#------------------------------------------------------------------------------ #$Date: 2026-06-05 20:27:44 +0100 (Fri, 05 Jun 2026) $ #$Revision: 306467 $ #$URL: svn://www.crystallography.net/cod/cif/7/06/43/7064395.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_7064395 loop_ _publ_author_name 'Shepelenko, Konstantin E.' 'Gnatiuk, Irina G.' 'Kolotova, Uliana A.' 'Minyaev, Mikhayl E.' 'Chernyshev, Victor M.' _publ_section_title ; Sustainable ruthenium-catalyzed C--H alkylation of 2-(hetero)aryl benzimidazoles with maleimides ; _journal_issue 20 _journal_name_full 'New Journal of Chemistry' _journal_page_first 8550 _journal_page_last 8554 _journal_paper_doi 10.1039/D6NJ00299D _journal_volume 50 _journal_year 2026 _chemical_absolute_configuration ad _chemical_formula_moiety 'C26 H23 N3 O3' _chemical_formula_sum 'C26 H23 N3 O3' _chemical_formula_weight 425.47 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2025-05-22 _audit_creation_method ; Olex2 1.5-ac6-020 (compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966) ; _audit_update_record ; 2025-10-12 deposited with the CCDC. 2026-04-29 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 110.1561(17) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.40197(15) _cell_length_b 9.52044(13) _cell_length_c 12.31548(18) _cell_measurement_reflns_used 19520 _cell_measurement_temperature 100.0(2) _cell_measurement_theta_max 79.3840 _cell_measurement_theta_min 3.8120 _cell_volume 1034.86(3) _computing_cell_refinement 'CrysAlisPro 1.171.44.111a (Rigaku OD, 2025)' _computing_data_collection 'CrysAlisPro system (CCD 44.106a 64-bit (release 18-04-2025))' _computing_data_reduction 'CrysAlisPro 1.171.44.111a (Rigaku OD, 2025)' _computing_molecular_graphics 'SHELXTL (Sheldrick, Acta Cryst., 2008, A64, 112-122)' _computing_publication_material 'SHELXTL (Sheldrick, Acta Cryst., 2008, A64, 112-122)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, Acta Cryst., 2015, C71, 3-8)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, Acta Cryst., 2015, A71, 3-8)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.0(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix-6000HE _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 -28.00 27.00 0.50 0.25 -- 46.59 -19.00-180.00 110 2 \w -27.00 -2.00 0.50 0.25 -- 46.59 -38.00 30.00 50 3 \w -10.00 16.00 0.50 0.25 -- 46.59 -73.00 168.00 52 4 \w 77.00 103.00 0.50 1.00 -- 113.25-125.00 150.00 52 5 \w 43.00 105.00 0.50 1.00 -- 113.25-125.00 30.00 124 6 \w 62.00 103.00 0.50 1.00 -- 113.25 -95.00 60.00 82 7 \w 41.00 104.00 0.50 1.00 -- 113.25 -95.00 30.00 126 8 \w -20.00 49.00 0.50 0.25 -- 46.46 -48.00 -16.00 138 9 \w -155.00-118.00 0.50 1.00 -- -91.75 -48.00 -16.00 74 10 \w -117.00 -38.00 0.50 0.25 -- -46.46 -48.00 -16.00 158 11 \w -42.00 -13.00 0.50 0.25 -- -46.46 125.00 60.00 58 12 \w -108.00 -34.00 0.50 0.25 -- -46.46 -57.00-120.00 148 13 \w -21.00 5.00 0.50 0.25 -- 46.46 -19.00-120.00 52 14 \w 45.00 81.00 0.50 0.25 -- 46.46 38.00 90.00 72 15 \w -28.00 27.00 0.50 0.25 -- 46.46 -19.00 -90.00 110 16 \w 84.00 110.00 0.50 0.25 -- 46.46 38.00 90.00 52 17 \w -162.00-133.00 0.50 1.00 -- -91.75 -61.00 30.00 58 18 \w -50.00 -23.00 0.50 1.00 -- -91.75 45.00 -30.00 54 19 \w 44.00 69.00 0.50 1.00 -- 113.25 -61.00 90.00 50 20 \w 44.00 108.00 0.50 1.00 -- 113.25-125.00 -60.00 128 21 \w 144.00 177.00 0.50 1.00 -- 113.25 61.00 90.00 66 22 \w 114.00 146.00 0.50 1.00 -- 113.25 45.00 150.00 64 23 \w 149.00 176.00 0.50 1.00 -- 113.25 45.00 150.00 54 24 \w 43.00 77.00 0.50 1.00 -- 113.25-125.00 -30.00 68 25 \w 43.00 70.00 0.50 1.00 -- 113.25 -61.00-180.00 54 26 \w 42.00 67.00 0.50 1.00 -- 113.25 -61.00 60.00 50 27 \w 99.00 177.00 0.50 1.00 -- 113.25 45.00 30.00 156 28 \w 126.00 177.00 0.50 1.00 -- 113.25 45.00 0.00 102 29 \w 48.00 96.00 0.50 1.00 -- 113.25-125.00-150.00 96 30 \w 100.00 130.00 0.50 1.00 -- 113.25 