#------------------------------------------------------------------------------ #$Date: 2024-11-30 01:33:07 +0200 (Sat, 30 Nov 2024) $ #$Revision: 296171 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/96/7249652.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_7249652 loop_ _publ_author_name 'Han, Jiali' 'Zhu, Shujun' 'Chen, Xinxin' 'Zhou, Haichao' 'Pan, Jianguo' 'Pan, Shangke' _publ_section_title ; Optical properties of [MMim]2[CuI3] crystals with 0D single-core trigonal planar structures ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D4CE00750F _journal_year 2024 _chemical_formula_moiety 'Cu I3, 2(C5 H9 N2)' _chemical_formula_sum 'C10 H18 Cu I3 N4' _chemical_formula_weight 638.52 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-08-07 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _audit_update_record ; 2023-08-08 deposited with the CCDC. 2024-11-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 103.034(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.1644(10) _cell_length_b 14.9055(16) _cell_length_c 15.8041(18) _cell_measurement_reflns_used 5447 _cell_measurement_temperature 193.00 _cell_measurement_theta_max 30.58 _cell_measurement_theta_min 2.73 _cell_volume 1873.7(4) _computing_cell_refinement 'SAINT V8.40B (Bruker, 2019)' _computing_data_collection 'APEX4 V2022.10-1 (Bruker, 2022)' _computing_data_reduction 'SAINT V8.40B (Bruker, 2019)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2019/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 193.00 _diffrn_detector CPAD _diffrn_detector_area_resol_mean 7.41 _diffrn_detector_type 'Bruker PHOTON 100' _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 VENTURE TXS PHOTON 100' _diffrn_measurement_method '\w and \f shutterless scans' _diffrn_measurement_specimen_support 'nylon loop' _diffrn_radiation_monochromator 'Helios Multi-layer Optic' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_unetI/netI 0.0432 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 10640 _diffrn_reflns_point_group_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.580 _diffrn_reflns_theta_min 2.646 _diffrn_source TXS _diffrn_source_current 40.0 _diffrn_source_power 1.8 _diffrn_source_type 'Rotaing Anode' _diffrn_source_voltage 45.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 6.100 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.5431 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1250 before and 0.0714 after correction. The Ratio of minimum to maximum transmission is 0.7279. The \l/2 correction factor is Not present. ; _exptl_crystal_density_diffrn 2.264 _exptl_crystal_description block _exptl_crystal_F_000 1176 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.673 _refine_diff_density_min -1.072 _refine_diff_density_rms 0.140 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 85 _refine_ls_number_reflns 2862 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.028 _refine_ls_R_factor_all 0.0406 _refine_ls_R_factor_gt 0.0322 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0213P)^2^+5.6670P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0705 _refine_ls_wR_factor_ref 0.0757 