#------------------------------------------------------------------------------ #$Date: 2024-10-12 01:11:25 +0300 (Sat, 12 Oct 2024) $ #$Revision: 295437 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/28/1572860.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_1572860 loop_ _publ_author_name 'Zhu, Jiaxuan' 'Wu, Wenbo' 'Qi, Haoqiang' 'Yao, Yutong' 'Yu, Hui' 'Huang, Xin' 'Wang, Na' 'Wang, Ting' 'Hao, Hongxun' _publ_section_title ; Dynamic organic crystal as exceptionally efficient artificial natural light-harvesting actuator ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC05684A _journal_year 2024 _chemical_formula_moiety 'C16 H16 Cl N3 O' _chemical_formula_sum 'C16 H16 Cl N3 O' _chemical_formula_weight 301.77 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2024-04-21 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2024-08-11 deposited with the CCDC. 2024-10-07 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 96.635(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.9184(5) _cell_length_b 12.9302(4) _cell_length_c 7.6631(3) _cell_measurement_reflns_used 4315 _cell_measurement_temperature 113.15 _cell_measurement_theta_max 31.1650 _cell_measurement_theta_min 2.0770 _cell_volume 1468.30(9) _computing_cell_refinement 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 113.15 _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.876 _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 -78.00 -8.00 1.00 35.00 -- -13.40 -57.00 30.00 70 2 \w -28.00 50.00 1.00 35.00 -- -13.40 38.00-150.00 78 3 \w -93.00 -3.00 1.00 35.00 -- -13.40 -57.00 120.00 90 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku MM007 Saturn944+' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0376945000 _diffrn_orient_matrix_UB_12 0.0336201000 _diffrn_orient_matrix_UB_13 -0.0144167000 _diffrn_orient_matrix_UB_21 -0.0294116000 _diffrn_orient_matrix_UB_22 -0.0424945000 _diffrn_orient_matrix_UB_23 0.0070336000 _diffrn_orient_matrix_UB_31 0.0019655000 _diffrn_orient_matrix_UB_32 0.0085088000 _diffrn_orient_matrix_UB_33 0.0918365000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_unetI/netI 0.0650 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.876 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 12460 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.876 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.554 _diffrn_reflns_theta_min 2.090 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.262 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.29565 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)' _exptl_crystal_density_diffrn 1.365 _exptl_crystal_description block _exptl_crystal_F_000 632 _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.470 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.070 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 196 _refine_ls_number_reflns 4677 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.079 _refine_ls_R_factor_all 0.0883 _refine_ls_R_factor_gt 0.0643 _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^)+(0.0501P)^2^+0.6811P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1280 _refine_ls_wR_factor_ref 0.1391 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3702 _reflns_number_total 4677 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc05684a11.cif _cod_data_source_block r20240420a _cod_database_code 1572860 _shelx_shelxl_version_number 2018/3 _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 0.949 _shelx_estimated_absorpt_t_min 0.911 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances N1-H1 0.9 with sigma of 0.01 3.a Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14) 3.b Idealised Me refined as rotating group: C15(H15A,H15B,H15C), C16(H16A,H16B,H16C) ; _shelx_res_file ; TITL r20240420a P 1 c 1 R = 0.08 New:P21/c r20240420a.res created by SHELXL-2018/3 at 16:13:46 on 21-Apr-2024 CELL 0.71073 14.9184 12.9302 7.6631 90 96.635 90 ZERR 4 0.0005 0.0004 0.0003 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl N O UNIT 64 64 4 12 4 DFIX 0.9 0.01 N1 H1 L.S. 5 PLAN 5 SIZE 0.36 0.25 0.2 TEMP -160 CONF htab MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.050100 0.681100 FVAR 0.56447 CL1 3 0.193175 -0.085689 -0.011382 11.00000 0.02956 0.03229 = 0.03234 -0.00149 -0.01675 -0.00746 O1 5 -0.106908 -0.138543 -0.738515 11.00000 0.02291 0.01714 = 0.01466 0.00221 0.00008 -0.00327 N1 4 -0.172126 -0.228029 -0.529653 11.00000 0.01358 0.01802 = 0.01145 0.00034 -0.00297 -0.00171 H1 2 -0.163095 -0.263777 -0.429224 11.00000 0.02573 N2 4 -0.249528 -0.247976 -0.642821 11.00000 0.01207 0.01813 = 0.01342 -0.00217 -0.00077 -0.00020 N3 4 -0.641523 -0.413768 -0.959845 11.00000 0.01625 0.02378 = 0.01972 -0.00051 -0.00181 -0.00642 C1 1 0.105633 -0.107361 -0.178092 11.00000 0.02151 0.01304 = 0.02367 0.00072 -0.00896 -0.00466 C2 1 0.126494 -0.126341 -0.346603 11.00000 0.01662 0.02081 = 0.02796 -0.00137 -0.00058 -0.00473 AFIX 43 H2 2 0.187553 -0.127674 -0.370587 11.00000 -1.20000 AFIX 0 C3 1 0.056693 -0.143431 -0.480269 11.00000 0.01767 0.01732 = 0.02031 -0.00262 0.00242 -0.00394 AFIX 43 H3 2 0.069943 -0.155396 -0.596890 11.00000 -1.20000 AFIX 0 C4 1 -0.032707 -0.143029 -0.443372 11.00000 0.01621 0.00945 = 0.01660 -0.00057 -0.00204 -0.00223 C5 1 -0.051574 -0.123057 -0.272854 11.00000 0.01822 0.01108 = 0.01888 -0.00065 0.00077 -0.00110 AFIX 43 H5 2 -0.112512 -0.121468 -0.248143 11.00000 -1.20000 AFIX 0 C6 1 0.017676 -0.105363 -0.137912 11.00000 0.02679 0.01181 = 0.01678 -0.00276 -0.00276 -0.00174 AFIX 43 H6 2 0.004775 -0.092275 -0.021404 11.00000 -1.20000 AFIX 0 C7 1 -0.106493 -0.168201 -0.585439 11.00000 0.01368 0.01254 = 0.01407 -0.00167 0.00071 0.00108 C8 1 -0.298143 -0.322396 -0.593371 11.00000 0.01438 0.01534 = 0.01178 -0.00050 0.00037 0.00248 AFIX 43 H8 2 -0.276301 -0.362874 -0.494012 11.00000 -1.20000 AFIX 0 C9 1 -0.386363 -0.345173 -0.688302 11.00000 0.01263 0.01580 = 0.01247 -0.00240 0.00312 -0.00012 C10 1 -0.431021 -0.274885 -0.806640 11.00000 0.01423 0.01421 = 0.01469 -0.00039 0.00376 -0.00162 AFIX 43 H10 2 -0.403363 -0.210242 -0.825136 11.00000 -1.20000 AFIX 0 C11 1 -0.514055 -0.296767 -0.897210 11.00000 0.01509 0.01623 = 0.01491 0.00093 0.00199 0.00039 AFIX 43 H11 2 -0.542197 -0.247526 -0.977727 11.00000 -1.20000 AFIX 0 C12 1 -0.557929 -0.391629 -0.871821 11.00000 0.01307 0.01906 = 0.01449 -0.00354 0.00335 -0.00239 C13 1 -0.513275 -0.461964 -0.750969 11.00000 0.01862 0.01728 = 0.01869 -0.00034 0.00460 -0.00593 AFIX 43 H13 2 -0.540832 -0.526437 -0.730813 11.00000 -1.20000 AFIX 0 C14 1 -0.429923 -0.438522 -0.661263 11.00000 0.01960 0.01591 = 0.01459 0.00172 0.00302 -0.00088 AFIX 43 H14 2 -0.401647 -0.486967 -0.579424 11.00000 -1.20000 AFIX 0 C15 1 -0.678650 -0.517417 -0.945275 11.00000 0.01751 0.02369 = 0.02934 -0.00741 0.00438 -0.00775 AFIX 137 H15A 2 -0.634520 -0.568762 -0.974929 11.00000 -1.50000 H15B 2 -0.734130 -0.524159 -1.026423 11.00000 -1.50000 H15C 2 -0.692231 -0.528933 -0.824688 11.00000 -1.50000 AFIX 0 C16 1 -0.677576 -0.348951 -1.105370 11.00000 0.01757 0.03536 = 0.02103 0.00066 -0.00366 -0.00514 AFIX 137 H16A 2 -0.685662 -0.278405 -1.063134 11.00000 -1.50000 H16B 2 -0.735920 -0.376470 -1.156828 11.00000 -1.50000 H16C 2 -0.635544 -0.348111 -1.194640 11.00000 -1.50000 AFIX 0 HKLF 4 1 -1 0 0 0 1 0 0 0 -1 REM r20240420a P 1 c 1 R = 0.08 New:P21/c REM wR2 = 0.1391, GooF = S = 1.079, Restrained GooF = 1.079 for all data REM R1 = 0.0643 for 3702 Fo > 4sig(Fo) and 0.0883 for all 4677 data REM 196 parameters refined using 1 restraints END WGHT 0.0500 0.6824 REM Instructions for potential hydrogen bonds EQIV $1 x, -y-1/2, z+1/2 HTAB N1 O1_$1 HTAB N1 N2_$1 EQIV $2 x-1, -y-1/2, z-3/2 HTAB C16 Cl1_$2 REM Highest difference peak 0.470, deepest hole -0.399, 1-sigma level 0.070 Q1 1 -0.3486 -0.3241 -0.6380 11.00000 0.05 0.47 Q2 1 -0.0706 -0.1417 -0.5105 11.00000 0.05 0.47 Q3 1 0.0915 -0.1454 -0.4058 11.00000 0.05 0.43 Q4 1 -0.4740 -0.2886 -0.8539 11.00000 0.05 0.43 Q5 1 -0.3993 -0.4023 -0.7017 11.00000 0.05 0.42 ; _shelx_res_checksum 6352 _shelx_hkl_file ; -2 0 0 491.04 15.75 2 0 0 491.06 15.80 -3 0 0 242.83 9.35 3 0 0 240.56 9.37 4 0 0 237.62 9.97 -4 0 0 240.67 9.97 5 0 0 68.87 4.84 -5 0 0 69.88 4.80 6 0 0 116.28 7.05 -6 0 0 107.30 6.80 -7 0 0 26.16 3.44 7 0 0 23.26 3.18 8 0 0 285.17 14.01 -8 0 0 300.70 14.43 -9 0 0 86.89 7.25 9 0 0 89.60 7.27 10 0 0 232.35 13.36 -10 0 0 258.23 14.15 -11 0 0 29.49 4.61 11 0 0 28.52 4.21 -12 0 0 20.99 4.04 12 0 0 29.75 4.75 13 0 0 694.90 29.70 14 0 0 258.66 16.00 15 0 0 108.20 9.92 16 0 0 435.25 23.20 17 0 0 4.28 2.52 17 0 0 0.45 1.87 18 0 0 8.21 4.45 19 0 0 7.57 3.20 20 0 0 10.16 4.95 1 -1 0 504.40 6.86 -1 1 0 507.00 5.85 -1 -1 0 454.00 5.53 2 1 0 5.05 0.87 -2 -1 0 4.06 0.76 2 -1 0 4.47 0.85 2 -1 0 4.40 0.83 -2 1 0 5.12 0.93 3 1 0 82.15 4.40 3 -1 0 84.26 4.43 -3 1 0 77.24 4.30 -3 -1 0 76.40 4.09 4 -1 0 16.58 2.14 -4 -1 0 14.52 1.93 -4 1 0 12.22 1.88 4 1 0 14.58 1.91 5 1 0 217.92 10.02 5 -1 0 219.17 9.84 -5 -1 0 211.31 9.62 -5 1 0 209.33 9.94 -6 -1 0 71.42 5.29 -6 1 0 75.19 5.54 6 -1 0 80.47 5.62 6 1 0 76.48 5.62 -7 1 0 845.96 29.85 -7 -1 0 837.33 29.44 7 -1 0 854.66 29.59 7 1 0 776.76 29.32 8 -1 0 646.18 25.44 -8 1 0 691.19 26.11 8 1 0 