61.00 60.00 60 31 \w 142.00 174.00 0.50 1.00 -- 113.25 61.00 60.00 64 32 \w 133.00 159.00 0.50 1.00 -- 113.25 125.00-150.00 52 33 \w 67.00 93.00 0.50 1.00 -- 113.25 -77.00 120.00 52 34 \w 90.00 118.00 0.50 1.00 -- 113.25 77.00 -90.00 56 35 \w 132.00 174.00 0.50 1.00 -- 113.25 77.00 -90.00 84 36 \w 119.00 167.00 0.50 1.00 -- 113.25 125.00 -30.00 96 37 \w 108.00 134.00 0.50 1.00 -- 113.25 77.00 -30.00 52 38 \w 138.00 169.00 0.50 1.00 -- 113.25 77.00 -30.00 62 39 \w 110.00 136.00 0.50 1.00 -- 113.25 45.00-180.00 52 40 \w 98.00 176.00 0.50 1.00 -- 113.25 15.00 90.00 156 41 \w 86.00 111.00 0.50 1.00 -- 113.25-125.00 -90.00 50 42 \w 41.00 87.00 0.50 1.00 -- 113.25 -77.00-180.00 92 43 \w 99.00 142.00 0.50 1.00 -- 113.25 61.00 30.00 86 44 \w 44.00 72.00 0.50 1.00 -- 113.25-125.00 -90.00 56 45 \w 44.00 69.00 0.50 1.00 -- 113.25 -61.00 -60.00 50 46 \w 60.00 104.00 0.50 1.00 -- 113.25 -77.00 -90.00 88 47 \w 111.00 178.00 0.50 1.00 -- 113.25 125.00 0.00 134 48 \w 41.00 66.00 0.50 1.00 -- 113.25 -61.00 30.00 50 49 \w 101.00 132.00 0.50 1.00 -- 113.25 30.00 -30.00 62 50 \w 147.00 177.00 0.50 1.00 -- 113.25 30.00 -30.00 60 51 \w 74.00 100.00 0.50 1.00 -- 113.25 -77.00 60.00 52 52 \w 91.00 156.00 0.50 1.00 -- 113.25 77.00-150.00 130 53 \w 129.00 156.00 0.50 1.00 -- 113.25 77.00-120.00 54 54 \w 101.00 127.00 0.50 1.00 -- 113.25 61.00 0.00 52 55 \w 104.00 129.00 0.50 1.00 -- 113.25 61.00 90.00 50 56 \w 99.00 138.00 0.50 1.00 -- 113.25 45.00 90.00 78 57 \w 91.00 120.00 0.50 1.00 -- 113.25 77.00-120.00 58 58 \w 148.00 173.00 0.50 1.00 -- 113.25 45.00-180.00 50 59 \w 48.00 74.00 0.50 1.00 -- 113.25 -95.00-150.00 52 60 \w 127.00 168.00 0.50 1.00 -- 113.25 45.00-120.00 82 61 \w 99.00 150.00 0.50 1.00 -- 113.25 45.00 60.00 102 62 \w 106.00 150.00 0.50 1.00 -- 113.25 61.00-150.00 88 63 \w 96.00 126.00 0.50 1.00 -- 113.25 61.00 -30.00 60 64 \w 41.00 66.00 0.50 1.00 -- 113.25 -61.00 150.00 50 65 \w 124.00 151.00 0.50 1.00 -- 113.25 125.00 30.00 54 66 \w 94.00 137.00 0.50 1.00 -- 113.25 -82.00 83.18 86 67 \w 41.00 66.00 0.50 1.00 -- 113.25 -61.00-150.00 50 68 \w -57.00 -31.00 0.50 0.25 -- -46.46 72.00 175.00 52 69 \w -61.00 -35.00 0.50 1.00 -- -91.75 61.00 -60.00 52 70 \w 48.00 92.00 0.50 1.00 -- 113.25 -95.00-120.00 88 71 \w 148.00 174.00 0.50 1.00 -- 113.25 61.00-120.00 52 72 \w 46.00 91.00 0.50 1.00 -- 113.25 -95.00 0.00 90 73 \w 41.00 67.00 0.50 1.00 -- 113.25 -61.00 -90.00 52 74 \w 107.00 133.00 0.50 1.00 -- 113.25 15.00 60.00 52 75 \w 153.00 178.00 0.50 1.00 -- 113.25 15.00 60.00 50 76 \w 91.00 117.00 0.50 1.00 -- 113.25 77.00 -30.00 52 77 \w 117.00 156.00 0.50 1.00 -- 113.25 30.00 150.00 78 78 \w 41.00 67.00 0.50 1.00 -- 113.25 -77.00 120.00 52 79 \w 75.00 101.00 0.50 1.00 -- 113.25 -77.00 120.00 52 80 \w 41.00 66.00 0.50 1.00 -- 113.25 -61.00-180.00 50 81 \w 146.00 172.00 0.50 1.00 -- 113.25 61.00-180.00 52 82 \w 99.00 125.00 0.50 1.00 -- 113.25 61.00-120.00 52 83 \w 46.00 86.00 0.50 1.00 -- 113.25 -95.00 -30.00 80 84 \w 130.00 156.00 0.50 1.00 -- 113.25 15.00 30.00 52 85 \w 41.00 66.00 0.50 1.00 -- 113.25 -61.00 120.00 50 86 \w 150.00 176.00 0.50 1.00 -- 113.25 77.00 -30.00 52 87 \w 98.00 145.00 0.50 1.00 -- 113.25 77.00 60.00 94 88 \w 80.00 127.00 0.50 1.00 -- 113.25 -2.00 92.43 94 89 \w 45.00 71.00 0.50 1.00 -- 113.25 -77.00 -30.00 52 90 \w 51.00 77.00 0.50 1.00 -- 113.25 -95.00 -90.00 52 91 \w 53.00 79.00 0.50 1.00 -- 113.25-125.00-120.00 52 92 \w 125.00 151.00 0.50 1.00 -- 113.25 45.00-150.00 52 93 \w 118.00 144.00 0.50 1.00 -- 113.25 45.00 90.00 52 94 \w 137.00 163.00 0.50 1.00 -- 113.25 61.00 -30.00 52 95 \w 138.00 164.00 0.50 1.00 -- 113.25 15.00-180.00 52 96 \w 107.00 141.00 0.50 1.00 -- 113.25 15.00 0.00 68 97 \w 99.00 125.00 0.50 1.00 -- 113.25 77.00 -60.00 52 98 \w 59.00 85.00 0.50 1.00 -- 113.25 -86.00 88.85 52 99 \w 87.00 113.00 0.50 1.00 -- 113.25 -86.00 88.85 52 100 \w 96.00 122.00 0.50 