#------------------------------------------------------------------------------ #$Date: 2023-06-06 07:32:37 +0200 (Tue, 06 Jun 2023) $ #$Revision: 284377 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/27/2022739.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2022739 loop_ _publ_author_name 'Petrenko, Yuliia P.' 'Khomenko, Dmytro M.' 'Doroshchuk, Roman O.' 'Raspertova, Ilona V.' 'Shova, Sergiu' 'Lampeka, Rostyslav D.' _publ_section_title ; Synthesis and crystal structure of a new copper(II) complex based on 5-ethyl-3-(pyridin-2-yl)-1,2,4-triazole. ; _journal_coeditor_code JY2029 _journal_issue 'Pt 5' _journal_name_full 'Acta crystallographica. Section E, Crystallographic communications' _journal_page_first 432 _journal_page_last 435 _journal_paper_doi 10.1107/S2056989023003079 _journal_volume 79 _journal_year 2023 _chemical_formula_iupac '[Cu2 (C9 H9 N4)2 (C2 H3 O2)2 (C3 H7 N O)2]' _chemical_formula_moiety 'C28 H38 Cu2 N10 O6' _chemical_formula_sum 'C28 H38 Cu2 N10 O6' _chemical_formula_weight 737.76 _chemical_name_systematic Bis[\m-3-ethyl-5-(pyridin-2-yl)-1H-1,2,4-triazol-1-ido]bis[acetato(dimethylacetamide)copper(II)] _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 geom _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.5 (compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439) ; _cell_angle_alpha 90 _cell_angle_beta 93.257(4) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.4445(5) _cell_length_b 8.9404(4) _cell_length_c 20.2237(9) _cell_measurement_reflns_used 2231 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.3410 _cell_measurement_theta_min 2.0280 _cell_volume 1704.88(14) _computing_cell_refinement ; CrysAlisPro 1.171.40.53 (Rigaku OD, 2019) ; _computing_data_collection ; CrysAlisPro 1.171.40.53 (Rigaku OD, 2019) ; _computing_data_reduction ; CrysAlisPro 1.171.40.53 (Rigaku OD, 2019) ; _computing_molecular_graphics ; Olex2 1.5 (Dolomanov et al., 2009) ; _computing_publication_material ; Olex2 1.5 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1593 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_unetI/netI 0.0509 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 7405 _diffrn_reflns_theta_full 25.027 _diffrn_reflns_theta_max 25.027 _diffrn_reflns_theta_min 2.017 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 1.302 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.87570 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2019) ; _exptl_crystal_colour 'clear dark blue' _exptl_crystal_density_diffrn 1.437 _exptl_crystal_description prism _exptl_crystal_F_000 764 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.314 _refine_diff_density_min -0.270 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 212 _refine_ls_number_reflns 3007 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.047 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0390 _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^)+(0.0304P)^2^+0.6113P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0775 _refine_ls_wR_factor_ref 0.0848 _reflns_number_gt 2382 _reflns_number_total 3007 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jy2029sup1.cif _cod_data_source_block I _cod_depositor_comments 'Adding full bibliography for 2022739.cif.' _cod_database_code 2022739 _cod_database_fobs_code 2022739 _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_min 0.696 _shelx_estimated_absorpt_t_max 0.829 _shelx_hkl_file ; 0 0 -2 266.72 5.32 0 0 2 3998.99 20.36 0 0 -3 0.39 0.52 0 0 3 1.57 1.10 0 0 -4 3323.31 26.45 0 0 4 3256.64 26.05 0 0 5 0.80 1.24 0 0 -5 1.11 1.35 0 0 -6 1456.30 21.54 0 0 6 1351.98 20.71 0 0 7 1.75 1.58 0 0 -7 0.90 1.28 0 0 8 395.53 13.02 0 0 -8 414.56 13.39 0 0 9 0.57 1.42 0 0 -9 0.42 1.56 0 0 10 1706.99 30.25 0 0 -10 1759.35 30.99 0 0 11 2.47 2.34 0 0 12 1722.60 33.57 