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2456 _reflns_number_total 2862 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00750f1.cif _cod_data_source_block 230805lu_lgpz025964_0m _cod_depositor_comments ; The following automatic conversions were performed: data item '_diffrn_radiation_probe' value 'X-ray' was changed to 'x-ray' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas ; _cod_database_code 7249652 _shelx_shelxl_version_number 2019/3 _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 0.581 _shelx_estimated_absorpt_t_min 0.504 _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.a Aromatic/amide H refined with riding coordinates: C2(H2), C4(H4), C3(H3) 2.b Idealised Me refined as rotating group: C5(H5A,H5B,H5C), C1(H1A,H1B,H1C) ; _shelx_res_file ; TITL 230805lu_lgpz025964_0m_a.res in C2/c 230805lu_lgpz025964_0m.res created by SHELXL-2019/3 at 10:05:28 on 07-Aug-2023 REM Old TITL 230805LU_LGPZ025964_0m in C2/c REM SHELXT solution in C2/c: R1 0.133, Rweak 0.005, Alpha 0.021 REM 0.925 for 77 systematic absences, Orientation as input REM Formula found by SHELXT: C12 N2 Cu I3 CELL 0.71073 8.1644 14.9055 15.8041 90 103.034 90 ZERR 4 0.001 0.0016 0.0018 0 0.004 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Cu I N UNIT 40 72 4 12 16 L.S. 10 0 0 PLAN 6 SIZE 0.1 0.12 0.13 TEMP -80.15 CONF BOND list 4 fmap 2 53 MORE -1 BOND $H ACTA SIZE 0.1 0.12 0.13 OMIT -6 18 6 REM REM REM WGHT 0.021300 5.667000 FVAR 0.22296 I2 4 0.380113 0.328641 0.362657 11.00000 0.04163 0.03811 = 0.03092 -0.00044 0.01374 0.00221 I1 4 0.500000 0.075302 0.250000 10.50000 0.08795 0.03302 = 0.03133 0.00000 0.02300 0.00000 CU1 3 0.500000 0.244305 0.250000 10.50000 0.04114 0.03676 = 0.03047 0.00000 0.00895 0.00000 N2 5 0.738983 0.492388 0.422841 11.00000 0.04604 0.03137 = 0.03514 -0.00021 0.01104 -0.00328 N1 5 0.856823 0.363871 0.421595 11.00000 0.03328 0.03395 = 0.03317 0.00036 0.00841 -0.00293 C2 1 0.776588 0.428951 0.371679 11.00000 0.03889 0.03543 = 0.02926 0.00078 0.00676 -0.00409 AFIX 43 H2 2 0.750624 0.429896 0.309987 11.00000 -1.20000 AFIX 0 C4 1 0.795200 0.466122 0.508128 11.00000 0.05414 0.04370 = 0.02745 -0.00260 0.01149 -0.00541 AFIX 43 H4 2 0.783811 0.498739 0.558125 11.00000 -1.20000 AFIX 0 C5 1 0.645271 0.574627 0.392562 11.00000 0.07486 0.04001 = 0.05343 0.00298 0.01885 0.01373 AFIX 137 H5A 2 0.680327 0.597575 0.341280 11.00000 -1.50000 H5B 2 0.668284 0.619836 0.438751 11.00000 -1.50000 H5C 2 0.524597 0.561411 0.377426 11.00000 -1.50000 AFIX 0 C3 1 0.868570 0.386301 0.507189 11.00000 0.04507 0.04781 = 0.02812 0.00426 0.00606 -0.00297 AFIX 43 H3 2 0.919448 0.351441 0.556437 11.00000 -1.20000 AFIX 0 C1 1 0.914718 0.280575 0.389474 11.00000 0.04200 0.04257 = 0.05108 -0.00112 0.01374 0.00625 AFIX 137 H1A 2 0.823260 0.236522 0.379168 11.00000 -1.50000 H1B 2 1.010477 0.256957 0.432665 11.00000 -1.50000 H1C 2 0.949285 0.292325 0.335023 11.00000 -1.50000 AFIX 0 HKLF 4 REM 230805lu_lgpz025964_0m_a.res in C2/c REM wR2 = 0.0757, GooF = S = 1.028, Restrained GooF = 1.028 for all data REM R1 = 0.0322 for 2456 Fo > 4sig(Fo) and 0.0406 for all 2862 data REM 85 parameters refined using 0 restraints END WGHT 0.0213 5.6671 REM Highest difference