1.00 -- 113.25 -88.00 131.50 52 101 \w 114.00 140.00 0.50 1.00 -- 113.25 -88.00-171.44 52 102 \w 145.00 171.00 0.50 1.00 -- 113.25 45.00 120.00 52 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.1521872000 _diffrn_orient_matrix_UB_12 -0.0791691000 _diffrn_orient_matrix_UB_13 0.0420570000 _diffrn_orient_matrix_UB_21 -0.0651410000 _diffrn_orient_matrix_UB_22 -0.1040442000 _diffrn_orient_matrix_UB_23 0.0665326000 _diffrn_orient_matrix_UB_31 -0.0553258000 _diffrn_orient_matrix_UB_32 -0.0953865000 _diffrn_orient_matrix_UB_33 -0.1074994000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_unetI/netI 0.0138 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 43379 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 79.901 _diffrn_reflns_theta_min 3.823 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.731 _exptl_absorpt_correction_T_max 0.919 _exptl_absorpt_correction_T_min 0.861 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.44.111a (Rigaku Oxford Diffraction, 2025) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 448 _exptl_crystal_size_max 0.243 _exptl_crystal_size_mid 0.241 _exptl_crystal_size_min 0.153 _refine_diff_density_max 0.276 _refine_diff_density_min -0.204 _refine_diff_density_rms 0.047 _refine_ls_abs_structure_details ; Classical Flack method preferred over Parsons because s.u. lower. ; _refine_ls_abs_structure_Flack 0.01(12) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 309 _refine_ls_number_reflns 8582 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.064 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0362 _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^)+(0.0778P)^2^+0.0762P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1028 _refine_ls_wR_factor_ref 0.1032 _reflns_Friedel_coverage 0.880 _reflns_Friedel_fraction_full 0.998 _reflns_Friedel_fraction_max 0.995 _reflns_number_gt 8517 _reflns_number_total 8582 _reflns_threshold_expression 'I > 2\s(I)' _twin_special_details ; Component 2 rotated by 179.9947\% around [1.00 0.00 -0.00] (reciprocal) or [0.97 0.00 0.25] (direct) ; _cod_data_source_file d6nj00299d2.cif _cod_data_source_block RuSk-15-39 _cod_depositor_comments 'Adding full bibliography for 7064394--7064395.cif.' _cod_database_code 7064395 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C26 H23 N3 O3' _chemical_oxdiff_usercomment RuSk-15-39 _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 0.896 _shelx_estimated_absorpt_t_min 0.842 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.5346(12) 0.4654(12) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 3.a Ternary CH refined with riding coordinates and stretchable bonds: C3(H3) 3.b Secondary CH2 refined with riding coordinates and stretchable bonds: C2(H2A,H2B) 3.c Aromatic/amide H refined with riding coordinates and stretchable bonds: C6(H6), C7(H7), C9(H9), C10(H10), C13(H13), C15(H15), C16(H16), C21(H21), C22(H22), C23(H23), C24(H24) 3.d Idealised Me refined as rotating group with stretchable bonds: C11(H11A,H11B,H11C), C18(H18A,H18B,H18C), C26(H26A,H26B,H26C) ; _shelx_res_file ; TITL RuSk-15-39 in P2(1) rusk-15-39.res created by SHELXL-2018/3 at 19:32:45 on 22-May-2025 REM SHELXT solution in P2(1) REM R1 0.072, Rweak 0.031, Alpha 0.004, Orientation as input REM Flack x = -0.072 ( 0.117 ) from Parsons' quotients REM Formula found by SHELXT: C26 N3 O3 CELL 1.54184 9.40197 9.52044 12.31548 90 110.1561 90 ZERR 2 0.00015 0.00013 0.00018 0 0.0017 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H N O UNIT 52 46 6 6 L.S. 7 PLAN 17 SIZE 0.153 0.241 0.243 TEMP -173.15 CONF list 4 MORE -1 BOND $H fmap 2 53 acta MERG 0 REM REM REM WGHT 0.077800 0.076200 BASF 0.46543 FVAR 11.27100 N1 3 0.457672 0.392704 0.633143 11.00000 0.01815 0.01788 = 0.01741 0.00024 0.00353 -0.00062 C1 1 0.571236 0.479432 0.619894 11.00000 0.01847 0.02121 = 0.02193 0.00040 0.00482 -0.00002 C2 1 0.527084 0.515775 0.493294 11.00000 0.01624 0.01838 = 0.02032 0.00044 0.00513 -0.00095 AFIX 24 H2A 2 0.613258 0.496373 0.464624 11.00000 -1.20000 H2B 2 0.498607 0.617836 0.480017 11.00000 -1.20000 AFIX 0 C3 1 0.390489 0.421572 0.430890 11.00000 0.01589 0.01405 = 0.01899 -0.00046 0.00558 -0.00018 AFIX 14 H3 2 0.427840 0.343159 0.398357 11.00000 -1.20000 AFIX 0 C4 1 0.342223 0.363803 0.528607 11.00000 0.01723 0.01417 = 0.01845 -0.00016 0.00401 0.00151 O1 4 0.681680 0.517445 0.698802 11.00000 0.02534 0.04075 = 0.02374 0.00065 0.00000 -0.01386 O2 4 0.228370 0.299654 0.519128 11.00000 0.01933 0.02042 = 0.02369 0.00082 0.00461 -0.00346 C5 1 0.454628 0.337679 0.740873 11.00000 0.02035 0.01798 = 0.01801 -0.00123 0.00541 -0.00116 C6 1 0.566124 0.245164 0.803693 11.00000 0.02120 0.02559 = 0.01928 -0.00107 0.00674 0.00450 AFIX 44 H6 2 0.647440 0.223758 0.779252 11.00000 -1.20000 AFIX 0 C7 1 0.556189 0.184003 0.903942 11.00000 0.02633 0.02360 = 0.01923 0.00165 0.00588 0.00583 AFIX 44 H7 2 0.635994 0.116763 0.948997 11.00000 -1.20000 AFIX 0 C8 1 0.435633 0.215828 0.942074 11.00000 0.02416 0.01974 = 0.01895 -0.00287 0.00716 -0.00283 C9 1 0.327877 0.312903 0.878793 11.00000 0.02168 0.02176 = 0.02557 -0.00152 0.00984 -0.00025 AFIX 44 H9 2 0.244969 0.338869 0.905581 11.00000 -1.20000 AFIX 0 C10 1 0.335919 0.373518 0.778399 11.00000 0.02080 0.02021 = 0.02479 0.00145 0.00668 0.00260 AFIX 44 H10 2 0.265445 0.434933 0.738376 11.00000 -1.20000 AFIX 0 C11 1 0.421962 0.146177 1.048260 11.00000 0.03245 0.02373 = 0.01974 -0.00137 0.00873 -0.00416 AFIX 138 H11A 2 0.338538 0.192867 1.069207 11.00000 -1.50000 H11B 2 0.520894 0.155669 1.114737 11.00000 -1.50000 H11C 2 0.397322 0.043457 1.031782 11.00000 -1.50000 AFIX 0 C12 1 0.260967 0.486466 0.334045 11.00000 0.01453 0.01634 = 0.01882 0.00027 0.00570 -0.00131 C13 1 0.229344 0.437352 0.221828 11.00000 0.01619 0.01847 = 0.02144 -0.00202 0.00732 -0.00029 AFIX 44 H13 2 0.288849 0.365479 0.207878 11.00000 -1.20000 AFIX 0 C14 1 0.110317 0.493390 0.129527 11.00000 0.01834 0.02045 = 0.01677 -0.00194 0.00565 -0.00410 C15 1 0.021200 0.600667 0.148464 11.00000 0.01846 0.02017 = 0.01840 0.00183 0.00343 0.00148 AFIX 44 H15 2 -0.056267 0.639488 0.087647 11.00000 -1.20000 AFIX 0 C16 1 0.051264 0.648268 0.261038 11.00000 0.02042 0.01740 = 0.02042 0.00016 0.00668 0.00398 AFIX 44 H16 2 -0.011583 0.721341 0.275105 11.00000 -1.20000 AFIX 0 C17 1 0.169406 0.593500 0.353955 11.00000 0.01722 0.01405 = 0.01708 -0.00020 0.00601 -0.00061 O3 4 0.087867 0.433148 0.024029 11.00000 0.02305 0.03011 = 0.01646 -0.00429 0.00497 0.00363 C18 1 -0.044705 0.475679 -0.069946 11.00000 0.02731 0.02794 = 0.01573 -0.00252 0.00374 0.00264 AFIX 138 H18A 2 -0.047696 0.427386 -0.139604 11.00000 -1.50000 H18B 2 -0.041429 0.575754 -0.081369 11.00000 -1.50000 H18C 2 -0.134076 0.452475 -0.052016 11.00000 -1.50000 AFIX 0 C19 1 0.188080 0.646217 0.471627 11.00000 0.01699 0.01210 = 0.01764 0.00043 0.00489 0.00207 N2 3 0.084182 0.613641 0.522929 11.00000 0.01664 0.01511 = 0.02033 -0.00183 0.00654 -0.00086 N3 3 0.295814 0.732078 0.533998 11.00000 0.01810 0.01660 = 0.01735 -0.00077 0.00456 -0.00109 C20 1 0.127867 0.684429 0.626731 11.00000 0.01902 0.01431 = 0.01861 0.00124 0.00536 0.00271 C21 1 0.063356 0.691270 0.713327 11.00000 0.02325 0.01820 = 0.02221 0.00107 0.01108 0.00271 AFIX 44 H21 2 -0.023656 0.641236 0.708427 11.00000 -1.20000 AFIX 0 C22 1 0.136514 0.776809 0.806714 11.00000 0.02684 0.02435 = 0.01945 0.00006 0.00937 0.00659 AFIX 44 H22 2 0.096090 0.783747 0.871183 11.00000 -1.20000 AFIX 0 C23 1 0.266579 0.854268 0.812959 11.00000 0.02591 0.02374 = 0.02067 -0.00462 0.00348 0.00388 AFIX 44 H23 2 0.315355 0.918107 0.882728 11.00000 -1.20000 AFIX 0 C24 1 0.330210 0.846350 0.727227 11.00000 0.01919 0.02140 = 0.02073 -0.00241 0.00251 0.00127 AFIX 44 H24 2 0.426365 0.903856 0.732581 11.00000 -1.20000 AFIX 