0 0 13 7.11 3.24 0 0 14 116.83 9.79 0 0 15 1.22 2.15 0 0 16 57.75 7.54 0 0 17 -3.77 2.96 0 0 18 12.68 4.13 0 0 19 -3.26 3.26 0 0 20 -1.13 2.90 0 0 21 0.83 3.34 0 0 22 93.68 11.76 0 0 23 2.53 3.54 0 0 24 20.04 6.29 0 0 25 1.06 3.72 0 0 26 0.11 3.76 0 -1 1 1759.98 13.74 0 1 -1 1756.65 13.56 0 1 1 1801.27 13.17 0 1 1 1742.54 15.05 0 -1 -1 1739.02 15.17 0 1 -2 973.49 10.70 0 1 -2 994.07 12.49 0 -1 2 979.41 12.40 0 1 -2 1014.21 12.43 0 -1 2 958.57 12.59 0 -1 2 974.68 10.96 0 1 -3 543.05 10.68 0 -1 3 565.54 10.79 0 1 3 576.73 8.40 0 -1 3 547.99 10.86 0 -1 3 559.51 9.95 0 1 -3 571.60 10.85 0 1 -3 554.64 9.77 0 1 4 1676.28 17.09 0 -1 4 1658.34 19.67 0 1 -4 1674.31 20.73 0 -1 4 1690.15 21.39 0 -1 4 1587.58 20.44 0 -1 5 241.88 8.80 0 1 -5 244.80 8.79 0 -1 5 252.91 8.73 0 -1 5 251.42 9.13 0 1 5 258.75 7.61 0 -1 6 397.07 11.96 0 -1 6 393.13 12.03 0 1 6 410.55 10.59 0 1 -6 415.80 12.32 0 -1 6 418.30 12.80 0 1 -7 722.56 17.54 0 -1 7 723.87 18.14 0 -1 7 758.25 17.83 0 -1 7 695.47 17.16 0 1 7 688.99 15.06 0 -1 8 437.39 14.99 0 1 8 413.29 12.59 0 1 -8 440.98 14.51 0 -1 8 386.26 13.56 0 -1 8 421.14 14.39 0 -1 9 183.02 10.10 0 -1 9 179.50 9.85 0 1 9 182.66 8.94 0 1 -9 187.36 10.05 0 -1 9 193.33 10.65 0 -1 10 90.83 7.42 0 -1 10 90.98 7.64 0 1 10 100.76 7.05 0 1 11 1315.59 26.84 0 -1 11 1241.86 28.47 0 1 12 0.06 1.60 0 -1 12 3.31 2.49 0 1 13 152.55 10.15 0 -1 13 145.70 10.78 0 -1 14 48.94 6.69 0 1 14 58.62 6.68 0 -1 15 22.97 4.88 0 1 15 28.48 5.15 0 1 16 4.89 2.54 0 -1 16 2.94 2.60 0 1 17 13.25 3.87 0 -1 17 18.95 4.82 0 -1 18 201.32 15.14 0 1 18 232.93 15.23 0 1 19 152.82 13.12 0 -1 19 136.68 13.01 0 -1 20 85.32 10.63 0 1 20 69.75 9.45 0 1 21 13.09 4.98 0 -1 21 7.63 4.24 0 1 22 4.07 3.46 0 -1 22 10.48 5.08 0 -1 23 71.62 11.12 0 1 23 72.63 10.43 0 1 24 17.78 5.54 0 -1 24 16.96 5.95 0 1 25 7.13 4.35 0 -1 25 7.43 4.72 0 1 26 13.10 5.57 0 2 0 20.29 1.73 0 -2 0 21.40 1.72 0 2 0 24.09 1.78 0 2 0 19.48 2.30 0 -2 -1 2.36 1.10 0 2 1 4.10 1.03 0 -2 1 2.56 0.85 0 2 -1 3.14 0.86 0 -2 1 2.70 0.85 0 2 -1 1.63 0.73 0 -2 -1 5.19 1.05 0 2 1 3.12 1.14 0 -2 -2 1193.65 18.09 0 -2 2 1201.42 13.60 0 2 2 1208.11 17.64 0 2 -2 1207.97 16.06 0 2 -2 1238.00 13.44 0 2 2 1241.83 15.71 0 -2 2 1195.75 16.20 0 2 -3 2256.87 20.50 0 2 -3 2306.67 24.33 0 -2 -3 2331.43 25.69 0 2 -3 2259.86 24.94 0 -2 3 2278.91 24.60 0 -2 3 2314.80 21.16 0 -2 4 156.85 7.12 0 2 -4 167.22 7.26 0 2 -4 156.64 6.09 0 -2 4 155.91 6.20 0 2 -4 148.66 7.04 0 2 -5 297.79 10.53 0 -2 5 292.48 10.45 0 2 5 311.39 7.87 0 2 -5 303.95 10.49 0 2 -5 299.15 9.30 0 -2 5 282.28 10.51 0 -2 5 302.53 9.61 0 -2 6 2.50 1.32 0 2 -6 5.23 1.73 0 2 6 4.75 1.38 0 2 -6 6.66 2.47 0 -2 6 2.83 1.73 0 -2 6 5.33 1.68 0 -2 7 643.86 17.98 0 2 -7 624.47 17.18 0 -2 7 622.65 16.29 0 -2 7 611.78 17.21 0 2 7 642.56 13.71 0 -2 8 191.45 10.44 0 -2 8 166.39 9.55 0 2 8 189.13 8.06 0 2 -8 173.37 9.69 0 -2 8 187.45 9.77 0 -2 9 1007.88 23.61 0 2 9 904.58 19.03 0 -2 9 945.73 23.74 0 2 10 174.53 8.87 0 -2 10 168.65 10.56 0 -2 10 176.81 10.64 0 -2 11 40.51 5.92 0 2 11 45.07 4.93 0 2 12 31.30 4.36 0 -2 12 28.53 5.03 0 2 13 274.81 13.18 0 -2 13 286.87 15.65 0 2 14 31.37 4.76 0 -2 14 36.07 6.10 0 -2 15 356.25 18.71 0 2 15 351.74 16.25 0 2 16 67.02 7.56 0 -2 16 63.38 8.58 0 -2 17 0.96 2.83 0 2 17 3.18 2.08 0 2 18 9.32 3.61 0 -2 18 6.75 4.20 0 2 19 168.39 13.20 0 -2 19 154.72 14.26 0 2 20 28.36 6.05 0 -2 20 19.77 6.01 0 -2 21 108.31 12.67 0 2 21 108.85 11.56 0 -2 22 5.51 4.99 0 2 22 11.32 4.58 0 -2 23 3.82 4.56 0 2 23 2.14 2.78 0 -2 24 39.18 8.84 0 2 24 29.47 6.77 0 -2 25 58.61 10.92 0 2 25 59.66 10.23 0 2 26 2.19 3.91 0 2 27 5.11 4.58 0 3 0 0.43 0.67 0 3 0 1.11 0.81 0 3 0 -1.18 1.57 0 -3 0 0.16 0.66 0 3 1 235.82 7.27 0 3 -1 246.79 7.48 0 3 -1 229.99 6.64 0 -3 -1 237.44 7.12 0 3 1 230.03 9.47 0 -3 1 241.11 6.61 0 -3 2 344.61 9.81 0 3 -2 345.43 9.65 0 3 -2 349.24 