peak 0.673, deepest hole -1.072, 1-sigma level 0.140 Q1 1 0.4255 0.1020 0.2542 11.00000 0.05 0.67 Q2 1 0.3936 0.3573 0.3019 11.00000 0.05 0.61 Q3 1 0.8600 0.2832 0.3047 11.00000 0.05 0.52 Q4 1 0.5023 0.2759 0.1742 11.00000 0.05 0.47 Q5 1 0.4001 0.2783 0.1609 11.00000 0.05 0.44 Q6 1 0.2616 0.3409 0.3163 11.00000 0.05 0.44 ; _shelx_res_checksum 31327 _shelx_hkl_file ; -2 0 0 1473.65 80.69 -2 0 0 1613.24 80.29 -2 0 0 1632.04 81.79 -2 0 0 1505.25 82.39 -4 0 0 374.26 22.20 4 0 0 470.55 23.40 -4 0 0 409.06 25.00 4 0 0 423.86 22.40 6 0 0 131.69 9.30 -6 0 0 113.49 11.40 6 0 0 143.09 8.30 8 0 0 1159.08 63.39 -10 0 0 40.40 9.40 10 0 0 49.70 6.40 1 -1 0 300.87 16.10 -1 -1 0 310.37 16.90 1 -1 0 299.97 17.00 1 -1 0 298.77 16.10 1 1 0 301.87 16.90 -1 1 0 301.37 16.10 1 1 0 314.27 16.20 -1 1 0 291.37 16.10 -1 1 0 338.67 17.10 3 -1 0 1416.06 75.29 3 -1 0 1414.36 75.59 -3 -1 0 1496.95 75.99 -3 -1 0 1397.56 77.69 3 1 0 1412.66 74.89 3 1 0 1544.85 75.89 -3 1 0 1469.85 75.79 5 -1 0 1126.49 59.79 -5 -1 0 1160.78 62.69 5 -1 0 1089.39 58.99 5 1 0 1205.58 59.99 5 1 0 1131.69 58.49 -5 1 0 1028.80 58.79 -7 -1 0 6.00 3.70 7 -1 0 4.00 1.80 7 1 0 3.40 1.90 -7 1 0 4.00 3.60 9 -1 0 9.30 3.30 -9 -1 0 14.10 6.00 9 1 0 11.70 3.40 -9 1 0 10.00 5.10 11 -1 0 4.90 3.00 -11 -1 0 8.20 6.30 11 1 0 10.10 3.50 -11 1 0 -3.30 6.00 0 -2 0 680.53 35.60 0 -2 0 678.73 34.80 0 -2 0 704.63 35.00 0 2 0 626.84 34.90 2 -2 0 778.02 44.80 2 -2 0 924.21 46.80 2 -2 0 873.11 44.80 -2 -2 0 827.72 46.30 -2 -2 0 833.62 45.00 -2 2 0 865.51 44.80 -2 2 0 843.02 44.80 2 2 0 862.41 46.60 2 2 0 853.51 45.00 -2 2 0 919.31 46.80 4 -2 0 1249.47 71.89 4 -2 0 1347.77 71.69 -4 2 0 1404.46 74.89 4 2 0 1373.16 70.69 4 2 0 1348.27 72.09 4 2 0 1514.95 76.39 6 -2 0 -0.40 0.90 6 -2 0 0.50 1.10 -6 -2 0 -0.40 2.10 -6 2 0 3.30 3.00 6 2 0 -1.20 1.20 -8 -2 0 174.48 15.90 8 -2 0 176.18 12.20 8 2 0 170.98 12.20 -8 2 0 149.59 15.70 -10 -2 0 20.90 7.60 10 -2 0 19.40 4.60 -10 2 0 16.80 7.80 10 2 0 13.60 3.50 1 -3 0 2255.77 120.69 -1 -3 0 2357.66 120.69 -1 3 0 2305.17 120.79 1 3 0 2339.47 120.79 3 -3 0 1098.59 57.49 -3 -3 0 1099.79 59.69 3 -3 0 1124.89 57.69 3 -3 0 1004.80 59.89 3 3 0 1131.59 60.39 -3 3 0 1144.39 60.19 3 3 0 1148.99 57.79 -3 3 0 991.90 57.29 -3 3 0 1121.39 57.49 5 -3 0 877.51 46.30 5 -3 0 831.72 46.40 -5 3 0 880.11 50.09 5 3 0 877.81 51.59 5 3 0 857.51 46.70 7 -3 0 134.69 9.80 -7 -3 0 154.98 13.90 7 -3 0 153.38 10.50 -7 3 0 138.19 14.00 7 3 0 156.38 10.80 -9 -3 0 195.78 18.40 9 -3 0 188.08 14.10 9 3 0 191.68 14.10 -9 3 0 207.58 18.90 11 -3 0 2.30 3.50 -11 -3 0 22.60 8.40 11 3 0 8.10 2.80 0 -4 0 483.45 24.90 0 -4 0 493.85 26.20 0 -4 0 464.95 24.40 0 4 0 471.05 26.20 0 4 0 409.66 24.70 0 4 0 480.35 24.40 -2 -4 0 5.80 1.30 -2 -4 0 5.90 1.90 2 -4 0 6.70 1.10 2 -4 0 4.80 1.20 2 -4 0 6.50 2.20 -2 4 0 5.00 2.00 -2 4 0 8.40 1.00 2 4 0 6.00 1.90 -2 4 0 6.50 1.20 2 4 0 6.40 0.80 2 4 0 7.90 1.40 4 -4 0 1549.54 86.09 4 -4 0 1764.62 86.09 4 4 0 1597.24 89.69 4 4 0 1660.03 86.29 -4 4 0 1628.94 89.19 6 -4 0 9.50 2.40 6 -4 0 11.00 2.50 6 4 0 10.30 2.70 6 4 0 15.00 5.40 -6 4 0 21.70 5.20 -8 -4 0 28.20 7.50 8 -4 0 22.90 4.30 -8 4 0 20.10 6.50 8 4 0 28.70 4.70 -10 -4 0 4.30 5.50 10 -4 0 5.10 2.90 10 4 0 