 0.210254 0.353538 0.675569 0.175 Uiso 0.726(5) 1 calc R U P A 1 N1 N 0.2212(5) 0.5702(11) 0.4849(2) 0.0451(9) Uani 0.726(5) 1 d . . P A 1 N2 N 0.2349(4) 0.4663(8) 0.54480(18) 0.0462(9) Uani 0.726(5) 1 d . . P A 1 C1 C 0.2949(3) 0.4393(5) 0.43335(12) 0.0505(7) Uani 1 1 d . . . . . C7 C 0.1696(9) 0.5974(10) 0.5956(3) 0.0437(13) Uani 0.726(5) 1 d D . P A 1 C5 C 0.4463(4) 0.1273(7) 0.38472(18) 0.0693(9) Uani 1 1 d . . . . . H5 H 0.502751 -0.022626 0.389376 0.083 Uiso 1 1 calc R U . . . C6 C 0.3764(3) 0.2215(6) 0.44050(15) 0.0622(8) Uani 1 1 d . . . . . H6 H 0.384340 0.136654 0.483696 0.075 Uiso 1 1 calc R U . . . C4 C 0.4339(3) 0.2519(7) 0.32184(15) 0.0707(10) Uani 1 1 d . . . . . H4 H 0.482946 0.187773 0.283511 0.085 Uiso 1 1 calc R U . . . C3 C 0.3514(4) 0.4667(7) 0.31473(15) 0.0703(9) Uani 1 1 d . . . . . H3 H 0.342757 0.551039 0.271427 0.084 Uiso 1 1 calc R U . . . C2 C 0.2808(4) 0.5609(6) 0.37017(14) 0.0592(7) Uani 1 1 d . . . . . H2 H 0.222489 0.709342 0.365027 0.071 Uiso 1 1 calc R U . . . N1A N 0.2466(15) 0.452(3) 0.5085(9) 0.067(4) Uani 0.274(5) 1 d . . P A 2 N2A N 0.1874(17) 0.646(3) 0.5090(8) 0.072(4) Uani 0.274(5) 1 d . . P A 2 C7A C 0.144(3) 0.681(3) 0.5816(9) 0.052(4) Uani 0.274(5) 1 d D U P A 2 S1A S 0.1717(5) 0.5156(10) 0.6546(3) 0.0612(13) Uani 0.274(5) 1 d . . P A 2 N4 N 0.1032(3) 0.6963(5) 0.70377(11) 0.0662(8) Uani 1 1 d . . . . . N3 N 0.0522(3) 0.8915(5) 0.67066(12) 0.0677(7) Uani 1 1 d . . . . . C8A C 0.082(3) 0.886(4) 0.6021(9) 0.0537(4) Uani 0.274(5) 1 d D U P A 2 H8A H 0.058462 1.019728 0.571469 0.064 Uiso 0.274(5) 1 calc R U P A 2 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 0.0682(6) 0.0545(6) 0.0404(7) -0.0021(6) 0.0145(6) -0.0009(4) C8 0.177(13) 0.141(13) 0.123(12) -0.026(9) 0.029(8) -0.055(10) N1 0.050(2) 0.051(3) 0.036(2) -0.0035(18) 0.0107(14) -0.0062(17) N2 0.0552(19) 0.055(2) 0.0297(15) -0.0015(17) 0.0102(14) -0.0074(14) C1 0.0459(14) 0.0616(19) 0.0455(12) -0.0099(11) 0.0116(10) -0.0100(12) C7 0.046(3) 0.044(3) 0.041(2) 0.000(2) 0.0076(19) -0.005(2) C5 0.0564(17) 0.062(2) 0.091(2) -0.0160(16) 0.0158(14) 0.0008(14) C6 0.0565(16) 0.072(2) 0.0596(15) 0.0080(14) 0.0115(12) -0.0038(15) C4 0.0542(16) 0.102(3) 0.0584(16) -0.0298(17) 0.0183(12) -0.0105(17) C3 0.0655(18) 0.100(3) 0.0480(14) 0.0073(15) 0.0170(12) -0.0046(18) C2 0.0586(16) 0.0611(19) 0.0599(15) 0.0013(13) 0.0147(12) -0.0044(14) N1A 0.062(7) 0.061(8) 0.074(11) 0.001(8) -0.005(7) -0.013(6) N2A 0.077(8) 0.072(10) 0.065(8) 0.002(6) 0.004(6) -0.019(7) C7A 0.054(9) 0.055(8) 0.050(8) -0.006(7) 0.019(6) -0.007(7) S1A 0.057(2) 0.064(3) 0.063(2) 0.025(2) 0.0111(17) -0.002(2) N4 0.0837(18) 0.0736(19) 0.0445(11) -0.0088(11) 0.0215(11) -0.0136(14) N3 0.0847(17) 0.0702(19) 0.0517(13) -0.0125(12) 0.0216(11) -0.0087(14) C8A 0.0682(6) 0.0545(6) 0.0404(7) -0.0021(6) 0.0145(6) -0.0009(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_ _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 N3 S1 C7 92.1(2) . . ? C7 C8 N4 107.6(11) . . ? N2 N1 C1 113.6(5) . . ? N1 N2 C7 113.7(5) . . ? C6 C1 N1 128.3(3) . . ? C6 C1 C2 120.2(2) . . ? C6 C1 N1A 97.0(6) . . ? C2 C1 N1 111.5(3) . . ? C2 C1 N1A 142.8(7) . . ? C8 C7 S1 113.4(8) . . ? C8 C7 N2 120.2(8) . . ? N2 C7 S1 126.4(4) . . ? C6 C5 C4 119.8(3) . . ? C1 C6 C5 119.7(3) . . ? C3 C4 C5 120.3(3) . . ? C4 C3 C2 120.1(3) . . ? C3 C2 C1 119.9(3) . . ? N2A N1A C1 101.5(17) . . ? N1A N2A C7A 105.7(16) . . ? N2A C7A S1A 133.7(12) . . ? C8A C7A N2A 122.3(15) . . ? C8A C7A S1A 103.7(13) . . ? N4 S1A C7A 97.9(6) . . ? N3 N4 C8 115.3(6) . . ? N3 N4 S1A 111.3(2) . . ? N4 N3 S1 111.6(2) . . ? N4 N3 C8A 111.8(11) . . ? C7A C8A N3 115.1(19) . . ? 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 C7 1.722(5) . ? S1 N3 1.682(2) . ? C8 C7 1.334(14) . ? C8 N4 1.489(15) . ? N1 N2 1.281(6) . ? N1 C1 1.420(5) . ? N2 C7 1.376(7) . ? C1 C6 1.378(4) . ? C1 C2 1.382(4) . ? C1 N1A 1.546(19) . ? C5 C6 1.378(4) . ? C5 C4 1.385(5) . ? C4 C3 1.367(5) . ? C3 C2 1.376(4) . ? N1A N2A 1.18(2) . ? N2A C7A 1.49(2) . ? C7A S1A 1.671(17) . ? C7A C8A 1.33(2) . ? S1A N4 1.530(7) . ? N4 N3 1.298(4) . ? N3 C8A 1.368(16) . ? 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 0.620(2) 5844 9741 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 2 0.380(2) 5869 9741 nmt -1.0004 -0.0012 -0.0006 0.0013 -0.9983 -0.0000 0.5720 -0.0046 1.0006