#------------------------------------------------------------------------------ #$Date: 2021-01-01 10:40:07 +0200 (Fri, 01 Jan 2021) $ #$Revision: 260342 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/23/2022306.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_2022306 loop_ _publ_author_name 'Niu, Xiang-Long' 'Wei, Lin' 'Liu, Jian-Cheng' 'Jia, Wan-He' 'Ma, Jian-Ping' 'Wang, Lei' 'Wang, Jian-Cheng' 'Dong, Yu-Bin' _publ_section_title ; Syntheses and structures of three macrocyclic supramolecular complexes and one Zn^II^-containing coordination polymer generated from a semi-rigid multidentate N-containing ligand ; _journal_coeditor_code OP3008 _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 29 _journal_page_last 39 _journal_paper_doi 10.1107/S2053229620016083 _journal_volume 77 _journal_year 2021 _chemical_formula_iupac '[Zn I2 (C12 H10 N6)], C H Cl3' _chemical_formula_moiety 'C12 H10 I2 N6 Zn, C H Cl3' _chemical_formula_sum 'C13 H11 Cl3 I2 N6 Zn' _chemical_formula_weight 676.80 _chemical_name_systematic 'catena-Poly[[[diiodidozinc(II)]-\m-4-{2-[(pyridin-3-yl)methyl]-2H-tetrazol-5-yl}pyridine] chloroform monosolvate]' _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-97 _cell_angle_alpha 69.430(14) _cell_angle_beta 65.912(18) _cell_angle_gamma 65.912(18) _cell_formula_units_Z 2 _cell_length_a 9.804(13) _cell_length_b 11.350(14) _cell_length_c 11.350(14) _cell_measurement_reflns_used 2745 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 20.624 _cell_measurement_theta_min 2.341 _cell_volume 1026(2) _computing_cell_refinement ; APEX2 (Bruker, 2012) ; _computing_data_collection ; APEX2 (Bruker, 2012) ; _computing_data_reduction ; SAINT (Bruker, 2012) ; _computing_publication_material ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1284 _diffrn_reflns_av_unetI/netI 0.1317 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 5299 _diffrn_reflns_theta_full 25.049 _diffrn_reflns_theta_max 25.049 _diffrn_reflns_theta_min 2.016 _exptl_absorpt_coefficient_mu 4.604 _exptl_absorpt_correction_T_max 0.6312 _exptl_absorpt_correction_T_min 0.4908 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2012) ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 636 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _refine_diff_density_max 2.403 _refine_diff_density_min -1.890 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.228 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 239 _refine_ls_number_reflns 3598 _refine_ls_number_restraints 48 _refine_ls_restrained_S_all 1.234 _refine_ls_R_factor_all 0.1638 _refine_ls_R_factor_gt 0.1308 _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^)+(0.1720P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3222 _refine_ls_wR_factor_ref 0.3469 _reflns_number_gt 2424 _reflns_number_total 3598 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file op3008sup1.cif _cod_data_source_block IV _cod_database_code 2022306 _shelx_hkl_file ; -1 0 0 565.13 7.24 -2 0 0 624.59 11.62 -3 0 0 5.04 1.22 -4 0 0 30.02 2.85 -5 0 0 48.98 5.44 -6 0 0 -0.27 1.53 -7 0 0 4.64 2.19 -8 0 0 71.28 7.22 -9 0 0 16.75 4.62 -10 0 0 31.75 7.74 0 1 -1 56.52 2.55 1 1 -1 263.84 7.20 -1 1 -1 195.96 5.55 2 1 -1 1892.96 18.92 -2 1 -1 56.15 2.60 -3 -1 1 852.13 14.88 -3 1 -1 4.20 1.40 -4 -1 1 185.07 6.20 -4 1 -1 46.50 3.80 -5 -1 1 34.89 3.81 -5 1 -1 326.48 12.80 -6 -1 1 8.29 1.97 -6 1 -1 