0 C25 1 0.260167 0.757821 0.632758 11.00000 0.01633 0.01350 = 0.01864 0.00086 0.00369 0.00229 C26 1 -0.043972 0.517890 0.480013 11.00000 0.01998 0.01855 = 0.02886 -0.00487 0.01005 -0.00357 AFIX 138 H26A 2 -0.042617 0.453766 0.539309 11.00000 -1.50000 H26B 2 -0.037144 0.467616 0.415494 11.00000 -1.50000 H26C 2 -0.135577 0.569956 0.457300 11.00000 -1.50000 AFIX 0 HKLF 5 REM RuSk-15-39 in P2(1) REM wR2 = 0.103161, GooF = S = 1.06418, Restrained GooF = 1.06412 for all data REM R1 = 0.036150 for 8517 Fo > 4sig(Fo) and 0.036350 for all 8582 data REM 309 parameters refined using 1 restraints END WGHT 0.0778 0.0762 REM Highest difference peak 0.276, deepest hole -0.204, 1-sigma level 0.047 Q1 1 0.0432 0.6232 0.2046 11.00000 0.05 0.28 Q2 1 0.1846 0.6165 0.4154 11.00000 0.05 0.26 Q3 1 0.5587 0.4978 0.5593 11.00000 0.05 0.24 Q4 1 0.4537 0.3798 0.6897 11.00000 0.05 0.24 Q5 1 0.1242 0.6369 0.3009 11.00000 0.05 0.21 Q6 1 0.4317 0.1805 1.0019 11.00000 0.05 0.21 Q7 1 0.3495 0.3640 0.8376 11.00000 0.05 0.21 Q8 1 0.3638 0.3949 0.4771 11.00000 0.05 0.20 Q9 1 0.0673 0.6064 0.3180 11.00000 0.05 0.19 Q10 1 0.5676 0.2325 0.8551 11.00000 0.05 0.19 Q11 1 0.7015 0.5170 0.7794 11.00000 0.05 0.18 Q12 1 0.0845 0.7031 0.6622 11.00000 0.05 0.17 Q13 1 0.0979 0.4499 0.0818 11.00000 0.05 0.17 Q14 1 0.2452 0.4675 0.2796 11.00000 0.05 0.17 Q15 1 0.0368 0.4323 0.6401 11.00000 0.05 0.17 Q16 1 0.3862 0.3594 0.7566 11.00000 0.05 0.16 Q17 1 0.4207 0.3589 0.5812 11.00000 0.05 0.16 ; _shelx_res_checksum 79187 _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 1.357 _oxdiff_exptl_absorpt_empirical_full_min 0.599 _oxdiff_twin_integration_method simultaneous _oxdiff_twin_items 2 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -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 N1 N 0.4577(2) 0.3927(2) 0.63314(14) 0.0185(4) Uani 1 1 d . . . . . C1 C 0.5712(2) 0.4794(2) 0.61989(18) 0.0211(4) Uani 1 1 d . . . . . C2 C 0.5271(2) 0.5158(2) 0.49329(17) 0.0186(4) Uani 1 1 d . . . . . H2A H 0.613(2) 0.4964(5) 0.4646(7) 0.022 Uiso 1 1 calc R U . . . H2B H 0.4986(7) 0.618(2) 0.4800(4) 0.022 Uiso 1 1 calc R U . . . C3 C 0.3905(2) 0.4216(2) 0.43089(17) 0.0164(4) Uani 1 1 d . . . . . H3 H 0.4278(13) 0.343(3) 0.3984(11) 0.020 Uiso 1 1 calc R U . . . C4 C 0.3422(2) 0.3638(2) 0.52861(16) 0.0172(4) Uani 1 1 d . . . . . O1 O 0.6817(2) 0.5174(2) 0.69880(14) 0.0321(4) Uani 1 1 d . . . . . O2 O 0.22837(17) 0.29965(18) 0.51913(13) 0.0219(3) Uani 1 1 d . . . . . C5 C 0.4546(2) 0.3377(2) 0.74087(17) 0.0191(4) Uani 1 1 d . . . . . C6 C 0.5661(2) 0.2452(3) 0.80369(18) 0.0221(4) Uani 1 1 d . . . . . H6 H 0.647(3) 0.2238(8) 0.7793(9) 0.027 Uiso 1 1 calc R U . . . C7 C 0.5562(3) 0.1840(3) 0.90394(18) 0.0236(4) Uani 1 1 d . . . . . H7 H 0.636(3) 0.117(2) 0.9490(16) 0.028 Uiso 1 1 calc R U . . . C8 C 0.4356(3) 0.2158(2) 0.94207(18) 0.0210(4) Uani 1 1 d . . . . . C9 C 0.3279(3) 0.3129(3) 0.87879(19) 0.0226(4) Uani 1 1 d . . . . . H9 H 0.245(3) 0.3389(9) 0.9056(9) 0.027 Uiso 1 1 calc R U . . . C10 C 0.3359(3) 0.3735(3) 0.77840(19) 0.0222(4) Uani 1 1 d . . . . . H10 H 0.265(3) 0.435(3) 0.7384(17) 0.027 Uiso 1 1 calc R U . . . C11 C 0.4220(3) 0.1462(3) 1.04826(18) 0.0254(5) Uani 1 1 d . . . . . H11A H 0.339(3) 0.1929(19) 1.0692(12) 0.038 Uiso 1 1 calc R U . . . H11B H 0.521(2) 0.156(2) 1.1147(16) 0.038 Uiso 1 1 calc R U . . . H11C H 0.397(3) 0.043(2) 1.0318(7) 0.038 Uiso 1 1 calc R U . . . C12 C 0.2610(2) 0.4865(2) 0.33404(17) 0.0166(4) Uani 1 1 d . . . . . C13 C 0.2293(2) 0.4374(2) 0.22183(18) 0.0185(4) Uani 1 1 d . . . . . H13 H 0.289(2) 0.365(3) 0.2079(5) 0.022 Uiso 1 1 calc R U . . . C14 C 0.1103(2) 0.4934(2) 0.12953(17) 0.0186(4) Uani 1 1 d . . . . . C15 C 0.0212(2) 0.6007(2) 0.14846(17) 0.0198(4) Uani 1 1 d . . . . . H15 H -0.056(3) 0.6395(14) 0.088(2) 0.024 Uiso 1 1 calc R U . . . C16 C 0.0513(2) 0.6483(2) 0.26104(18) 0.0195(4) Uani 1 1 d . . . . . H16 H -0.012(2) 0.721(3) 0.2751(5) 0.023 Uiso 1 1 calc R U . . . C17 C 0.1694(2) 0.5935(2) 0.35395(16) 0.0161(4) Uani 1 1 d . . . . . O3 O 0.08787(18) 0.43315(19) 0.02403(12) 0.0237(3) Uani 1 1 d . . . . . C18 C -0.0447(3) 0.4757(3) -0.06995(17) 0.0246(5) Uani 1 1 d . . . . . H18A H -0.0477(13) 0.427(2) -0.1396(16) 0.037 Uiso 1 1 calc R U . . . H18B H -0.0414(12) 0.576(2) -0.0814(12) 0.037 Uiso 1 1 calc R U . . . H18C H -0.134(2) 0.452(2) -0.0520(9) 0.037 Uiso 1 1 calc R U . . . C19 C 0.1881(2) 0.6462(2) 0.47163(17) 0.0159(4) Uani 1 1 d . . . . . N2 N 0.0842(2) 0.61364(19) 0.52293(15) 0.0173(3) Uani 1 1 d . . . . . N3 N 0.2958(2) 0.7321(2) 0.53400(14) 0.0178(4) Uani 1 1 d . . . . . C20 C 0.1279(2) 0.6844(2) 0.62673(17) 0.0176(4) Uani 1 1 d . . . . . C21 C 0.0634(3) 0.6913(2) 0.71333(18) 0.0204(4) Uani 1 1 d . . . . . H21 H -0.024(3) 0.6412(19) 0.7084(3) 0.024 Uiso 1 1 calc R U . . . C22 C 0.1365(3) 0.7768(2) 0.80671(18) 0.0232(4) Uani 1 1 d . . . . . H22 H 0.0961(13) 0.7837(3) 0.871(2) 0.028 Uiso 1 1 calc R U . . . C23 C 0.2666(3) 0.8543(3) 0.81296(18) 0.0246(4) Uani 1 1 d . . . . . H23 H 0.3154(17) 0.918(2) 0.883(2) 0.030 Uiso 1 1 calc R U . . . C24 C 0.3302(2) 0.8464(2) 0.72723(18) 0.0216(4) Uani 1 1 d . . . . . H24 H 0.426(3) 0.9039(19) 0.7326(2) 0.026 Uiso 1 1 calc R U . . . C25 C 0.2602(2) 0.7578(2) 0.63276(17) 0.0168(4) Uani 1 1 d . . . . . C26 C -0.0440(3) 0.5179(3) 0.48001(19) 0.0220(4) Uani 1 1 d . . . . . H26A H -0.0426(14) 0.454(2) 0.5393(14) 0.033 Uiso 1 1 calc R U . . . H26B H -0.0371(13) 0.4676(19) 0.4155(18) 0.033 Uiso 1 1 calc R U . . . H26C H -0.1356(19) 0.5700(11) 0.4573(17) 0.033 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 N1 0.0182(8) 0.0179(9) 0.0174(8) 0.0002(6) 0.0035(6) -0.0006(7) C1 0.0185(9) 0.0212(11) 0.0219(9) 0.0004(8) 0.0048(7) 0.0000(8) C2 0.0162(9) 0.0184(10) 0.0203(9) 0.0004(7) 0.0051(7) -0.0010(7) C3 0.0159(9) 0.0140(9) 0.0190(8) -0.0005(7) 0.0056(7) -0.0002(7) C4 0.0172(9) 0.0142(9) 0.0184(8) -0.0002(7) 0.0040(7) 0.0015(7) O1 0.0253(9) 0.0407(11) 0.0237(7) 0.0007(7) 0.0000(6) -0.0139(8) O2 0.0193(7) 0.0204(8) 0.0237(7) 0.0008(6) 0.0046(5) -0.0035(6) C5 0.0204(10) 0.0180(10) 0.0180(9) -0.0012(7) 0.0054(7) -0.0012(8) C6 0.0212(10) 0.0256(12) 0.0193(9) -0.0011(8) 0.0067(8) 0.0045(9) C7 0.0263(11) 0.0236(11) 0.0192(9) 0.0017(8) 0.0059(8) 0.0058(9) C8 0.0242(10) 0.0197(11) 0.0190(9) -0.0029(7) 0.0072(8) -0.0028(8) C9 0.0217(10) 0.0218(11) 0.0256(10) -0.0015(8) 0.0098(8) -0.0002(9) C10 0.0208(10) 0.0202(10) 0.0248(10) 0.0015(8) 0.0067(8) 0.0026(8) C11 0.0324(12) 0.0237(11) 0.0197(9) -0.0014(8) 0.0087(8) -0.0042(9) C12 0.0145(9) 0.0163(9) 0.0188(8) 0.0003(7) 0.0057(7) -0.0013(8) C13 0.0162(9) 0.0185(10) 0.0214(9) -0.0020(8) 0.0073(7) -0.0003(8) C14 0.0183(9) 0.0205(10) 0.0168(8) -0.0019(8) 0.0057(7) -0.0041(8) C15 0.0185(9) 0.0202(10) 0.0184(9) 0.0018(8) 0.0034(7) 0.0015(8) C16 0.0204(10) 0.0174(10) 0.0204(9) 0.0002(7) 0.0067(8) 0.0040(8) C17 0.0172(9) 0.0140(9) 0.0171(8) -0.0002(7) 0.0060(7) -0.0006(7) O3 0.0230(7) 0.0301(9) 0.0165(7) -0.0043(6) 0.0050(6) 0.0036(7) C18 0.0273(11) 0.0279(12) 0.0157(9) -0.0025(8) 0.0037(8) 0.0026(9) C19 0.0170(9) 0.0121(9) 0.0176(9) 0.0004(7) 0.0049(7) 0.0021(7) N2 0.0166(8) 0.0151(8) 0.0203(8) -0.0018(6) 0.0065(6) -0.0009(6) N3 0.0181(8) 0.0166(9) 0.0173(7) -0.0008(6) 0.0046(6) -0.0011(7) C20 0.0190(9) 0.0143(10) 0.0186(9) 0.0012(7) 0.0054(7) 0.0027(7) C21 0.0233(10) 0.0182(10) 0.0222(9) 0.0011(8) 0.0111(8) 0.0027(8) C22 0.0268(11) 0.0244(12) 0.0195(9) 0.0001(8) 0.0094(8) 0.0066(9) C23 0.0259(10) 0.0237(11) 0.0207(9) -0.0046(8) 0.0035(8) 0.0039(9) C24 0.0192(9) 0.0214(11) 0.0207(9) -0.0024(8) 0.0025(7) 0.0013(8) C25 0.0163(9) 0.0135(9) 0.0186(8) 0.0009(7) 0.0037(7) 0.0023(7) C26 0.0200(10) 0.0185(11) 0.0289(10) -0.0049(7) 0.0100(8) -0.0036(8) 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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -1 