660.36 25.71 -8 -1 0 683.96 25.63 -9 1 0 4.09 2.17 9 1 0 6.24 1.80 -9 -1 0 3.12 1.77 9 -1 0 5.08 1.83 10 1 0 12.09 2.92 -10 -1 0 13.38 3.08 -10 1 0 12.16 3.12 10 -1 0 11.48 2.96 -11 1 0 57.37 6.39 -11 -1 0 45.04 5.47 11 1 0 64.16 6.62 11 -1 0 47.25 5.67 -12 -1 0 5.55 2.62 12 1 0 10.21 2.86 12 -1 0 10.02 2.66 13 -1 0 56.94 6.46 13 1 0 58.61 6.98 14 1 0 196.55 13.99 14 -1 0 216.09 14.25 15 1 0 35.43 5.70 15 -1 0 36.57 7.25 15 -1 0 44.25 6.40 16 1 0 119.93 11.33 16 -1 0 128.51 13.98 17 -1 0 84.83 11.69 17 1 0 124.45 11.41 18 1 0 5.81 3.08 18 -1 0 12.31 5.75 19 -1 0 9.69 5.62 19 1 0 -1.66 3.24 20 -1 0 -1.73 3.22 20 1 0 0.27 3.47 0 2 0 317.31 10.05 0 2 0 298.37 10.64 0 -2 0 302.46 10.74 0 -2 0 301.99 10.06 -1 2 0 128.98 5.51 -1 -2 0 125.02 5.34 -1 2 0 136.77 5.06 1 -2 0 130.41 5.04 1 2 0 108.83 5.09 1 -2 0 122.80 5.55 -2 -2 0 30.30 2.30 2 -2 0 33.63 2.35 -2 2 0 37.19 2.46 -2 2 0 32.01 2.55 2 2 0 31.82 2.26 2 -2 0 37.58 2.93 -3 2 0 72.99 4.19 -3 2 0 69.16 3.97 -3 -2 0 68.13 3.74 3 2 0 72.96 3.90 3 -2 0 62.58 3.96 -3 -2 0 58.62 3.62 -4 -2 0 6.98 1.18 4 -2 0 7.35 1.44 -4 2 0 6.83 1.39 4 2 0 8.75 1.65 4 -2 0 9.72 1.56 5 -2 0 88.09 6.03 -5 -2 0 92.54 5.41 -5 2 0 87.12 5.72 5 -2 0 88.80 5.45 5 2 0 93.43 5.79 6 2 0 300.13 13.36 -6 2 0 314.36 13.85 6 -2 0 284.40 13.97 6 -2 0 333.40 13.27 -6 -2 0 307.86 13.02 7 -2 0 177.75 10.39 7 -2 0 160.73 9.02 -7 2 0 186.94 10.12 7 2 0 158.01 9.24 -7 -2 0 158.09 8.94 8 -2 0 76.78 6.90 -8 -2 0 80.29 6.14 8 -2 0 75.50 6.02 8 2 0 78.96 6.60 -8 2 0 82.10 6.72 -9 -2 0 88.60 6.95 9 2 0 90.49 7.31 9 -2 0 93.24 6.97 9 -2 0 78.07 7.58 -9 2 0 93.21 7.64 10 2 0 56.37 6.02 10 -2 0 56.15 6.65 10 -2 0 57.76 5.85 -10 -2 0 63.34 6.15 -10 2 0 56.32 6.13 -11 -2 0 4.63 2.55 11 2 0 3.97 2.11 11 -2 0 4.88 2.12 -11 2 0 4.46 2.42 11 -2 0 5.83 2.43 -12 -2 0 39.22 5.26 12 2 0 36.16 5.43 12 -2 0 30.87 5.69 12 -2 0 36.40 5.09 13 -2 0 31.59 5.68 13 2 0 40.26 5.82 13 -2 0 36.81 5.34 14 2 0 34.04 5.61 14 -2 0 31.81 6.26 15 -2 0 72.04 9.91 15 2 0 82.41 8.92 16 -2 0 1.97 2.59 16 2 0 3.48 2.66 17 -2 0 19.38 5.54 17 2 0 23.31 5.14 18 -2 0 10.56 4.45 18 2 0 22.50 5.39 19 -2 0 -1.19 2.63 19 2 0 6.78 3.47 20 -2 0 6.46 4.44 20 2 0 8.18 4.95 0 -3 0 -0.02 0.55 0 3 0 0.48 0.61 0 -3 0 0.62 0.41 0 3 0 0.77 0.48 -1 3 0 4029.38 131.80 1 -3 0 5041.54 132.33 1 3 0 4863.35 133.08 1 -3 0 4893.52 133.56 -1 3 0 3997.89 132.89 -1 -3 0 5008.01 133.42 -2 3 0 601.27 19.00 2 -3 0 611.46 20.29 -2 -3 0 627.80 19.78 2 -3 0 608.42 19.17 -2 3 0 616.58 20.02 -3 3 0 205.97 9.17 -3 3 0 208.20 8.58 3 3 0 206.54 8.32 -3 -3 0 204.66 8.72 3 -3 0 207.85 8.60 -3 3 0 180.54 8.20 4 -3 0 1748.34 53.97 -4 -3 0 1844.12 53.61 -4 3 0 1712.29 53.52 -4 3 0 1751.97 54.73 4 3 0 1714.10 53.34 -4 3 0 1750.44 54.17 5 -3 0 106.45 6.60 -5 -3 0 95.30 5.84 -5 -3 0 107.32 5.92 -5 3 0 106.64 6.33 5 3 0 101.41 6.22 -6 3 0 277.42 12.52 6 -3 0 267.73 12.85 -6 -3 0 276.35 11.69 6 3 0 278.05 12.47 -6 -3 0 267.18 11.90 -7 -3 0 201.61 10.37 7 -3 0 215.93 11.71 -7 -3 0 234.36 10.36 -7 3 0 210.91 11.43 7 3 0 206.17 10.98 -8 -3 0 26.71 3.31 8 -3 0 29.33 4.05 8 3 0 26.90 3.84 -8 3 0 27.61 3.82 -9 3 0 22.50 3.79 9 3 0 22.44 3.74 -9 -3 0 27.05 3.57 9 -3 0 25.30 4.01 10 3 0 63.43 6.50 10 -3 0 59.18 6.78 -10 -3 0 57.34 5.76 -10 3 0 62.59 6.48 11 3 0 3.13 1.98 -11 -3 0 0.79 1.39 11 -3 0 0.02 1.30 -11 3 0 3.18 2.01 12 3 0 459.18 22.67 12 -3 0 457.75 24.21 -12 -3 0 510.83 20.74 -12 -3 0 465.96 21.69 13 3 0 1.78 1.63 13 -3 0 -0.79 1.78 14 -3 0 10.07 3.86 14 3 0 8.68 3.25 15 3 0 60.25 7.60 15 -3 0 52.13 8.06 16 -3 0 1.91 2.92 16 3 0 9.72 3.56 17 3 0 175.09 14.35 17 -3 0 177.39 16.78 18 3 0 45.88 7.55 18 -3 0 40.02 8.56 19 3 0 16.79 4.99 19 -3 0 17.81 6.55 20 -3 0 6.70 4.91 0 -4 0 5288.60 144.40 0 -4 0 5260.04 142.67 0 4 0 5027.45 143.81 1 4 0 3937.13 119.10 -1 -4 0 4472.76 119.98 1 4 0 3951.69 117.88 -1 4 0 3350.82 117.45 1 -4 0 4352.21 118.40 -1 4 0 4728.13 120.43 1 -4 0 4464.72 120.28 -2 4 0 795.12 25.78 2 -4 0 866.09 27.69 -2 -4 0 859.32 27.19 2 4 0 711.63 26.18 2 -4 0 775.95 25.83 -2 4 0 846.39 27.47 -3 -4 0 373.19 14.57 -3 4 0 368.82 14.93 3 -4 0 374.45 14.12 3 -4 0 384.43 15.49 3 4 0 347.33 13.95 -3 4 0 379.24 13.90 4 -4 0 999.21 31.38 4 4 0 1064.34 30.97 -4 4 0 1060.44 31.37 -4 4 0 1050.60 30.90 -4 4 0 989.47 32.17 -5 -4 0 0.35 0.61 5 -4 0 0.24 0.61 -5 4 0 -0.73 1.30 -5 4 0 0.60 0.95 5 4 0 0.31 0.82 -5 4 0 0.08 0.65 -6 4 0 47.85 4.49 -6 4 0 46.44 4.76 6 4 0 45.63 4.28 6 -4 0 47.35 4.67 -6 -4 0 48.91 4.29 -7 -4 0 104.80 6.74 -7 4 0 102.85 8.10 7 4 0 98.79 7.19 7 -4 0 108.53 7.70 -7 4 0 108.59 7.39 -8 4 0 3.86 1.72 -8 -4 0 2.35 1.03 -8 -4 0 2.38 1.18 8 4 0 0.87 1.20 8 -4 0 1.47 1.02 -9 -4 0 185.82 10.02 -9 4 0 169.01 11.01 9 -4 0 166.83 11.21 -9 -4 0 175.92 10.42 9 4 0 177.66 11.12 -10 4 0 132.23 9.83 -10 -4 0 126.71 8.88 10 -4 0 128.31 10.07 10 4 0 122.02 9.43 -10 -4 0 128.11 8.41 -11 -4 0 23.55 3.78 -11 -4 0 24.41 3.70 11 -4 0 24.15 4.49 11 4 0 19.55 3.90 12 4 0 724.63 30.76 12 -4 0 732.48 32.09 -12 -4 0 681.62 29.05 13 -4 0 191.40 14.63 13 4 0 190.11 13.53 14 4 0 29.48 5.21 14 -4 0 19.31 4.89 15 4 0 13.97 4.02 15 -4 0 5.85 3.23 16 4 0 4.58 2.78 16 -4 0 6.51 3.04 17 4 0 4.53 2.96 17 -4 0 2.97 4.03 18 4 0 25.29 6.16 18 -4 0 23.23 6.67 19 -4 0 4.35 4.96 19 4 0 0.34 2.61 20 4 0 50.30 8.24 20 -4 0 61.61 11.16 0 5 0 -0.55 0.49 0 -5 0 1.33 0.89 0 -5 0 0.19 0.72 1 -5 0 48.34 3.58 1 -5 0 43.22 4.14 1 5 0 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43.68 9.70 -5 -3 -10 8.58 4.78 -5 3 -10 2.32 3.94 -6 -3 -10 9.84 5.37 12 -4 -10 38.05 9.79 11 -4 -10 7.43 4.87 10 -4 -10 11.45 5.02 9 -4 -10 10.02 4.74 9 4 -10 11.90 4.83 8 4 -10 33.27 7.07 7 4 -10 15.66 4.52 6 4 -10 16.78 5.23 5 4 -10 1.54 2.64 5 4 -10 5.21 3.07 4 4 -10 20.56 5.84 3 4 -10 15.61 5.31 2 4 -10 79.47 11.08 1 4 -10 50.44 9.42 0 4 -10 -0.47 2.90 -1 4 -10 6.87 4.78 -2 -4 -10 33.77 6.19 -2 4 -10 43.98 9.37 -3 -4 -10 14.44 4.49 -3 4 -10 20.10 6.60 -4 -4 -10 4.22 4.11 -4 4 -10 -1.25 3.10 -5 4 -10 -4.14 4.33 7 -4 10 -0.07 2.15 8 5 -10 1.27 2.38 7 5 -10 29.92 6.71 6 5 -10 12.58 4.49 6 5 -10 7.11 3.20 5 5 -10 -4.17 2.83 5 5 -10 -0.43 2.11 4 5 -10 12.96 5.24 3 5 -10 38.71 8.32 2 5 -10 3.45 3.64 1 5 -10 31.36 7.65 0 5 -10 