8.32 0 3 2 343.39 11.59 0 3 2 354.28 9.58 0 -3 -2 364.98 12.11 0 -3 2 350.98 8.24 0 3 3 317.19 11.07 0 3 -3 313.14 10.03 0 3 -3 302.12 8.27 0 -3 3 313.89 10.17 0 -3 -3 323.76 11.50 0 -3 3 308.91 8.35 0 3 3 319.49 9.86 0 3 4 111.03 6.23 0 -3 4 111.67 5.58 0 3 -4 112.39 6.50 0 3 -4 111.22 5.47 0 3 -4 109.88 6.61 0 -3 -4 114.93 7.05 0 -3 4 101.40 6.44 0 3 -5 40.28 4.22 0 -3 5 44.12 3.93 0 -3 -5 47.14 4.74 0 3 -5 40.70 4.51 0 -3 5 40.86 4.36 0 3 -5 43.01 3.78 0 3 -6 15.64 2.53 0 -3 6 15.80 3.03 0 3 6 18.80 2.15 0 3 -6 20.46 3.38 0 -3 -6 16.55 2.92 0 3 -6 17.84 3.21 0 -3 6 12.63 2.30 0 3 -7 46.78 5.11 0 -3 7 44.55 4.58 0 3 7 50.21 3.71 0 -3 7 48.14 5.23 0 3 -7 43.81 5.00 0 -3 8 208.83 10.22 0 3 8 200.38 7.97 0 -3 8 206.54 11.35 0 -3 9 2.37 2.22 0 3 9 1.57 1.39 0 -3 9 2.13 1.74 0 -3 10 418.81 16.21 0 -3 10 385.74 16.65 0 3 10 387.42 12.66 0 -3 11 64.17 7.12 0 3 11 69.38 5.71 0 3 12 211.34 10.43 0 -3 12 195.39 12.94 0 3 13 27.74 4.31 0 -3 13 19.01 4.84 0 -3 14 534.02 22.94 0 3 14 528.90 18.19 0 -3 15 9.92 4.17 0 3 15 11.63 3.24 0 3 16 100.76 8.87 0 -3 16 99.11 10.83 0 -3 17 16.68 5.42 0 3 17 13.04 3.73 0 -3 18 62.22 9.32 0 3 18 70.51 8.21 0 -3 19 -3.98 3.71 0 3 19 4.10 3.08 0 -3 20 180.84 16.45 0 3 20 197.98 14.45 0 -3 21 37.43 7.97 0 3 21 41.08 7.10 0 3 22 21.57 5.19 0 -3 22 37.65 8.20 0 3 23 8.55 4.24 0 -3 23 4.72 4.04 0 3 24 60.01 9.38 0 -3 24 55.85 10.39 0 3 25 4.89 3.96 0 3 26 68.55 10.50 0 4 0 765.61 19.83 0 4 0 780.60 13.86 0 -4 0 748.34 13.77 0 4 0 751.56 14.06 0 4 1 298.35 12.33 0 4 -1 303.44 8.77 0 4 1 307.35 8.06 0 4 1 290.78 9.34 0 4 -1 309.16 9.42 0 -4 1 308.13 8.56 0 4 2 305.35 12.63 0 -4 2 307.20 8.60 0 4 -2 282.72 8.64 0 4 2 307.18 10.01 0 4 -2 314.64 10.22 0 4 -3 74.29 4.56 0 4 3 90.62 5.85 0 -4 -3 86.43 6.89 0 -4 3 79.79 4.73 0 4 -3 85.29 5.74 0 4 3 95.25 7.17 0 -4 4 151.33 6.82 0 4 -4 138.85 6.63 0 4 -4 156.06 8.66 0 -4 4 163.65 8.63 0 4 -4 153.76 8.22 0 -4 -4 151.05 9.22 0 4 4 169.78 8.45 0 -4 5 242.82 9.19 0 4 -5 239.06 8.93 0 -4 5 241.53 11.04 0 4 5 255.39 10.88 0 -4 -5 257.35 12.19 0 4 -5 237.13 11.03 0 4 -5 266.46 11.33 0 4 -6 830.64 17.42 0 -4 6 814.69 17.78 0 4 -6 836.80 21.19 0 -4 6 822.21 21.40 0 4 -6 862.81 21.73 0 4 6 808.07 20.34 0 4 -7 17.74 3.00 0 -4 7 23.13 4.10 0 4 -7 19.83 3.90 0 -4 7 21.49 3.33 0 4 7 24.01 2.60 0 4 7 22.15 3.78 0 4 8 83.45 5.03 0 -4 8 93.60 8.04 0 -4 8 81.25 6.58 0 4 -8 96.64 8.29 0 -4 9 275.68 14.30 0 -4 9 261.26 12.27 0 4 9 270.73 9.48 0 4 -9 254.25 13.74 0 -4 10 234.67 13.82 0 -4 10 269.75 13.12 0 4 10 247.23 9.63 0 -4 11 41.00 6.14 0 4 11 37.39 4.07 0 4 12 302.06 12.01 0 -4 12 304.02 16.85 0 -4 13 380.52 19.51 0 4 13 384.11 14.26 0 -4 14 26.10 5.80 0 4 14 27.60 4.05 0 -4 15 11.14 4.35 0 4 15 9.83 2.98 0 -4 16 116.16 12.16 0 4 16 109.85 8.87 0 4 17 22.65 4.58 0 -4 17 23.34 6.63 0 4 18 135.88 10.83 0 -4 18 132.73 13.96 0 4 19 57.35 7.37 0 -4 19 70.93 10.65 0 -4 20 8.99 4.83 0 4 20 9.67 4.06 0 4 21 41.44 7.03 0 -4 21 37.73 8.68 0 4 22 59.12 8.49 0 -4 22 51.04 10.24 0 -4 23 10.91 6.05 0 5 0 -0.27 1.32 0 5 0 0.36 0.88 0 -5 0 0.03 1.09 0 5 0 0.57 1.94 0 5 -1 192.88 7.96 0 -5 1 187.54 7.45 0 5 -1 177.78 7.90 0 5 -1 181.99 11.00 0 5 1 174.60 8.07 0 5 1 174.97 6.89 0 5 1 186.70 11.18 0 5 2 15.59 3.63 0 5 -2 16.73 2.66 0 -5 2 22.53 2.68 0 5 2 14.96 1.89 0 5 2 16.53 2.82 0 5 -2 12.81 2.20 0 5 -3 74.01 5.75 0 5 3 71.19 6.92 0 5 -3 61.61 4.60 0 5 3 78.12 5.84 0 5 3 70.69 3.87 0 -5 3 68.46 4.64 0 5 4 45.62 4.75 0 5 -4 38.03 3.65 0 5 -4 54.35 5.73 0 5 -4 54.92 5.37 0 5 4 51.44 6.11 0 -5 4 47.98 4.12 0 5 5 551.90 16.96 0 5 -5 514.54 13.73 0 -5 5 547.33 14.15 0 5 -5 547.56 17.88 0 5 -6 21.64 3.03 0 -5 6 19.97 3.11 0 5 6 19.38 3.77 0 -5 6 22.83 4.26 0 5 -6 22.25 4.12 0 -5 7 646.85 17.38 0 5 -7 651.17 21.01 0 5 7 654.61 20.42 0 5 -7 636.25 16.55 0 -5 7 640.46 21.02 0 5 8 13.18 1.98 0 -5 8 13.70 2.95 