0.00 2.00 -10 4 0 12.70 6.10 -1 -5 0 2528.55 133.59 1 -5 0 2764.92 134.09 -1 -5 0 2713.53 131.89 1 -5 0 2478.35 132.19 1 5 0 2417.26 133.69 -1 5 0 2444.36 133.79 1 5 0 2324.67 131.59 -1 5 0 2719.53 132.09 3 -5 0 126.49 8.50 3 -5 0 133.59 8.10 3 5 0 144.29 10.80 -3 5 0 122.49 10.30 -3 5 0 131.09 7.90 3 5 0 136.29 8.40 3 5 0 129.69 7.20 5 -5 0 116.89 8.10 5 -5 0 101.79 7.60 5 5 0 110.29 11.50 -5 5 0 112.09 10.90 5 5 0 112.29 8.10 7 -5 0 168.68 12.10 7 -5 0 183.68 12.40 -7 5 0 180.88 16.20 7 5 0 188.98 12.60 9 -5 0 114.59 9.30 -9 -5 0 105.99 13.60 -9 5 0 94.19 12.30 9 5 0 84.79 8.70 -11 -5 0 33.20 8.90 11 5 0 19.50 4.70 0 -6 0 88.59 5.70 0 -6 0 98.89 7.30 0 -6 0 74.79 4.90 0 6 0 92.09 5.00 0 6 0 75.19 5.40 0 6 0 75.89 6.90 -2 -6 0 1677.73 92.89 2 -6 0 1815.32 93.39 2 6 0 1660.43 95.29 -2 6 0 1851.81 92.19 -2 6 0 1707.03 95.49 2 6 0 1827.22 92.29 2 6 0 1914.71 92.79 4 -6 0 4905.21 241.58 4 -6 0 4606.34 242.08 4 6 0 4740.43 245.98 -4 6 0 4420.76 245.08 6 -6 0 559.24 30.40 6 -6 0 496.65 30.40 6 6 0 541.75 30.60 -6 6 0 539.45 34.50 6 6 0 548.45 36.40 -8 -6 0 104.79 13.20 8 -6 0 98.89 8.50 8 6 0 96.89 8.80 -8 6 0 109.39 12.10 -10 -6 0 0.60 4.90 10 6 0 3.30 2.50 -10 6 0 9.80 5.70 -1 -7 0 1694.83 94.49 -1 7 0 1773.72 97.59 1 7 0 1850.41 94.69 -1 7 0 1756.02 94.09 1 7 0 1997.10 94.49 1 7 0 1841.92 97.59 3 -7 0 417.56 25.00 3 7 0 454.85 24.50 -3 7 0 461.35 23.90 3 7 0 432.06 23.40 3 7 0 452.45 27.80 -3 7 0 431.06 27.70 5 -7 0 57.49 5.50 5 7 0 56.69 5.30 -5 7 0 52.29 8.80 5 7 0 59.49 8.20 7 -7 0 16.30 3.70 7 -7 0 22.30 3.90 -7 7 0 13.10 5.10 7 7 0 21.30 4.00 7 7 0 20.70 7.50 -9 -7 0 70.39 12.60 -9 7 0 58.99 10.90 9 7 0 67.69 7.30 0 -8 0 1442.96 79.59 0 8 0 1557.54 82.39 0 8 0 1535.15 78.39 2 -8 0 91.59 7.20 -2 8 0 91.19 8.90 2 8 0 94.09 6.10 2 8 0 99.99 9.10 2 8 0 100.79 6.40 -2 8 0 103.49 5.80 4 -8 0 427.26 25.60 4 8 0 407.26 23.20 4 8 0 470.15 29.50 -4 8 0 455.25 29.00 4 8 0 464.45 25.00 6 -8 0 6.00 2.60 -6 8 0 9.40 4.50 6 8 0 10.60 2.70 6 8 0 4.00 4.30 8 8 0 49.60 11.70 8 8 0 66.69 6.90 -8 8 0 60.19 11.10 10 8 0 4.60 2.60 -10 8 0 -0.10 5.40 1 -9 0 1115.79 57.09 1 9 0 1080.99 59.69 -1 9 0 999.60 54.99 -1 9 0 1000.80 59.39 1 9 0 1090.29 55.39 -3 9 0 912.61 48.00 -3 9 0 871.31 52.99 3 9 0 983.90 53.59 3 9 0 928.31 48.80 3 9 0 878.91 48.00 5 -9 0 994.30 53.39 5 9 0 966.30 52.29 -5 9 0 906.61 56.69 5 9 0 982.10 58.09 -7 9 0 106.59 12.50 7 9 0 111.49 9.00 7 9 0 111.69 14.60 9 9 0 75.09 7.80 -9 9 0 71.09 12.60 0 10 0 377.96 24.50 0 10 0 358.26 19.60 2 -10 0 147.69 10.40 -2 -10 0 124.99 9.10 2 10 0 155.58 9.00 -2 10 0 153.78 13.10 -2 10 0 146.69 8.00 2 10 0 145.89 12.60 -2 10 0 137.69 8.40 4 -10 0 0.60 1.70 4 10 0 -1.40 1.00 4 10 0 4.70 3.30 -4 10 0 4.20 3.20 4 10 0 1.10 1.40 6 -10 0 32.20 5.40 -6 10 0 33.90 7.70 6 10 0 31.50 4.80 6 10 0 30.90 8.50 8 10 0 36.20 5.60 -8 10 0 31.90 8.70 8 10 0 17.30 8.80 -10 -10 0 22.80 8.70 -10 10 0 13.90 8.10 1 -11 0 397.66 24.10 -1 11 0 410.96 21.50 1 11 0 456.65 27.80 1 11 0 389.86 22.00 -1 11 0 394.26 27.10 -1 11 0 403.06 21.40 3 -11 0 524.15 32.40 3 11 0 583.84 36.40 -3 11 0 557.04 29.80 3 11 0 603.04 30.90 -3 11 0 533.95 35.80 5 -11 0 263.17 17.20 -5 11 0 236.48 20.00 5 11 0 242.78 13.50 5 