40.26 8.47 -1 5 -10 0.09 3.42 -2 5 -10 8.39 5.29 -3 -5 -10 1.91 2.38 -3 5 -10 5.02 5.21 -4 5 -10 9.54 5.61 7 -5 10 4.49 3.41 6 6 -10 8.15 3.65 6 6 -10 9.08 4.48 5 6 -10 -1.81 2.55 4 6 -10 0.10 3.38 3 6 -10 6.53 4.71 2 6 -10 2.14 3.09 1 6 -10 34.30 8.01 0 6 -10 16.25 6.80 -1 6 -10 11.50 5.58 -2 6 -10 15.92 7.12 -3 6 -10 57.70 11.06 6 7 -10 17.35 6.48 5 7 -10 9.97 4.66 4 7 -10 2.00 4.45 3 7 -10 36.41 8.57 2 7 -10 14.89 7.07 1 7 -10 29.89 8.08 0 7 -10 25.20 7.75 -1 7 -10 17.49 7.41 7 8 -10 5.25 3.87 6 8 -10 44.03 9.00 5 8 -10 26.70 7.10 4 8 -10 24.36 7.42 3 8 -10 11.22 5.89 2 8 -10 24.31 7.76 1 8 -10 11.01 6.12 8 0 -11 10.94 5.24 7 0 -11 8.49 5.11 6 0 -11 9.63 4.40 5 0 -11 3.30 2.82 4 0 -11 3.24 2.53 -2 0 -11 8.51 4.94 -3 0 -11 -0.19 2.82 9 -1 -11 0.90 3.90 8 -1 -11 29.72 7.20 7 1 -11 20.53 5.91 7 -1 -11 18.62 5.23 6 1 -11 15.42 4.64 5 1 -11 12.20 4.04 4 1 -11 2.45 2.74 3 1 -11 2.82 2.23 2 1 -11 7.11 2.81 -1 1 -11 1.96 3.52 -2 1 -11 2.98 2.81 -3 -1 -11 2.35 3.38 -3 1 -11 3.90 3.11 -4 -1 -11 34.76 7.98 6 2 -11 23.28 5.29 5 2 -11 1.64 2.21 4 2 -11 50.28 7.10 3 2 -11 10.45 3.53 2 2 -11 2.81 2.56 0 2 -11 1.88 3.70 -1 2 -11 7.38 4.77 -2 2 -11 2.84 3.57 5 3 -11 -2.31 2.44 4 3 -11 3.97 3.05 3 3 -11 5.73 2.77 1 3 -11 9.00 4.50 0 3 -11 8.35 4.19 -1 3 -11 2.35 3.05 -2 3 -11 4.75 4.99 1 4 -11 62.89 10.63 0 4 -11 12.57 5.21 -1 4 -11 4.94 4.09 2 5 -11 15.88 6.28 1 5 -11 5.12 4.37 0 0 0 0.00 0.00 TITL r20240420a in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 14.918358 12.930211 7.663075 90.0000 96.6350 90.0000 ZERR 6.00 0.000547 0.000435 0.000263 0.0000 0.0031 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O UNIT 66.00 60.00 6.00 6.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 63523 _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 1.708 _oxdiff_exptl_absorpt_empirical_full_min 0.574 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.19318(3) -0.08569(4) -0.01138(7) 0.03299(15) Uani 1 1 d . . . . . O1 O -0.10691(8) -0.13854(9) -0.73851(15) 0.0184(3) Uani 1 1 d . . . . . N1 N -0.17213(9) -0.22803(11) -0.52965(17) 0.0147(3) Uani 1 1 d D . . . . H1 H -0.1631(13) -0.2638(14) -0.4292(18) 0.026(6) Uiso 1 1 d D . . . . N2 N -0.24953(9) -0.24798(11) -0.64282(17) 0.0147(3) Uani 1 1 d . . . . . N3 N -0.64152(10) -0.41377(12) -0.95984(19) 0.0202(3) Uani 1 1 d . . . . . C1 C 0.10563(12) -0.10736(13) -0.1781(2) 0.0203(4) Uani 1 1 d . . . . . C2 C 0.12649(12) -0.12634(14) -0.3466(3) 0.0220(4) Uani 1 1 d . . . . . H2 H 0.187553 -0.127674 -0.370587 0.026 Uiso 1 1 calc R U . . . C3 C 0.05669(11) -0.14343(13) -0.4803(2) 0.0184(3) Uani 1 1 d . . . . . H3 H 0.069943 -0.155396 -0.596890 0.022 Uiso 1 1 calc R U . . . C4 C -0.03271(11) -0.14303(12) -0.4434(2) 0.0144(3) Uani 1 1 d . . . . . C5 C -0.05157(12) -0.12306(12) -0.2729(2) 0.0162(3) Uani 1 1 d . . . . . H5 H -0.112512 -0.121468 -0.248143 0.019 Uiso 1 1 calc R U . . . C6 C 0.01768(12) -0.10536(12) -0.1379(2) 0.0189(3) Uani 1 1 d . . . . . H6 H 0.004775 -0.092275 -0.021404 0.023 Uiso 1 1 calc R U . . . C7 C -0.10649(10) -0.16820(12) -0.5854(2) 