0 5 8 8.26 3.00 0 -5 8 14.63 3.98 0 5 -8 10.72 3.20 0 -5 9 18.77 4.34 0 5 -9 13.50 3.94 0 5 9 16.68 2.46 0 -5 9 12.64 3.18 0 5 9 15.00 3.74 0 5 10 47.61 4.07 0 5 -10 60.14 7.31 0 -5 10 51.05 5.95 0 5 10 47.52 6.40 0 -5 10 56.12 6.90 0 5 11 327.76 16.88 0 -5 11 302.60 16.98 0 5 11 322.35 11.09 0 5 12 11.78 2.49 0 -5 12 9.87 3.42 0 5 12 15.39 4.92 0 -5 13 284.52 17.57 0 5 13 301.30 11.99 0 5 13 296.59 17.33 0 5 14 0.29 1.34 0 -5 14 2.26 2.54 0 5 15 2.19 1.56 0 -5 15 2.12 3.25 0 -5 16 18.67 5.79 0 5 16 12.60 3.34 0 5 17 320.57 15.07 0 -5 17 308.33 21.01 0 -5 18 45.35 8.72 0 5 18 48.12 6.40 0 -5 19 122.28 14.42 0 -5 20 -1.57 3.33 0 -5 21 17.46 6.60 0 -5 22 -5.30 3.92 0 5 22 10.00 6.09 0 6 0 6.03 1.88 0 6 0 6.06 1.82 0 6 0 2.27 2.03 0 6 -1 2.82 1.42 0 6 1 7.51 2.92 0 6 -1 4.70 2.81 0 6 1 3.03 1.19 0 -6 1 2.24 1.04 0 6 1 1.73 1.65 0 6 -1 3.18 1.60 0 6 2 15.36 2.23 0 6 -2 14.59 3.85 0 6 2 16.66 3.06 0 6 -2 13.11 2.39 0 -6 2 14.11 2.23 0 6 2 18.07 3.98 0 6 -2 14.81 2.73 0 6 -3 47.57 5.05 0 6 3 55.89 5.33 0 6 3 59.01 7.14 0 6 3 53.92 3.68 0 -6 3 62.70 4.71 0 6 -3 49.35 4.51 0 6 4 35.06 5.88 0 6 -4 22.55 3.01 0 6 4 20.94 3.74 0 6 4 28.32 2.50 0 6 -4 25.44 4.38 0 -6 4 25.98 3.28 0 6 5 0.50 0.78 0 6 -5 1.40 2.29 0 6 5 -2.54 2.15 0 6 -5 -1.39 1.54 0 -6 5 -0.80 1.34 0 6 6 322.84 14.41 0 6 -6 289.10 14.54 0 6 -6 305.71 11.20 0 -6 6 310.87 11.55 0 6 7 664.42 21.48 0 -6 7 667.53 17.68 0 6 -7 672.36 22.70 0 6 -7 639.58 16.90 0 6 8 57.39 6.81 0 6 -8 67.11 7.65 0 -6 8 52.43 5.34 0 -6 8 68.53 7.78 0 6 8 57.60 3.59 0 6 -9 139.31 11.10 0 -6 9 134.36 10.90 0 6 9 141.84 5.86 0 6 9 134.69 10.68 0 -6 9 139.47 9.08 0 6 10 4.47 2.21 0 6 10 4.25 1.44 0 -6 10 3.53 2.79 0 6 -10 6.86 3.86 0 6 11 35.52 6.11 0 6 11 37.90 3.52 0 -6 11 27.25 6.09 0 6 12 71.01 5.14 0 6 12 67.49 8.59 0 -6 12 66.40 8.76 0 -6 13 61.73 8.76 0 6 13 60.94 5.04 0 6 13 52.65 8.06 0 6 14 38.61 4.34 0 6 14 28.69 6.55 0 -6 14 45.31 8.12 0 -6 15 40.95 7.79 0 6 15 42.99 7.70 0 -6 16 80.17 11.05 0 6 16 84.80 10.76 0 -6 17 11.63 5.78 0 6 17 4.12 3.80 0 -6 18 119.06 14.21 0 6 18 109.30 13.28 0 -6 19 63.98 10.76 0 6 19 68.98 10.85 0 6 20 -0.22 3.61 0 -6 20 2.62 4.07 0 -6 21 3.00 4.42 0 6 21 8.52 4.15 0 6 22 20.18 7.29 0 7 0 -0.75 2.58 0 7 0 1.61 1.53 0 7 0 0.11 1.28 0 7 1 1.28 1.02 0 7 -1 6.49 3.04 0 7 1 7.72 2.50 0 7 1 6.99 2.93 0 7 -1 4.04 1.67 0 7 -1 5.71 2.12 0 7 -2 289.59 16.99 0 7 2 274.65 16.16 0 -7 2 268.12 10.21 0 7 -2 253.69 11.51 0 7 2 248.50 8.82 0 7 -2 242.16 10.15 0 7 2 264.37 11.81 0 7 -3 2.17 3.18 0 7 3 0.58 3.17 0 7 -3 0.88 1.46 0 -7 3 -2.51 1.65 0 7 3 0.37 1.56 0 7 3 1.41 1.16 0 7 4 117.70 5.05 0 7 -4 128.54 7.12 0 7 -4 130.01 11.69 0 7 -4 153.66 10.68 0 7 4 155.23 12.41 0 7 4 127.63 9.10 0 7 -5 46.01 4.46 0 7 5 53.59 6.27 0 7 5 38.22 2.59 0 7 -5 54.50 6.77 0 7 6 6.84 2.91 0 7 -6 1.70 1.51 0 7 6 3.73 0.90 0 7 -6 7.23 3.22 0 7 -7 78.67 8.29 0 7 -7 87.08 6.31 0 7 7 80.92 7.97 0 7 -8 34.56 5.93 0 7 8 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-11 1 -6 -5.06 4.94 -11 -1 -7 26.80 8.26 -11 1 -7 32.73 8.84 -11 -1 -8 -1.62 4.05 -11 1 -8 0.53 4.20 -11 -1 -9 8.28 5.96 -11 1 -9 11.32 5.97 -11 -1 -10 -8.56 6.85 11 2 -13 36.64 8.37 11 2 -12 -6.47 4.76 -11 2 11 10.46 5.40 11 2 -11 -0.75 3.66 -11 2 10 7.20 5.68 -11 2 9 8.45 5.46 -11 -2 8 -1.55 3.39 -11 2 8 9.65 4.59 -11 -2 7 13.88 5.20 -11 2 7 18.70 6.74 -11 -2 6 5.50 4.17 -11 2 6 -0.62 4.84 -11 -2 5 -2.80 3.34 -11 2 5 -2.35 4.45 -11 -2 4 0.81 3.91 -11 2 4 2.92 3.75 -11 -2 3 19.33 6.15 -11 2 3 20.55 7.02 -11 -2 2 3.00 3.92 -11 2 2 2.01 4.59 -11 2 1 15.22 7.34 -11 -2 1 9.08 4.18 -11 2 0 23.34 7.17 -11 -2 0 24.89 6.86 -11 2 -1 4.17 6.04 -11 -2 -1 -1.32 3.66 -11 2 -2 19.89 7.75 -11 -2 -2 11.81 4.41 -11 2 -3 86.08 13.81 -11 -2 -3 74.90 11.73 -11 -2 -4 -4.55 4.02 -11 2 -4 6.59 7.06 -11 -2 -5 58.94 10.41 -11 2 -5 61.94 11.59 -11 -2 -6 3.87 4.29 -11 2 -6 3.36 5.75 -11 -2 -7 2.86 3.59 -11 2 -7 2.67 4.48 -11 -2 -8 -2.63 5.34 -11 -2 -9 32.81 8.65 -11 -2 -10 3.17 4.68 -11 -2 -11 10.12 6.38 11 3 -12 9.00 4.74 -11 3 9 -0.49 3.96 -11 3 8 5.31 5.05 -11 3 7 -5.10 4.67 -11 3 6 44.67 9.84 -11 3 5 5.67 6.29 -11 3 4 6.55 5.36 -11 3 3 3.99 5.27 -11 3 2 29.86 8.74 -11 3 1 13.03 6.09 -11 3 0 -1.90 4.79 -11 3 -1 -4.95 4.89 -11 -3 -1 -2.65 4.95 -11 3 -2 10.07 5.32 -11 -3 -2 10.99 4.58 -11 3 -3 12.53 6.77 -11 -3 -3 17.05 6.54 -11 -3 -4 23.05 6.83 -11 3 -4 24.37 8.90 -11 -3 -5 1.08 3.81 -11 3 -5 -11.73 5.28 -11 -3 -6 6.37 5.54 -11 -3 -7 16.76 6.17 -11 -3 -8 16.45 6.65 -11 -3 -9 2.71 4.27 -11 -3 -10 46.95 10.32 -11 -3 -11 1.83 3.93 -11 4 4 56.95 12.39 -11 4 3 13.27 9.32 -11 4 2 3.90 5.37 -11 4 1 13.93 6.82 -11 4 0 -2.48 5.07 -11 4 -1 4.28 6.03 11 -5 7 29.86 8.23 -12 0 10 12.79 5.04 -12 0 9 -6.85 6.01 -12 0 8 14.51 6.56 -12 0 7 0.52 4.99 -12 0 6 13.66 5.74 -12 0 5 2.52 6.31 -12 0 4 66.00 12.07 -12 0 3 -7.34 4.32 -12 0 2 17.48 6.51 -12 0 1 -7.97 6.02 -12 0 0 2.64 5.04 -12 0 -1 -2.42 4.10 -12 0 -2 31.18 8.85 -12 0 -3 -1.25 4.10 -12 0 -4 -3.48 4.97 -12 0 -5 -4.99 4.85 -12 -1 10 -2.76 5.16 -12 -1 9 15.83 5.84 -12 -1 8 1.23 4.87 -12 1 8 11.07 6.15 -12 -1 7 -8.59 5.26 -12 1 7 8.37 6.10 -12 -1 6 19.63 6.83 -12 1 6 10.26 5.90 -12 -1 5 22.59 7.32 -12 1 5 17.00 7.39 -12 -1 4 9.19 6.08 -12 1 4 10.80 5.81 -12 -1 3 18.25 7.30 -12 1 3 23.76 7.58 -12 -1 2 3.04 4.75 -12 1 2 5.86 5.98 -12 -1 1 0.61 4.06 -12 1 1 0.32 5.37 -12 1 0 -1.06 5.64 -12 -1 0 4.88 4.88 -12 1 -1 26.77 8.27 -12 -1 -1 32.92 8.69 -12 -1 -2 6.41 4.69 -12 1 -2 9.41 5.89 -12 -1 -3 15.92 6.37 -12 1 -3 8.24 5.48 -12 -1 -4 5.97 5.02 -12 -1 -5 1.69 3.81 -12 -1 -6 3.04 4.27 -12 -2 2 0.99 3.76 -12 -2 1 19.65 6.61 -12 -2 0 8.56 5.38 -12 -2 -1 -2.70 4.65 -12 -2 -2 -1.13 3.55 -12 -2 -3 7.29 5.51 -12 -2 -4 5.02 5.35 -12 -2 -5 17.71 7.18 -12 -2 -6 -3.52 4.11 -12 -2 -7 -6.82 5.64 0 0 0 0.00 0.00 TITL shI_4520_RoLa in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 9.444492 8.940422 20.223676 90.0000 93.2575 90.0000 ZERR 1.00 0.000459 0.000396 0.000858 0.0000 0.0037 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O Cu UNIT 2.00 2.00 6.00 7.00 1.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 5871 _shelx_res_file ; TITL shi_4520_rola_a.res in P2(1)/c shi_4520_rola.res created by SHELXL-2018/3 at 13:01:50 on 28-Mar-2022 REM Old TITL shI_4520_RoLa in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.121, Rweak 0.370, Alpha 0.037 REM 0.622 for 240 systematic absences, Orientation as input REM Formula found by SHELXT: C15 N4 O3 Cu CELL 0.71073 9.4445 8.9404 20.2237 90 93.257 90 ZERR 2 0.0005 0.0004 0.0009 0 0.004 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cu N O UNIT 56 76 4 20 12 L.S. 12 0 0 PLAN 3 SIZE 0.15 0.2 0.3 CONF BOND list 4 fmap 2 53 acta MORE -1 BOND $H SHEL 99 0.84 OMIT -4 5 7 OMIT -2 0 4 OMIT 1 3 8 REM REM REM WGHT 0.030400 0.611300 FVAR 0.42452 CU1 3 0.489068 0.601484 0.588137 11.00000 0.03764 0.03926 = 0.02645 0.00220 0.00264 0.00146 O1 5 0.429431 0.547729 0.677656 11.00000 0.04151 0.05161 = 0.03163 -0.00012 0.00431 -0.00473 O2 5 0.238474 0.488864 0.614843 11.00000 0.05386 0.07868 = 0.04686 -0.00037 -0.00626 -0.00690 O3 5 0.717004 0.688386 0.606520 11.00000 0.03858 0.06361 = 0.05697 -0.00524 0.00845 -0.00712 N1 4 0.577367 0.184168 0.398233 11.00000 0.03747 0.03729 = 0.03141 -0.00031 0.00509 -0.00065 N2 4 0.553882 0.337998 0.507367 11.00000 0.03485 0.03558 = 0.02757 0.00520 0.00161 0.00144 N3 4 0.568979 0.402035 0.569058 11.00000 0.03573 0.03762 = 0.02469 0.00378 0.00087 0.00190 N4 4 0.681568 0.180133 0.573763 11.00000 0.04299 0.04350 = 0.03451 0.00614 0.00001 0.00708 N5 4 0.924671 0.729095 0.558187 11.00000 0.03486 0.06430 = 0.05712 0.00231 0.00260 -0.00653 C1 1 0.574090 0.107805 0.341351 11.00000 0.05072 0.04869 = 