11 0 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27.80 8.90 -1 11 18 20.10 6.60 -1 11 18 12.20 5.80 1 -11 18 14.30 4.00 1 -11 18 10.00 3.90 1 11 18 20.90 6.60 -4 -12 18 4.30 4.00 -4 -12 18 1.30 2.70 4 12 -18 4.90 7.80 -4 12 18 -0.60 4.30 -4 12 18 -5.10 6.60 -2 -12 18 24.80 5.10 -2 -12 18 24.60 5.10 2 12 -18 4.50 8.90 -2 12 18 37.10 8.80 -2 12 18 43.00 8.30 0 -12 18 287.37 20.70 0 12 18 321.77 24.60 -8 0 19 5.90 7.00 -6 0 19 7.50 3.60 -6 0 19 -2.30 5.50 -4 0 19 3.00 5.80 -4 0 19 0.90 3.00 -2 0 19 11.00 3.40 0 0 19 10.00 4.20 2 0 19 -5.80 2.80 -7 -1 19 386.76 31.40 -7 1 19 339.87 30.10 -7 1 19 386.06 27.70 -5 -1 19 28.30 6.50 -5 -1 19 54.09 10.80 -5 1 19 39.50 8.10 -3 -1 19 80.09 9.30 -3 -1 19 96.39 11.40 -3 1 19 71.29 10.20 -3 1 19 63.99 8.90 -1 -1 19 75.99 8.90 1 -1 19 340.77 25.00 1 1 19 386.76 25.90 3 -1 19 65.19 7.70 3 -1 19 47.90 8.00 3 1 19 63.99 8.50 -8 -2 19 25.50 9.20 -8 2 19 33.50 9.80 -6 -2 19 -0.50 5.40 -6 -2 19 2.40 3.70 -6 2 19 7.90 4.10 -6 2 19 7.40 7.00 -4 -2 19 396.56 27.40 -4 -2 19 414.16 29.80 -4 2 19 414.76 29.90 -4 2 19 378.86 27.60 -2 -2 19 406.96 25.60 -2 -2 19 327.27 24.00 -2 2 19 357.86 25.50 -2 2 19 364.26 23.20 0 -2 19 9.80 4.00 0 2 19 -5.60 3.20 2 -2 19 14.10 5.00 2 -2 19 10.90 4.40 2 2 19 7.00 4.20 -7 -3 19 -8.10 5.70 -7 3 19 -1.00 3.60 -7 3 19 -3.20 5.80 -5 -3 19 7.70 5.00 -5 -3 19 13.80 6.70 -5 3 19 18.90 7.90 -5 3 19 18.20 5.30 -3 -3 19 52.89 8.00 -3 -3 19 42.70 8.70 -3 3 19 48.60 8.60 -3 3 19 48.60 9.40 -1 -3 19 18.20 3.60 -1 -3 19 30.60 6.60 -1 3 19 26.50 6.00 1 -3 19 -2.80 1.80 1 -3 19 -3.00 3.00 3 -3 19 3.90 3.60 3 3 19 3.30 4.60 -8 -4 19 159.78 19.20 -8 4 19 139.39 18.40 -8 4 19 148.09 15.70 -6 -4 19 276.67 20.90 -6 -4 19 264.17 23.80 -6 4 19 268.57 22.00 -6 4 19 270.57 24.70 -4 -4 19 18.00 5.90 -4 -4 19 4.50 3.70 -4 4 19 2.70 3.80 -4 4 19 7.90 5.90 -2 -4 19 15.20 4.90 -2 -4 19 26.80 6.60 -2 4 19 18.60 5.30 -2 4 19 16.10 4.70 0 -4 19 235.38 18.20 0 -4 19 271.27 18.00 0 4 19 208.58 18.50 2 -4 19 194.78 16.00 2 -4 19 198.68 16.00 2 4 19 212.88 17.70 -7 -5 19 21.90 8.40 -7 5 19 20.20 6.90 -7 5 19 19.00 7.60 -5 -5 19 85.99 10.50 -5 -5 19 120.49 14.10 -5 5 19 105.29 14.00 -5 5 19 119.69 12.80 -3 -5 19 465.95 32.20 -3 -5 19 507.05 34.40 -3 5 19 518.95 34.20 -3 5 19 578.84 35.70 -1 -5 19 116.19 11.10 -1 -5 19 88.89 9.70 -1 -5 19 124.09 10.40 -1 5 19 108.89 12.10 1 -5 19 7.70 3.70 1 -5 19 13.20 4.00 1 5 19 18.60 6.00 3 -5 19 20.50 5.20 3 -5 19 18.10 4.80 3 5 19 13.30 5.80 -6 -6 19 0.10 3.10 -6 -6 19 -6.00 4.70 -6 -6 19 -3.40 1.90 -6 6 19 -6.10 3.20 -6 6 19 -1.00 5.20 -4 -6 19 17.60 5.00 -4 -6 19 16.20 3.90 -4 -6 19 25.00 6.50 -4 6 19 7.80 5.10 -4 6 19 20.40 7.70 -2 -6 19 25.00 5.50 -2 -6 19 16.50 5.80 -2 -6 19 24.90 4.70 -2 6 19 11.70 5.20 -2 6 19 17.90 6.00 0 -6 19 -4.30 2.00 0 -6 19 6.70 3.90 0 6 19 -3.90 3.50 2 -6 19 -1.50 2.80 2 -6 19 5.00 3.50 2 6 19 13.00 4.70 -7 -7 19 76.89 14.90 -7 -7 19 69.99 7.60 -7 7 19 91.49 12.20 -5 -7 19 31.50 6.50 -5 -7 19 35.30 5.60 -5 -7 19 33.90 8.60 -5 7 19 28.30 9.50 -5 7 19 25.50 6.90 -3 -7 19 314.67 26.90 -3 -7 19 371.06 25.10 -3 -7 19 391.86 24.40 -3 7 19 408.86 27.60 -3 7 19 375.86 27.60 -1 -7 19 26.20 5.50 -1 -7 19 16.10 5.30 -1 -7 19 