2 0.1376 -1 -2 2 0.1384 -1 2 0 0.1052 -1 0 1 0.1016 2 2 -1 0.1131 -1 0 0 0.0723 -1 0 -1 0.0912 0 0 1 0.1239 1 0 0 0.0802 1 0 1 0.1007 0 0 -1 0.1128 2 -1 0 0.0875 2 1 0 0.0901 2 0 -1 0.0838 1 0 -2 0.1112 0 1 0 0.1118 -1 0 2 0.1086 1 -2 0 0.1112 -2 -1 0 0.0773 -2 1 0 0.0684 -1 -2 0 0.1193 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C5 125.48(17) . . ? C4 N1 C1 112.94(16) . . ? C4 N1 C5 121.57(17) . . ? N1 C1 C2 107.80(17) . . ? O1 C1 N1 124.10(19) . . ? O1 C1 C2 128.1(2) . . ? C1 C2 H2A 110.6 . . ? C1 C2 H2B 110.6 . . ? C1 C2 C3 105.53(16) . . ? H2A C2 H2B 108.8 . . ? C3 C2 H2A 110.6 . . ? C3 C2 H2B 110.6 . . ? C2 C3 H3 107.3 . . ? C4 C3 C2 103.88(16) . . ? C4 C3 H3 107.3 . . ? C12 C3 C2 117.57(18) . . ? C12 C3 H3 107.3 . . ? C12 C3 C4 113.04(16) . . ? N1 C4 C3 107.94(17) . . ? O2 C4 N1 124.95(18) . . ? O2 C4 C3 127.05(18) . . ? C6 C5 N1 119.76(19) . . ? C6 C5 C10 120.7(2) . . ? C10 C5 N1 119.45(19) . . ? C5 C6 H6 120.3 . . ? C5 C6 C7 119.4(2) . . ? C7 C6 H6 120.3 . . ? C6 C7 H7 119.5 . . ? C6 C7 C8 120.9(2) . . ? C8 C7 H7 119.5 . . ? C7 C8 C11 121.0(2) . . ? C9 C8 C7 118.2(2) . . ? C9 C8 C11 120.8(2) . . ? C8 C9 H9 119.3 . . ? C10 C9 C8 121.4(2) . . ? C10 C9 H9 119.3 . . ? C5 C10 C9 119.3(2) . . ? C5 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C3 119.00(18) . . ? C13 C12 C17 118.81(18) . . ? C17 C12 C3 122.18(17) . . ? C12 C13 H13 119.4 . . ? C12 C13 C14 121.1(2) . . ? C14 C13 H13 119.4 . . ? C15 C14 C13 120.26(19) . . ? O3 C14 C13 115.51(19) . . ? O3 C14 C15 124.21(19) . . ? C14 C15 H15 120.7 . . ? C14 C15 C16 118.61(19) . . ? C16 C15 H15 120.7 . . ? C15 C16 H16 119.1 . . ? C15 C16 C17 121.82(19) . . ? C17 C16 H16 119.1 . . ? C12 C17 C19 122.69(18) . . ? C16 C17 C12 119.34(17) . . ? C16 C17 C19 117.89(18) . . ? C14 O3 C18 117.00(17) . . ? O3 C18 H18A 109.5 . . ? O3 C18 H18B 109.5 . . ? O3 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C19 C17 120.68(18) . . ? N3 C19 C17 125.80(18) . . ? N3 C19 N2 113.42(17) . . ? C19 N2 C20 106.59(17) . . ? C19 N2 C26 127.34(17) . . ? C20 N2 C26 126.01(17) . . ? C19 N3 C25 104.47(17) . . ? N2 C20 C21 131.5(2) . . ? N2 C20 C25 105.53(17) . . ? C21 C20 C25 123.0(2) . . ? C20 C21 H21 122.0 . . ? C22 C21 C20 116.1(2) . . ? C22 C21 H21 122.0 . . ? C21 C22 H22 119.1 . . ? C21 C22 C23 121.8(2) . . ? C23 C22 H22 119.1 . . ? C22 C23 H23 119.1 . . ? C24 C23 C22 121.7(2) . . ? C24 C23 H23 119.1 . . ? C23 C24 H24 121.2 . . ? C23 C24 C25 117.6(2) . . ? C25 C24 H24 121.2 . . ? N3 C25 C20 109.98(18) . . ? N3 C25 C24 130.2(2) . . ? C24 C25 C20 119.74(19) . . ? N2 C26 H26A 109.5 . . ? N2 C26 H26B 109.5 . . ? N2 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 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 N1 C1 1.403(3) . ? N1 C4 1.396(3) . ? N1 C5 1.436(2) . ? C1 C2 1.509(3) . ? C1 O1 1.208(3) . ? C2 H2A 1.01(2) . ? C2 H2B 1.01(2) . ? C2 C3 1.538(3) . ? C3 H3 0.97(3) . ? C3 C4 1.527(3) . ? C3 C12 1.512(3) . ? C4 O2 1.203(3) . ? C5 C6 1.384(3) . ? C5 C10 1.390(3) . ? C6 H6 0.94(4) . ? C6 C7 1.397(3) . ? C7 H7 1.00(4) . ? C7 C8 1.401(3) . ? C8 C9 1.394(3) . ? C8 C11 1.511(3) . ? C9 H9 0.98(3) . ? C9 C10 1.390(3) . ? C10 H10 0.89(4) . ? C11 H11A 1.01(2) . ? C11 H11B 1.01(2) . ? C11 H11C 1.01(2) . ? C12 C13 1.391(3) . ? C12 C17 1.409(3) . ? C13 H13 0.94(3) . ? C13 C14 1.397(3) . ? C14 C15 1.391(3) . ? C14 O3 1.368(2) . ? C15 H15 0.92(3) . ? C15 C16 1.392(3) . ? C16 H16 0.97(3) . ? C16 C17 1.393(3) . ? C17 C19 1.486(3) . ? O3 C18 1.436(3) . ? C18 H18A 0.97(2) . ? C18 H18B 0.97(2) . ? C18 H18C 0.97(2) . ? C19 N2 1.369(3) . ? C19 N3 1.322(3) . ? N2 C20 1.377(3) . ? N2 C26 1.457(3) . ? N3 C25 1.390(3) . ? C20 C21 1.398(3) . ? C20 C25 1.406(3) . ? C21 H21 0.93(3) . ? C21 C22 1.383(3) . ? C22 H22 0.99(3) . ? C22 C23 1.407(4) . ? C23 H23 1.02(4) . ? C23 C24 1.383(3) . ? C24 H24 1.04(3) . ? C24 C25 1.403(3) . ? C26 H26A 0.95(2) . ? C26 H26B 0.95(2) . ? C26 H26C 0.95(2) . ? 