0.03791 -0.00295 0.00397 -0.00099 AFIX 43 H1 2 0.537481 0.154425 0.302982 11.00000 -1.20000 AFIX 0 C2 1 0.622580 -0.036895 0.337120 11.00000 0.07083 0.04827 = 0.04473 -0.01007 0.00994 -0.00434 AFIX 43 H2 2 0.618426 -0.086813 0.296711 11.00000 -1.20000 AFIX 0 C3 1 0.677596 -0.106876 0.393950 11.00000 0.06277 0.03915 = 0.06408 -0.00860 0.00954 0.00006 AFIX 43 H3 2 0.712383 -0.204028 0.392220 11.00000 -1.20000 AFIX 0 C4 1 0.680037 -0.030205 0.453265 11.00000 0.04820 0.04115 = 0.04897 0.00609 0.00199 0.00415 AFIX 43 H4 2 0.715879 -0.075095 0.492185 11.00000 -1.20000 AFIX 0 C5 1 0.628121 0.114937 0.453834 11.00000 0.03047 0.03707 = 0.03958 0.00164 0.00691 -0.00264 C6 1 0.623134 0.207434 0.513079 11.00000 0.02979 0.03929 = 0.03224 0.00612 0.00459 0.00002 C7 1 0.646358 0.304661 0.606947 11.00000 0.03482 0.04523 = 0.03268 0.00824 0.00035 -0.00116 C8 1 0.694374 0.332234 0.677660 11.00000 0.05872 0.05904 = 0.03461 0.00428 -0.00780 0.01058 AFIX 23 H8A 2 0.656363 0.254626 0.705100 11.00000 -1.20000 H8B 2 0.656717 0.427334 0.691653 11.00000 -1.20000 AFIX 0 C9 1 0.854585 0.334398 0.688254 11.00000 0.07216 0.13284 = 0.05612 0.01048 -0.02498 -0.00683 AFIX 137 H9A 2 0.892006 0.418177 0.665222 11.00000 -1.50000 H9B 2 0.892983 0.243409 0.671529 11.00000 -1.50000 H9C 2 0.880205 0.342977 0.734718 11.00000 -1.50000 AFIX 0 C10 1 0.795733 0.672134 0.560376 11.00000 0.03653 0.04448 = 0.05434 0.00550 -0.00345 -0.00452 AFIX 43 H10 2 0.761756 0.615416 0.524331 11.00000 -1.20000 AFIX 0 C11 1 1.010954 0.707461 0.501368 11.00000 0.04976 0.08757 = 0.07590 0.00599 0.01609 -0.00593 AFIX 137 H11A 2 1.096094 0.654624 0.515113 11.00000 -1.50000 H11B 2 1.035153 0.803030 0.483543 11.00000 -1.50000 H11C 2 0.958395 0.650492 0.468059 11.00000 -1.50000 AFIX 0 C12 1 0.984326 0.816310 0.613189 11.00000 0.06516 0.13459 = 0.09432 -0.03491 0.00937 -0.04213 AFIX 137 H12A 2 0.975052 0.920858 0.603018 11.00000 -1.50000 H12B 2 1.082830 0.791748 0.620908 11.00000 -1.50000 H12C 2 0.934694 0.794217 0.652151 11.00000 -1.50000 AFIX 0 C13 1 0.303284 0.497423 0.669367 11.00000 0.04604 0.03801 = 0.03824 0.00022 0.00514 0.00155 C14 1 0.234314 0.443556 0.731021 11.00000 0.06445 0.08168 = 0.05418 0.00526 0.02276 -0.01780 AFIX 137 H14A 2 0.221006 0.337203 0.728592 11.00000 -1.50000 H14B 2 0.144052 0.491720 0.733999 11.00000 -1.50000 H14C 2 0.294255 0.467671 0.769470 11.00000 -1.50000 AFIX 0 HKLF 4 REM shi_4520_rola_a.res in P2(1)/c REM wR2 = 0.0848, GooF = S = 1.047, Restrained GooF = 1.047 for all data REM R1 = 0.0390 for 2382 Fo > 4sig(Fo) and 0.0564 for all 3007 data REM 212 parameters refined using 0 restraints END WGHT 0.0304 0.6113 REM Highest difference peak 0.314, deepest hole -0.270, 1-sigma level 0.067 Q1 1 0.5122 0.5224 0.6347 11.00000 0.05 0.31 Q2 1 0.2315 0.5597 0.6372 11.00000 0.05 0.25 Q3 1 0.2251 0.5193 0.7787 11.00000 0.05 0.24 ; _shelx_res_checksum 54945 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_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu1 0.48907(4) 0.60148(4) 0.58814(2) 0.03442(13) Uani d 1 . . O O1 0.4294(2) 0.5477(2) 0.67766(10) 0.0415(5) Uani d 1 . . O O2 0.2385(3) 0.4889(3) 0.61484(12) 0.0601(7) Uani d 1 . . O O3 0.7170(2) 0.6884(3) 0.60652(12) 0.0528(6) Uani d 1 . . N N1 0.5774(3) 0.1842(3) 0.39823(12) 0.0353(6) Uani d 1 . . N N2 0.5539(2) 0.3380(3) 0.50737(11) 0.0327(6) Uani d 1 . . N N3 0.5690(2) 0.4020(2) 0.56906(11) 0.0327(6) Uani d 1 . . N N4 0.6816(3) 0.1801(3) 0.57376(12) 0.0404(6) Uani d 1 . . N N5 0.9247(3) 0.7291(3) 0.55819(14) 0.0521(7) Uani d 1 . . C C1 0.5741(3) 0.1078(4) 0.34135(16) 0.0457(8) Uani d 1 . . H H1 0.537481 0.154425 0.302982 0.055 Uiso calc 1 . . C C2 0.6226(4) -0.0369(4) 0.33712(17) 0.0544(9) Uani d 1 . . H H2 0.618426 -0.086813 0.296711 0.065 Uiso calc 1 . . C C3 0.6776(4) -0.1069(4) 0.39395(19) 0.0551(10) Uani d 1 . . H