24.70 5.90 -1 7 19 26.00 5.00 -1 7 19 31.90 7.40 1 -7 19 64.99 7.90 1 -7 19 58.69 7.30 1 7 19 47.60 9.00 -6 -8 19 151.48 13.30 -6 -8 19 100.39 17.40 -6 -8 19 124.79 10.10 -6 8 19 94.29 16.20 -6 8 19 105.89 13.80 -4 -8 19 4.10 3.60 -4 -8 19 5.60 3.10 -4 -8 19 16.00 6.40 -4 8 19 11.60 5.20 -4 8 19 14.70 7.00 -2 -8 19 11.30 3.70 -2 -8 19 6.30 6.00 -2 -8 19 7.10 4.40 -2 8 19 15.20 5.50 -2 8 19 17.10 5.50 0 -8 19 130.79 12.00 0 -8 19 158.38 12.70 0 8 19 134.49 14.20 2 -8 19 92.29 9.80 2 -8 19 97.39 9.70 2 8 19 94.29 11.70 -5 -9 19 13.50 6.80 -5 -9 19 29.00 6.10 -5 9 19 12.90 6.10 -5 9 19 22.90 8.50 -3 -9 19 -0.90 2.40 -3 -9 19 -0.40 6.10 -3 -9 19 0.80 3.50 -3 9 19 4.00 5.50 -3 9 19 3.80 4.20 -1 -9 19 15.20 4.80 -1 -9 19 16.70 6.60 -1 -9 19 14.40 4.20 -1 9 19 9.30 4.60 -1 9 19 9.40 4.90 1 -9 19 30.30 5.40 1 -9 19 16.90 5.10 1 9 19 15.60 5.80 -4 -10 19 216.88 16.10 -4 -10 19 227.98 17.40 -4 10 19 234.98 22.50 -2 -10 19 212.48 15.20 -2 -10 19 210.78 15.60 -2 10 19 185.98 16.80 -2 10 19 151.48 17.10 0 -10 19 -6.90 3.40 0 -10 19 4.40 2.80 0 10 19 -0.60 4.30 -3 -11 19 1.60 2.60 -3 -11 19 -5.20 3.40 -3 11 19 -3.10 6.30 3 11 -19 15.90 8.00 -3 11 19 9.20 5.00 -1 -11 19 81.09 8.50 -1 11 19 77.59 12.40 -1 11 19 81.79 15.30 -6 0 20 690.63 45.70 -6 0 20 608.74 41.50 -4 0 20 110.29 11.80 -4 0 20 110.59 14.20 -2 0 20 21.80 5.60 -2 0 20 24.30 4.40 0 0 20 98.09 10.90 2 0 20 495.95 33.10 -7 -1 20 1.20 6.90 -7 -1 20 11.00 4.50 -7 1 20 2.70 3.40 -7 1 20 5.00 7.10 -5 -1 20 11.30 4.30 -5 -1 20 22.20 6.70 -5 1 20 15.50 7.10 -5 1 20 8.40 4.10 -3 -1 20 231.48 19.40 -3 -1 20 252.47 19.30 -3 1 20 248.88 19.40 -3 1 20 221.88 18.50 -1 -1 20 134.79 12.90 -1 1 20 135.19 13.30 1 -1 20 4.40 3.80 1 1 20 4.40 4.30 -6 -2 20 41.60 10.70 -6 -2 20 37.60 7.30 -6 2 20 31.10 7.90 -6 2 20 40.90 10.30 -4 -2 20 7.20 3.20 -4 -2 20 -11.40 4.80 -4 2 20 -2.20 2.90 -4 2 20 1.30 5.60 -2 -2 20 70.99 9.40 -2 -2 20 93.19 10.30 -2 2 20 102.69 11.10 -2 2 20 89.49 8.20 0 -2 20 2.00 3.60 0 2 20 -1.30 3.40 2 -2 20 26.80 6.40 2 -2 20 17.80 4.90 2 2 20 26.20 6.20 -7 -3 20 136.49 14.00 -7 3 20 156.38 15.20 -7 3 20 129.09 18.20 -5 -3 20 85.19 10.30 -5 -3 20 86.99 13.80 -5 3 20 75.29 13.00 -5 3 20 71.49 9.90 -3 -3 20 122.89 13.80 -3 -3 20 144.19 12.90 -3 3 20 118.49 13.00 -3 3 20 115.79 13.00 -1 -3 20 129.39 11.80 -1 3 20 83.79 11.40 1 -3 20 84.89 9.40 1 -3 20 91.09 10.20 1 3 20 89.29 10.70 -6 -4 20 20.10 9.60 -6 -4 20 25.20 6.10 -6 4 20 8.40 7.80 -6 4 20 12.20 5.50 -4 -4 20 0.50 3.00 -4 -4 20 -11.70 5.40 -4 4 20 6.10 5.80 -4 4 20 -6.60 2.80 -2 -4 20 64.59 9.60 -2 -4 20 92.49 9.70 -2 4 20 61.49 7.50 -2 4 20 82.19 10.50 0 -4 20 7.10 3.80 0 4 20 1.20 3.20 2 -4 20 15.50 5.20 2 -4 20 16.80 4.70 2 4 20 3.90 4.60 -5 -5 20 98.19 13.40 -5 -5 20 78.39 10.50 -5 5 20 86.19 14.00 -5 5 20 98.59 11.90 -3 -5 20 -4.10 3.10 -3 -5 20 1.10 5.60 -3 5 20 10.90 5.30 -3 5 20 5.20 3.90 -1 -5 20 5.60 3.20 -1 -5 20 2.70 3.60 -1 5 20 3.70 4.00 1 -5 20 63.79 8.60 1 5 20 50.99 9.00 -6 -6 20 25.10 6.10 -6 -6 20 25.00 4.70 -6 -6 20 19.80 8.90 -6 6 20 11.90 7.50 -6 6 20 22.40 6.40 -4 -6 20 130.79 11.30 -4 -6 20 127.19 12.30 -4 -6 20 113.19 15.00 -4 6 20 128.39 15.60 -4 6 20 159.08 15.20 -2 -6 20 546.85 32.60 -2 6 