0.0135(3) Uani 1 1 d . . . . . C8 C -0.29814(10) -0.32240(12) -0.5934(2) 0.0139(3) Uani 1 1 d . . . . . H8 H -0.276301 -0.362874 -0.494012 0.017 Uiso 1 1 calc R U . . . C9 C -0.38636(10) -0.34517(12) -0.6883(2) 0.0135(3) Uani 1 1 d . . . . . C10 C -0.43102(11) -0.27489(12) -0.8066(2) 0.0142(3) Uani 1 1 d . . . . . H10 H -0.403363 -0.210242 -0.825136 0.017 Uiso 1 1 calc R U . . . C11 C -0.51405(11) -0.29677(13) -0.8972(2) 0.0154(3) Uani 1 1 d . . . . . H11 H -0.542197 -0.247526 -0.977727 0.018 Uiso 1 1 calc R U . . . C12 C -0.55793(11) -0.39163(13) -0.8718(2) 0.0154(3) Uani 1 1 d . . . . . C13 C -0.51328(11) -0.46196(13) -0.7510(2) 0.0180(3) Uani 1 1 d . . . . . H13 H -0.540832 -0.526437 -0.730813 0.022 Uiso 1 1 calc R U . . . C14 C -0.42992(11) -0.43852(13) -0.6613(2) 0.0166(3) Uani 1 1 d . . . . . H14 H -0.401647 -0.486967 -0.579424 0.020 Uiso 1 1 calc R U . . . C15 C -0.67865(12) -0.51742(14) -0.9453(3) 0.0234(4) Uani 1 1 d . . . . . H15A H -0.634520 -0.568762 -0.974929 0.035 Uiso 1 1 calc R U . . . H15B H -0.734130 -0.524159 -1.026423 0.035 Uiso 1 1 calc R U . . . H15C H -0.692231 -0.528933 -0.824688 0.035 Uiso 1 1 calc R U . . . C16 C -0.67758(12) -0.34895(16) -1.1054(2) 0.0251(4) Uani 1 1 d . . . . . H16A H -0.685662 -0.278405 -1.063134 0.038 Uiso 1 1 calc R U . . . H16B H -0.735920 -0.376470 -1.156828 0.038 Uiso 1 1 calc R U . . . H16C H -0.635544 -0.348111 -1.194640 0.038 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 Cl1 0.0296(3) 0.0323(3) 0.0323(3) -0.0015(2) -0.01675(19) -0.00746(19) O1 0.0229(6) 0.0171(6) 0.0147(6) 0.0022(5) 0.0001(5) -0.0033(5) N1 0.0136(6) 0.0180(7) 0.0115(6) 0.0003(6) -0.0030(5) -0.0017(5) N2 0.0121(6) 0.0181(7) 0.0134(6) -0.0022(6) -0.0008(5) -0.0002(5) N3 0.0163(7) 0.0238(8) 0.0197(7) -0.0005(6) -0.0018(6) -0.0064(6) C1 0.0215(9) 0.0130(8) 0.0237(9) 0.0007(7) -0.0090(7) -0.0047(6) C2 0.0166(8) 0.0208(9) 0.0280(9) -0.0014(8) -0.0006(7) -0.0047(6) C3 0.0177(8) 0.0173(8) 0.0203(8) -0.0026(7) 0.0024(6) -0.0039(6) C4 0.0162(8) 0.0094(7) 0.0166(7) -0.0006(6) -0.0020(6) -0.0022(5) C5 0.0182(8) 0.0111(7) 0.0189(8) -0.0007(6) 0.0008(6) -0.0011(6) C6 0.0268(9) 0.0118(8) 0.0168(8) -0.0028(7) -0.0028(7) -0.0017(6) C7 0.0137(7) 0.0125(7) 0.0141(7) -0.0017(6) 0.0007(6) 0.0011(6) C8 0.0144(7) 0.0153(8) 0.0118(7) -0.0005(6) 0.0004(6) 0.0025(6) C9 0.0126(7) 0.0158(8) 0.0125(7) -0.0024(6) 0.0031(6) -0.0001(6) C10 0.0142(7) 0.0142(7) 0.0147(7) -0.0004(6) 0.0038(6) -0.0016(6) C11 0.0151(8) 0.0162(8) 0.0149(7) 0.0009(6) 0.0020(6) 0.0004(6) C12 0.0131(7) 0.0191(8) 0.0145(7) -0.0035(7) 0.0033(6) -0.0024(6) C13 0.0186(8) 0.0173(8) 0.0187(8) -0.0003(7) 0.0046(6) -0.0059(6) C14 0.0196(8) 0.0159(8) 0.0146(7) 0.0017(6) 0.0030(6) -0.0009(6) C15 0.0175(8) 0.0237(9) 0.0293(9) -0.0074(8) 0.0044(7) -0.0078(7) C16 0.0176(9) 0.0354(11) 0.0210(9) 0.0007(8) -0.0037(7) -0.0051(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 N2 N1 H1 118.3(13) . . ? C7 N1 H1 121.6(13) . . ? C7 N1 N2 119.27(13) . . ? C8 N2 N1 114.31(13) . . ? C12 N3 C15 118.91(15) . . ? C12 N3 C16 119.44(14) . . ? C16 N3 C15 