H3 0.712383 -0.204028 0.392220 0.066 Uiso calc 1 . . C C4 0.6800(3) -0.0302(3) 0.45327(17) 0.0461(8) Uani d 1 . . H H4 0.715879 -0.075095 0.492185 0.055 Uiso calc 1 . . C C5 0.6281(3) 0.1149(3) 0.45383(15) 0.0355(7) Uani d 1 . . C C6 0.6231(3) 0.2074(3) 0.51308(14) 0.0337(7) Uani d 1 . . C C7 0.6464(3) 0.3047(3) 0.60695(15) 0.0376(7) Uani d 1 . . C C8 0.6944(4) 0.3322(4) 0.67766(16) 0.0512(9) Uani d 1 . . H H8A 0.656363 0.254626 0.705100 0.061 Uiso calc 1 . . H H8B 0.656717 0.427334 0.691653 0.061 Uiso calc 1 . . C C9 0.8546(4) 0.3344(5) 0.6883(2) 0.0881(14) Uani d 1 . . H H9A 0.892006 0.418177 0.665222 0.132 Uiso calc 1 . . H H9B 0.892983 0.243409 0.671529 0.132 Uiso calc 1 . . H H9C 0.880205 0.342977 0.734718 0.132 Uiso calc 1 . . C C10 0.7957(3) 0.6721(3) 0.56038(17) 0.0453(8) Uani d 1 . . H H10 0.761756 0.615416 0.524331 0.054 Uiso calc 1 . . C C11 1.0110(4) 0.7075(4) 0.5014(2) 0.0706(12) Uani d 1 . . H H11A 1.096094 0.654624 0.515113 0.106 Uiso calc 1 . . H H11B 1.035153 0.803030 0.483543 0.106 Uiso calc 1 . . H H11C 0.958395 0.650492 0.468059 0.106 Uiso calc 1 . . C C12 0.9843(5) 0.8163(6) 0.6132(2) 0.0978(16) Uani d 1 . . H H12A 0.975052 0.920858 0.603018 0.147 Uiso calc 1 . . H H12B 1.082830 0.791748 0.620908 0.147 Uiso calc 1 . . H H12C 0.934694 0.794217 0.652151 0.147 Uiso calc 1 . . C C13 0.3033(4) 0.4974(3) 0.66937(16) 0.0407(8) Uani d 1 . . C C14 0.2343(4) 0.4436(4) 0.73102(18) 0.0660(11) Uani d 1 . . H H14A 0.221006 0.337203 0.728592 0.099 Uiso calc 1 . . H H14B 0.144052 0.491720 0.733999 0.099 Uiso calc 1 . . H H14C 0.294255 0.467671 0.769470 0.099 Uiso calc 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu1 0.0376(2) 0.0393(2) 0.0265(2) 0.00146(18) 0.00264(15) 0.00220(17) O1 0.0415(14) 0.0516(13) 0.0316(12) -0.0047(11) 0.0043(10) -0.0001(10) O2 0.0539(16) 0.0787(17) 0.0469(15) -0.0069(13) -0.0063(12) -0.0004(13) O3 0.0386(14) 0.0636(15) 0.0570(16) -0.0071(11) 0.0085(12) -0.0052(12) N1 0.0375(15) 0.0373(14) 0.0314(15) -0.0007(12) 0.0051(11) -0.0003(12) N2 0.0348(15) 0.0356(13) 0.0276(14) 0.0014(11) 0.0016(11) 0.0052(11) N3 0.0357(15) 0.0376(13) 0.0247(13) 0.0019(12) 0.0009(11) 0.0038(11) N4 0.0430(16) 0.0435(15) 0.0345(15) 0.0071(13) 0.0000(12) 0.0061(13) N5 0.0349(17) 0.0643(18) 0.057(2) -0.0065(14) 0.0026(14) 0.0023(15) C1 0.051(2) 0.049(2) 0.0379(19) -0.0010(16) 0.0040(16) -0.0029(16) C2 0.071(3) 0.048(2) 0.045(2) -0.0043(19) 0.0099(19) -0.0101(18) C3 0.063(3) 0.0392(18) 0.064(3) 0.0001(17) 0.010(2) -0.0086(18) C4 0.048(2) 0.0411(18) 0.049(2) 0.0041(16) 0.0020(16) 0.0061(16) C5 0.0305(17) 0.0371(17) 0.0396(18) -0.0026(14) 0.0069(13) 0.0016(14) C6 0.0298(17) 0.0393(17) 0.0322(17) 0.0000(14) 0.0046(13) 0.0061(14) C7 0.0348(18) 0.0452(18) 0.0327(18) -0.0012(15) 0.0003(14) 0.0082(15) C8 0.059(2) 0.059(2) 0.0346(19) 0.0106(18) -0.0078(16) 0.0043(17) C9 0.072(3) 0.133(4) 0.056(3) -0.007(3) -0.025(2) 0.010(3) C10 0.037(2) 0.0445(19) 0.054(2) -0.0045(16) -0.0035(16) 0.0055(17) C11 0.050(2) 0.088(3) 0.076(3) -0.006(2) 0.016(2) 0.006(2) C12 0.065(3) 0.135(4) 0.094(4) -0.042(3) 0.009(3) -0.035(3) C13 0.046(2) 0.0380(18) 0.038(2) 0.0015(16) 0.0051(16) 0.0002(14) C14 0.064(3) 0.082(3) 0.054(2) -0.018(2) 0.023(2) 0.005(2) 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' 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Cu1 O3 . . 104.24(9) ? O1 Cu1 N1 . 3_666 89.93(9) ? O1 Cu1 N2 . 3_666 151.98(9) ? N1 Cu1 O3 3_666 . 87.31(9) ? N2 Cu1 O3 3_666 . 101.48(9) ? N2 Cu1 N1 3_666 3_666 80.29(10) ? N3 Cu1 O1 . . 95.20(9) ? N3 Cu1 O3 . . 88.40(9) ? N3 Cu1 N1 . 3_666 173.99(10) ? N3 Cu1 N2 . 3_666 96.46(9) ? C13 O1 Cu1 . . 106.07(19) ? C10 O3 Cu1 . . 115.9(2) ? C1 N1 Cu1 . 3_666 127.1(2) ? C1 N1 C5 . . 118.2(3) ? C5 N1 Cu1 . 3_666 114.60(19) ? N3 N2 Cu1 . 3_666 139.50(18) ? C6 N2 Cu1 . 3_666 112.67(19) ? C6 N2 N3 . . 