20 462.95 30.10 0 -6 20 98.99 10.40 0 -6 20 109.39 10.30 0 6 20 81.99 11.30 -5 -7 20 59.39 6.80 -5 -7 20 31.30 9.70 -5 -7 20 41.50 8.00 -5 7 20 53.69 11.90 -5 7 20 58.19 10.30 -3 -7 20 31.50 6.20 -3 -7 20 31.70 8.30 -3 -7 20 33.60 5.70 -3 7 20 17.20 7.40 -3 7 20 39.80 8.40 -1 -7 20 25.90 6.20 -1 -7 20 25.30 5.10 -1 7 20 41.10 8.30 1 -7 20 59.29 7.50 1 -7 20 57.49 8.60 1 7 20 49.99 9.40 -4 -8 20 -0.90 3.50 -4 -8 20 4.00 6.80 -4 -8 20 2.50 2.80 -4 8 20 7.90 6.80 -2 -8 20 30.00 7.90 -2 -8 20 37.90 6.10 -2 -8 20 28.20 5.80 -2 8 20 27.90 7.40 0 -8 20 4.80 3.10 0 -8 20 -2.40 3.80 0 8 20 2.40 4.60 -3 -9 20 138.99 15.90 -3 -9 20 148.39 12.30 -3 -9 20 147.69 13.30 -3 9 20 119.69 15.20 -3 9 20 149.99 16.10 -1 -9 20 80.29 8.90 -1 -9 20 71.09 9.30 -1 9 20 75.09 11.80 -6 0 21 -9.30 6.70 -4 0 21 -0.70 6.10 -4 0 21 -5.70 2.90 -2 0 21 3.90 3.30 0 0 21 5.50 3.40 -5 -1 21 372.06 30.10 -5 -1 21 383.96 27.10 -5 1 21 357.66 29.60 -5 1 21 362.66 27.10 -3 -1 21 12.70 5.00 -3 -1 21 10.70 5.80 -3 1 21 8.90 4.80 -3 1 21 8.90 5.50 -1 -1 21 17.10 5.80 -1 1 21 21.40 6.50 1 -1 21 33.80 7.60 1 1 21 46.50 8.00 -6 -2 21 24.70 8.10 -6 -2 21 26.40 6.50 -6 2 21 12.40 8.00 -6 2 21 12.50 5.30 -4 -2 21 2.30 5.80 -4 -2 21 7.00 3.80 -4 2 21 12.90 6.40 -4 2 21 2.30 3.20 -2 -2 21 212.78 17.80 -2 2 21 225.88 18.70 0 -2 21 212.08 17.80 0 2 21 209.98 18.50 -5 -3 21 -4.20 6.80 -5 -3 21 3.60 4.20 -5 3 21 14.40 4.90 -5 3 21 15.40 7.40 -3 -3 21 13.20 6.80 -3 -3 21 15.90 4.90 -3 3 21 16.30 5.40 -3 3 21 13.90 5.40 -1 -3 21 36.10 7.70 -1 3 21 46.90 8.00 1 -3 21 16.30 4.40 1 -3 21 8.60 4.30 1 3 21 11.80 5.00 -6 -4 21 240.58 18.80 -6 -4 21 162.38 20.40 -6 4 21 192.78 20.50 -4 -4 21 196.18 16.60 -4 -4 21 184.78 18.70 -4 4 21 170.68 17.50 -4 4 21 164.08 16.50 -2 -4 21 15.90 5.20 -2 4 21 15.80 5.20 0 -4 21 -3.30 2.60 0 -4 21 -6.00 3.50 0 4 21 0.00 3.90 -5 -5 21 -3.70 6.70 -5 -5 21 7.00 4.20 -5 5 21 10.50 7.20 -5 5 21 -0.50 3.30 -3 -5 21 82.19 12.50 -3 -5 21 104.69 11.10 -3 5 21 92.89 11.40 -3 5 21 122.19 12.60 -1 -5 21 288.27 20.70 -1 -5 21 283.57 21.40 -1 5 21 283.97 23.00 -4 -6 21 4.20 2.70 -4 -6 21 8.30 6.70 -4 -6 21 -0.40 4.10 -4 6 21 -1.70 3.80 -4 6 21 4.70 6.30 -2 -6 21 9.40 4.00 -2 -6 21 9.60 4.10 -2 6 21 15.00 5.40 0 -6 21 8.40 4.80 0 -6 21 20.30 4.80 0 6 21 9.70 5.00 -3 -7 21 26.20 8.10 -3 -7 21 36.70 6.60 -3 -7 21 31.30 6.70 -3 7 21 37.40 8.70 -1 -7 21 218.08 17.50 -1 -7 21 227.18 16.90 -1 7 21 188.78 18.80 -4 0 22 236.88 20.90 -5 -1 22 15.20 7.90 -5 1 22 18.60 8.00 -3 -1 22 -2.40 3.80 -3 1 22 10.90 4.80 -1 1 22 87.99 12.60 -4 -2 22 37.40 9.80 -4 -2 22 39.20 8.20 -4 2 22 45.90 8.80 -2 -2 22 12.70 4.60 -2 2 22 12.50 5.20 -3 -3 22 20.40 6.20 -3 3 22 25.90 7.20 -1 -3 22 47.80 9.20 -1 3 22 54.19 9.60 -4 -4 22 15.80 7.40 -4 -4 22 16.70 5.80 -4 4 22 12.80 5.10 -4 4 22 17.10 7.10 -2 -4 22 5.00 4.10 -2 4 22 3.00 3.50 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 76098 _olex2_submission_special_instructions 'No special instructions were received' _site XU loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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 I2 I 0.38011(3) 0.32864(2) 0.36266(2) 0.03601(8) Uani 1 1 d . . . . . I1 I 0.500000 0.07530(2) 0.250000 