118.68(14) . . ? C2 C1 Cl1 118.85(14) . . ? C6 C1 Cl1 118.98(14) . . ? C6 C1 C2 122.17(16) . . ? C1 C2 H2 120.5 . . ? C1 C2 C3 119.01(16) . . ? C3 C2 H2 120.5 . . ? C2 C3 H3 119.9 . . ? C2 C3 C4 120.13(16) . . ? C4 C3 H3 119.9 . . ? C3 C4 C7 119.56(15) . . ? C5 C4 C3 119.51(15) . . ? C5 C4 C7 120.88(14) . . ? C4 C5 H5 119.5 . . ? C4 C5 C6 120.93(16) . . ? C6 C5 H5 119.5 . . ? C1 C6 C5 118.23(16) . . ? C1 C6 H6 120.9 . . ? C5 C6 H6 120.9 . . ? O1 C7 N1 123.58(14) . . ? O1 C7 C4 123.25(14) . . ? N1 C7 C4 113.17(13) . . ? N2 C8 H8 119.7 . . ? N2 C8 C9 120.70(14) . . ? C9 C8 H8 119.7 . . ? C10 C9 C8 121.84(14) . . ? C10 C9 C14 117.58(14) . . ? C14 C9 C8 120.58(15) . . ? C9 C10 H10 119.1 . . ? C11 C10 C9 121.80(15) . . ? C11 C10 H10 119.1 . . ? C10 C11 H11 119.6 . . ? C10 C11 C12 120.82(15) . . ? C12 C11 H11 119.6 . . ? N3 C12 C11 121.33(15) . . ? N3 C12 C13 121.34(15) . . ? C13 C12 C11 117.32(15) . . ? C12 C13 H13 119.5 . . ? C14 C13 C12 120.98(15) . . ? C14 C13 H13 119.5 . . ? C9 C14 H14 119.3 . . ? C13 C14 C9 121.49(15) . . ? C13 C14 H14 119.3 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? N3 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 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 Cl1 C1 1.7409(17) . ? O1 C7 1.2335(19) . ? N1 H1 0.895(9) . ? N1 N2 1.3858(18) . ? N1 C7 1.355(2) . ? N2 C8 1.288(2) . ? N3 C12 1.378(2) . ? N3 C15 1.459(2) . ? N3 C16 1.448(2) . ? C1 C2 1.385(3) . ? C1 C6 1.382(3) . ? C2 H2 0.9500 . ? C2 C3 1.391(2) . ? C3 H3 0.9500 . ? C3 C4 1.395(2) . ? C4 C5 1.392(2) . ? C4 C7 1.492(2) . ? C5 H5 0.9500 . ? C5 C6 1.394(2) . ? C6 H6 0.9500 . ? C8 H8 0.9500 . ? C8 C9 1.458(2) . ? C9 C10 1.397(2) . ? C9 C14 1.398(2) . ? C10 H10 0.9500 . ? C10 C11 1.378(2) . ? C11 H11 0.9500 . ? C11 C12 1.414(2) . ? C12 C13 1.409(2) . ? C13 H13 0.9500 . ? C13 C14 1.383(2) . ? C14 H14 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? 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 Cl1 C1 C2 C3 -179.83(13) . . . . ? Cl1 C1 C6 C5 -179.88(12) . . . . ? N1 N2 C8 C9 173.27(13) . . . . ? N2 N1 C7 O1 -7.9(2) . . . . ? N2 N1 C7 C4 173.02(13) . . . . ? N2 C8 C9 C10 -15.6(2) . . . . ? N2 C8 C9 C14 165.40(15) . . . . ? N3 C12 C13 C14 -179.07(15) . . . . ? C1 C2 C3 C4 -1.1(3) . . . . ? C2 C1 C6 C5 -0.1(3) . . . . ? C2 C3 C4 C5 1.5(2) . . . . ? C2 C3 C4 C7 -176.06(15) . . . . ? C3 C4 C5 C6 -1.2(2) . . . . ? C3 C4 C7 O1 -39.4(2) . . . . ? C3 C4 C7 N1 139.74(15) . . . . ? C4 C5 C6 C1 0.5(2) . . . . ? C5 C4 C7 O1 143.12(16) . . . . ? C5 C4 C7 N1 -37.8(2) . . . . ? C6 C1 C2 C3 0.4(3) . . . . ? C7 N1 N2 C8 165.56(14) . . . . ? C7 C4 C5 C6 176.30(15) . . . . ? C8 C9 C10 C11 179.52(14) . . . . ? C8 C9 C14 C13 -179.49(15) . . . . ? C9 C10 C11 C12 0.7(2) . . . . ? C10 C9 C14 C13 1.5(2) . . . . ? C10 C11 C12 N3 179.09(15) . . . . ? C10 C11 C12 C13 0.0(2) . . . . ? C11 C12 C13 C14 0.0(2) . . . . ? C12 C13 C14 C9 -0.8(3) . . . . ? C14 C9 C10 C11 -1.4(2) . . . . ? C15 N3 C12 C11 172.54(15) . . . . ? C15 N3 C12 C13 -8.4(2) . . . . ? C16 N3 C12 C11 12.3(2) . . . . ? C16 N3 C12 C13 -168.67(16) . . . . ?