105.1(2) ? N2 N3 Cu1 . . 122.07(17) ? C7 N3 Cu1 . . 132.1(2) ? C7 N3 N2 . . 105.8(2) ? C6 N4 C7 . . 101.8(2) ? C10 N5 C11 . . 122.1(3) ? C10 N5 C12 . . 120.1(3) ? C12 N5 C11 . . 117.8(3) ? N1 C1 H1 . . 118.6 ? N1 C1 C2 . . 122.8(3) ? C2 C1 H1 . . 118.6 ? C1 C2 H2 . . 120.5 ? C1 C2 C3 . . 118.9(3) ? C3 C2 H2 . . 120.5 ? C2 C3 H3 . . 120.5 ? C4 C3 C2 . . 119.0(3) ? C4 C3 H3 . . 120.5 ? C3 C4 H4 . . 120.6 ? C3 C4 C5 . . 118.9(3) ? C5 C4 H4 . . 120.6 ? N1 C5 C4 . . 122.1(3) ? N1 C5 C6 . . 113.5(2) ? C4 C5 C6 . . 124.4(3) ? N2 C6 C5 . . 117.5(3) ? N4 C6 N2 . . 114.3(3) ? N4 C6 C5 . . 128.2(3) ? N3 C7 N4 . . 113.0(3) ? N3 C7 C8 . . 124.2(3) ? N4 C7 C8 . . 122.7(3) ? C7 C8 H8A . . 109.1 ? C7 C8 H8B . . 109.1 ? C7 C8 C9 . . 112.5(3) ? H8A C8 H8B . . 107.8 ? C9 C8 H8A . . 109.1 ? C9 C8 H8B . . 109.1 ? C8 C9 H9A . . 109.5 ? C8 C9 H9B . . 109.5 ? C8 C9 H9C . . 109.5 ? H9A C9 H9B . . 109.5 ? H9A C9 H9C . . 109.5 ? H9B C9 H9C . . 109.5 ? O3 C10 N5 . . 125.1(3) ? O3 C10 H10 . . 117.4 ? N5 C10 H10 . . 117.4 ? N5 C11 H11A . . 109.5 ? N5 C11 H11B . . 109.5 ? N5 C11 H11C . . 109.5 ? H11A C11 H11B . . 109.5 ? H11A C11 H11C . . 109.5 ? H11B C11 H11C . . 109.5 ? N5 C12 H12A . . 109.5 ? N5 C12 H12B . . 109.5 ? N5 C12 H12C . . 109.5 ? H12A C12 H12B . . 109.5 ? H12A C12 H12C . . 109.5 ? H12B C12 H12C . . 109.5 ? O1 C13 C14 . . 116.4(3) ? O2 C13 O1 . . 123.5(3) ? O2 C13 C14 . . 120.0(3) ? C13 C14 H14A . . 109.5 ? C13 C14 H14B . . 109.5 ? C13 C14 H14C . . 109.5 ? H14A C14 H14B . . 109.5 ? H14A C14 H14C . . 109.5 ? H14B C14 H14C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu1 O1 . 1.985(2) ? Cu1 O3 . 2.299(2) ? Cu1 N1 3_666 2.040(2) ? Cu1 N2 3_666 2.025(2) ? Cu1 N3 . 1.983(2) ? O1 C13 . 1.276(4) ? O2 C13 . 1.233(4) ? O3 C10 . 1.234(4) ? N1 C1 . 1.337(4) ? N1 C5 . 1.348(4) ? N2 N3 . 1.373(3) ? N2 C6 . 1.340(3) ? N3 C7 . 1.347(3) ? N4 C6 . 1.339(3) ? N4 C7 . 1.351(4) ? N5 C10 . 1.323(4) ? N5 C11 . 1.459(4) ? N5 C12 . 1.446(5) ? C1 H1 . 0.9300 ? C1 C2 . 1.377(4) ? C2 H2 . 0.9300 ? C2 C3 . 1.384(5) ? C3 H3 . 0.9300 ? C3 C4 . 1.381(4) ? C4 H4 . 0.9300 ? C4 C5 . 1.387(4) ? C5 C6 . 1.459(4) ? C7 C8 . 1.496(4) ? C8 H8A . 0.9700 ? C8 H8B . 0.9700 ? C8 C9 . 1.516(5) ? C9 H9A . 0.9600 ? C9 H9B . 0.9600 ? C9 H9C . 0.9600 ? C10 H10 . 0.9300 ? C11 H11A . 0.9600 ? C11 H11B . 0.9600 ? C11 H11C . 0.9600 ? C12 H12A . 0.9600 ? C12 H12B . 0.9600 ? C12 H12C . 0.9600 ? C13 C14 . 1.518(4) ? C14 H14A . 0.9600 ? C14 H14B . 0.9600 ? C14 H14C . 0.9600 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C3 H3 O2 3_656 0.93 2.59 3.513(4) 170 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Cu1 O1 C13 O2 . . . . -0.5(4) ? Cu1 O1 C13 C14 . . . . 178.2(2) ? Cu1 O3 C10 N5 . . . . 172.0(2) ? Cu1 N1 C1 C2 3_666 . . . 179.5(2) ? Cu1 N1 C5 C4 3_666 . . . -178.8(2) ? Cu1 N1 C5 C6 3_666 . . . 0.9(3) ? Cu1 N2 N3 Cu1 3_666 . . . 20.3(4) ? Cu1 N2 N3 C7 3_666 . . . -158.4(2) ? Cu1 N2 C6 N4 3_666 . . . 165.50(19) ? Cu1 N2 C6 C5 3_666 . . . -13.5(3) ? Cu1 N3 C7 N4 . . . . -179.03(19) ? Cu1 N3 C7 C8 . . . . -1.4(5) ? N1 C1 C2 C3 . . . . -0.2(5) ? N1 C5 C6 N2 . . . . 8.5(4) ? N1 C5 C6 N4 . . . . -170.3(3) ? N2 N3 C7 N4 . . . . -0.6(3) ? N2 N3 C7 C8 . . . . 177.1(3) ? N3 N2 C6 N4 . . . . 0.5(3) ? N3 N2 C6 C5 . . . . -178.5(2) ? N3 C7 C8 C9 . . . . -118.2(4) ? N4 C7 C8 C9 . . . . 59.2(4) ? C1 N1 C5 C4 . . . . 1.8(4) ? C1 N1 C5 C6 . . . . -178.5(3) ? C1 C2 C3 C4 . . . . 1.0(5) ? C2 C3 C4 C5 . . . . -0.4(5) ? C3 C4 C5 N1 . . . . -1.0(5) ? C3 C4 C5 C6 . . . . 179.3(3) ? C4 C5 C6 N2 . . . . -171.7(3) ? C4 C5 C6 N4 . . . . 9.4(5) ? C5 N1 C1 C2 . . . . -1.2(5) ? C6 N2 N3 Cu1 . . . . 178.70(18) ? C6 N2 N3 C7 . . . . 0.1(3) ? C6 N4 C7 N3 . . . . 0.8(3) ? C6 N4 C7 C8 . . . . -176.8(3) ? C7 N4 C6 N2 . . . . -0.8(3) ? C7 N4 C6 C5 . . . . 178.1(3) ? C11 N5 C10 O3 . . . . -178.9(3) ? C12 N5 C10 O3 . . . . 1.0(5) ?