0.04925(11) Uani 1 2 d S T P . . Cu1 Cu 0.500000 0.24430(4) 0.250000 0.03599(14) Uani 1 2 d S T P . . N2 N 0.7390(4) 0.49239(19) 0.42284(19) 0.0372(6) Uani 1 1 d . . . . . N1 N 0.8568(3) 0.36387(19) 0.42160(18) 0.0333(6) Uani 1 1 d . . . . . C2 C 0.7766(4) 0.4290(2) 0.3717(2) 0.0347(7) Uani 1 1 d . . . . . H2 H 0.750624 0.429896 0.309987 0.042 Uiso 1 1 calc R U . . . C4 C 0.7952(5) 0.4661(3) 0.5081(2) 0.0414(8) Uani 1 1 d . . . . . H4 H 0.783811 0.498739 0.558125 0.050 Uiso 1 1 calc R U . . . C5 C 0.6453(6) 0.5746(3) 0.3926(3) 0.0554(11) Uani 1 1 d . . . . . H5A H 0.680327 0.597575 0.341280 0.083 Uiso 1 1 calc R U . . . H5B H 0.668284 0.619836 0.438751 0.083 Uiso 1 1 calc R U . . . H5C H 0.524597 0.561411 0.377426 0.083 Uiso 1 1 calc R U . . . C3 C 0.8686(5) 0.3863(3) 0.5072(2) 0.0407(8) Uani 1 1 d . . . . . H3 H 0.919448 0.351441 0.556437 0.049 Uiso 1 1 calc R U . . . C1 C 0.9147(5) 0.2806(3) 0.3895(3) 0.0447(8) Uani 1 1 d . . . . . H1A H 0.823260 0.236522 0.379168 0.067 Uiso 1 1 calc R U . . . H1B H 1.010477 0.256957 0.432665 0.067 Uiso 1 1 calc R U . . . H1C H 0.949285 0.292325 0.335023 0.067 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 I2 0.04163(13) 0.03811(13) 0.03092(12) -0.00044(7) 0.01374(9) 0.00221(9) I1 0.0879(3) 0.03302(17) 0.03133(16) 0.000 0.02300(17) 0.000 Cu1 0.0411(3) 0.0368(3) 0.0305(3) 0.000 0.0090(2) 0.000 N2 0.0460(16) 0.0314(14) 0.0351(14) -0.0002(11) 0.0110(12) -0.0033(12) N1 0.0333(13) 0.0340(14) 0.0332(14) 0.0004(11) 0.0084(11) -0.0029(11) C2 0.0389(17) 0.0354(16) 0.0293(15) 0.0008(12) 0.0068(13) -0.0041(13) C4 0.054(2) 0.0437(19) 0.0274(15) -0.0026(13) 0.0115(15) -0.0054(16) C5 0.075(3) 0.040(2) 0.053(2) 0.0030(17) 0.019(2) 0.014(2) C3 0.0451(19) 0.048(2) 0.0281(16) 0.0043(13) 0.0061(14) -0.0030(16) C1 0.0420(19) 0.043(2) 0.051(2) -0.0011(16) 0.0137(17) 0.0063(16) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' 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 I2 Cu1 I2 120.89(3) . 2_655 ? I1 Cu1 I2 119.557(14) . 2_655 ? I1 Cu1 I2 119.556(14) . . ? C2 N2 C4 108.8(3) . . ? C2 N2 C5 125.0(3) . . ? C4 N2 C5 126.2(3) . . ? C2 N1 C3 108.8(3) . . ? C2 N1 C1 124.8(3) . . ? C3 N1 C1 126.3(3) . . ? N2 C2 N1 108.1(3) . . ? N2 C2 H2 126.0 . . ? N1 C2 H2 126.0 . . ? N2 C4 H4 126.5 . . ? C3 C4 N2 107.1(3) . . ? C3 C4 H4 126.5 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C3 H3 126.4 . . ? C4 C3 N1 107.2(3) . . ? C4 C3 H3 126.4 . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 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 I2 Cu1 2.5484(4) . ? I1 Cu1 2.5191(8) . ? N2 C2 1.324(4) . ? N2 C4 1.379(4) . ? N2 C5 1.467(5) . ? N1 C2 1.326(4) . ? N1 C3 1.376(4) . ? N1 C1 1.460(5) . ? C2 H2 0.9500 . ? C4 H4 0.9500 . ? C4 C3 1.334(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C3 H3 0.9500 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 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 N2 C4 C3 N1 -0.1(4) . . . . ? C2 N2 C4 C3 0.6(4) . . . . ? C2 N1 C3 C4 -0.4(4) . . . . ? C4 N2 C2 N1 -0.9(4) . . . . ? C5 N2 C2 N1 -178.0(4) . . . . ? C5 N2 C4 C3 177.7(4) . . . . ? C3 N1 C2 N2 0.8(4) . . . . ? C1 N1 C2 N2 178.0(3) . . . . ? C1 N1 C3 C4 -177.6(3) . . . . ?