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 N1 C1 C2 C3 -9.4(2) . . . . ? N1 C5 C6 C7 -175.3(2) . . . . ? N1 C5 C10 C9 175.8(2) . . . . ? C1 N1 C4 C3 7.7(2) . . . . ? C1 N1 C4 O2 -174.9(2) . . . . ? C1 N1 C5 C6 -64.1(3) . . . . ? C1 N1 C5 C10 118.6(2) . . . . ? C1 C2 C3 C4 13.3(2) . . . . ? C1 C2 C3 C12 139.03(18) . . . . ? C2 C3 C4 N1 -13.0(2) . . . . ? C2 C3 C4 O2 169.7(2) . . . . ? C2 C3 C12 C13 114.7(2) . . . . ? C2 C3 C12 C17 -66.4(2) . . . . ? C3 C12 C13 C14 179.64(18) . . . . ? C3 C12 C17 C16 -179.61(19) . . . . ? C3 C12 C17 C19 -2.9(3) . . . . ? C4 N1 C1 C2 1.2(2) . . . . ? C4 N1 C1 O1 -179.9(2) . . . . ? C4 N1 C5 C6 116.4(2) . . . . ? C4 N1 C5 C10 -60.9(3) . . . . ? C4 C3 C12 C13 -124.2(2) . . . . ? C4 C3 C12 C17 54.7(3) . . . . ? O1 C1 C2 C3 171.7(2) . . . . ? C5 N1 C1 C2 -178.34(19) . . . . ? C5 N1 C1 O1 0.6(4) . . . . ? C5 N1 C4 C3 -172.74(17) . . . . ? C5 N1 C4 O2 4.6(3) . . . . ? C5 C6 C7 C8 -0.5(3) . . . . ? C6 C5 C10 C9 -1.5(3) . . . . ? C6 C7 C8 C9 -1.6(3) . . . . ? C6 C7 C8 C11 178.0(2) . . . . ? C7 C8 C9 C10 2.1(3) . . . . ? C8 C9 C10 C5 -0.6(3) . . . . ? C10 C5 C6 C7 2.0(3) . . . . ? C11 C8 C9 C10 -177.4(2) . . . . ? C12 C3 C4 N1 -141.53(18) . . . . ? C12 C3 C4 O2 41.2(3) . . . . ? C12 C13 C14 C15 0.3(3) . . . . ? C12 C13 C14 O3 -178.03(19) . . . . ? C12 C17 C19 N2 -107.4(2) . . . . ? C12 C17 C19 N3 76.5(3) . . . . ? C13 C12 C17 C16 -0.7(3) . . . . ? C13 C12 C17 C19 175.95(19) . . . . ? C13 C14 C15 C16 -1.4(3) . . . . ? C13 C14 O3 C18 172.38(19) . . . . ? C14 C15 C16 C17 1.4(3) . . . . ? C15 C14 O3 C18 -5.9(3) . . . . ? C15 C16 C17 C12 -0.3(3) . . . . ? C15 C16 C17 C19 -177.1(2) . . . . ? C16 C17 C19 N2 69.3(3) . . . . ? C16 C17 C19 N3 -106.8(2) . . . . ? C17 C12 C13 C14 0.7(3) . . . . ? C17 C19 N2 C20 -176.34(18) . . . . ? C17 C19 N2 C26 6.3(3) . . . . ? C17 C19 N3 C25 176.22(19) . . . . ? O3 C14 C15 C16 176.9(2) . . . . ? C19 N2 C20 C21 179.1(2) . . . . ? C19 N2 C20 C25 -0.2(2) . . . . ? C19 N3 C25 C20 0.0(2) . . . . ? C19 N3 C25 C24 -176.7(2) . . . . ? N2 C19 N3 C25 -0.1(2) . . . . ? N2 C20 C21 C22 -178.5(2) . . . . ? N2 C20 C25 N3 0.1(2) . . . . ? N2 C20 C25 C24 177.21(19) . . . . ? N3 C19 N2 C20 0.2(2) . . . . ? N3 C19 N2 C26 -177.1(2) . . . . ? C20 C21 C22 C23 1.1(3) . . . . ? C21 C20 C25 N3 -179.26(19) . . . . ? C21 C20 C25 C24 -2.2(3) . . . . ? C21 C22 C23 C24 -1.5(4) . . . . ? C22 C23 C24 C25 0.1(3) . . . . ? C23 C24 C25 N3 178.1(2) . . . . ? C23 C24 C25 C20 1.7(3) . . . . ? C25 C20 C21 C22 0.7(3) . . . . ? C26 N2 C20 C21 -3.5(4) . . . . ? C26 N2 C20 C25 177.20(19) . . . . ? 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 0.5346(12) 19766 3896 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 2 0.4654(12) 19717 3896 nmt 0.9999 0.0006 0.5260 0.0005 -1.0001 -0.0002 -0.0005 0.0001 -1.0002 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -0.0004 -1.0005 2.0006 0.1633 0.2372 -0.1196 -1.0005 -2.0008 2.0010 0.0903 0.4065 0.0311 -1.0004 1.9999 0.0011 -0.3105 -0.1428 -0.1355 -1.0005 -0.0004 1.0010 -0.1101 0.1318 -0.0522 2.0005 2.0008 -1.0012 0.1039 -0.4051 -0.1939 -1.0002 -0.0002 0.0006 -0.1522 0.0652 0.0553 -1.0000 -0.0000 -0.9998 -0.1942 -0.0014 0.1628 -0.0002 -0.0002 1.0004 0.0421 0.0666 -0.1075 1.0002 0.0002 -0.0006 0.1522 -0.0652 -0.0553 1.0000 0.0000 0.9998 0.1942 0.0014 -0.1628 0.0002 0.0002 -1.0004 -0.0421 -0.0666 0.1075 2.0006 -0.9996 -0.0015 0.3835 -0.0264 -0.0152 2.0004 1.0005 -0.0010 0.2252 -0.2345 -0.2060 2.0007 0.0007 -1.0017 0.2623 -0.1970 -0.0031 1.0007 0.0006 -2.0015 0.0681 -0.1984 0.1597 -0.0001 1.0001 0.0003 -0.0792 -0.1040 -0.0954 -1.0007 -0.0006 2.0015 -0.0681 0.1984 -0.1597 1.0004 -1.9999 -0.0011 0.3105 0.1428 0.1355 -2.0004 -1.0005 0.0010 -0.2252 0.2345 0.2060 -2.0006 0.9996 0.0015 -0.3835 0.0264 0.0152 -1.0000 -2.0004 0.0001 0.0062 0.2733 0.2461