497.48 21.60 -7 -1 1 0.96 1.22 -7 1 -1 126.95 8.40 -8 -1 1 1.70 2.28 -8 1 -1 61.09 8.88 -9 -1 1 9.92 4.91 -9 1 -1 2.61 3.44 10 1 -1 16.52 6.68 -10 1 -1 4.22 3.39 0 2 -2 40.46 2.51 1 2 -2 0.64 0.71 -1 2 -2 62.27 4.52 2 2 -2 12.48 2.29 -2 2 -2 156.32 6.53 3 2 -2 0.47 0.48 -3 2 -2 58.67 3.81 4 2 -2 264.06 8.55 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2.95 1.91 8 6 3 9.13 2.67 7 3 6 85.67 6.05 7 6 3 22.37 4.67 6 3 6 326.49 13.65 6 6 3 2.63 1.98 5 3 6 853.82 19.06 5 6 3 27.07 4.28 4 3 6 214.99 7.01 4 6 3 71.36 6.49 3 3 6 74.01 3.36 3 6 3 108.45 7.53 2 3 6 6.63 0.79 2 6 3 137.59 7.36 1 3 6 39.99 1.84 1 6 3 76.16 5.89 0 3 6 24.34 1.61 0 6 3 -0.06 1.30 -1 3 6 8.77 1.55 -1 6 3 28.46 5.01 -2 3 6 18.09 2.47 -2 6 3 23.74 4.15 -3 3 6 44.72 3.80 -3 6 3 11.50 3.07 -4 3 6 76.07 6.89 -4 6 3 37.26 5.44 -5 3 6 16.83 3.54 -5 6 3 12.76 3.20 -6 3 6 6.35 2.81 -6 6 3 8.61 3.15 -7 6 3 6.59 4.36 12 2 7 19.35 5.05 -11 -2 -7 19.27 8.07 11 7 2 16.94 5.07 -10 -2 -7 4.15 3.89 10 7 2 41.51 6.79 -9 -2 -7 0.10 3.81 9 7 2 24.21 4.67 -8 -2 -7 28.37 4.34 8 7 2 1.15 1.53 -7 -2 -7 58.74 5.30 7 7 2 10.79 3.13 -6 -2 -7 66.69 6.85 6 7 2 106.01 8.18 5 7 2 69.58 5.53 4 7 2 173.07 9.68 3 7 2 10.19 4.13 2 7 2 6.45 2.32 1 7 2 31.92 5.55 0 7 2 7.70 3.28 -1 7 2 51.05 6.65 -2 7 2 3.42 2.34 -3 7 2 0.77 1.54 -4 7 2 4.49 1.69 -5 7 2 4.00 2.72 -6 7 2 3.80 2.26 -7 7 2 3.43 2.50 11 8 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96.35 8.32 -2 4 6 2.86 1.22 -2 6 4 46.00 5.28 -3 4 6 22.51 4.28 -3 6 4 28.47 4.96 -4 4 6 32.59 4.64 -4 6 4 8.29 3.38 -5 4 6 84.43 10.90 -5 6 4 3.48 3.13 -6 4 6 34.03 6.02 -6 6 4 14.17 3.73 -7 6 4 17.57 6.99 12 3 7 12.28 7.57 12 7 3 9.65 4.00 11 3 7 10.47 3.62 11 7 3 29.12 6.32 10 3 7 5.38 2.77 10 7 3 67.44 9.15 9 3 7 7.67 2.80 9 7 3 36.68 6.07 8 3 7 33.76 4.30 8 7 3 4.46 2.09 7 3 7 97.77 9.36 7 7 3 2.87 2.34 6 3 7 250.11 11.58 6 7 3 78.38 7.54 5 3 7 34.16 2.74 5 7 3 54.56 5.20 4 3 7 20.51 2.25 4 7 3 3.78 2.28 3 7 3 221.03 10.07 2 7 3 368.04 13.54 1 7 3 317.47 13.13 0 7 3 121.19 7.44 -1 7 3 106.71 8.42 -2 7 3 0.17 2.10 -3 7 3 2.90 1.60 -4 7 3 2.39 2.18 -5 7 3 2.06 2.26 -6 7 3 4.13 3.12 -7 7 3 2.73 2.33 11 8 2 2.36 1.73 10 8 2 0.89 1.57 9 8 2 7.24 2.75 8 8 2 1.65 1.77 7 8 2 5.63 2.33 6 8 2 34.50 4.03 5 8 2 176.88 10.14 4 8 2 191.96 12.27 3 8 2 144.37 11.28 2 8 2 2.81 2.49 1 8 2 7.55 2.91 0 8 2 47.99 7.75 -1 8 2 86.85 9.22 -2 8 2 1.85 1.84 -3 8 2 4.48 2.19 -4 8 2 14.98 3.18 -5 8 2 8.45 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64.27 4.63 3 7 5 84.24 6.16 2 5 7 239.46 7.90 2 7 5 56.09 6.24 1 5 7 113.95 5.85 1 7 5 58.57 7.76 0 7 5 6.71 2.27 -1 7 5 16.07 3.42 -2 7 5 55.83 5.70 -3 7 5 19.64 4.06 -4 7 5 8.71 2.68 -5 7 5 10.36 3.73 -6 7 5 14.50 4.35 12 4 8 15.42 6.75 12 8 4 11.24 3.82 11 4 8 14.25 5.55 11 8 4 3.33 2.43 10 4 8 20.05 5.71 10 8 4 3.08 2.14 9 4 8 60.16 8.64 9 8 4 7.08 2.78 8 8 4 2.04 2.14 7 8 4 20.03 3.71 6 8 4 -0.40 2.50 5 8 4 26.55 4.72 4 8 4 22.15 5.24 3 8 4 8.58 2.80 2 8 4 0.20 2.74 1 8 4 6.77 2.81 0 8 4 3.12 2.01 -1 8 4 19.17 4.07 -2 8 4 12.43 3.21 -3 8 4 47.31 5.86 -4 8 4 21.47 4.30 -5 8 4 11.95 3.20 -6 8 4 8.53 3.23 11 9 3 0.73 2.06 10 9 3 2.51 2.05 9 9 3 1.98 1.96 8 9 3 6.47 2.78 7 9 3 38.20 5.85 6 9 3 39.03 5.16 5 9 3 126.08 10.83 4 9 3 55.21 8.02 3 9 3 52.86 6.07 2 9 3 4.15 3.54 1 9 3 13.36 3.80 0 9 3 15.04 3.36 -1 9 3 24.95 4.60 -2 9 3 12.63 3.80 -3 9 3 10.25 2.71 -4 9 3 6.23 1.99 -5 9 3 3.62 2.94 10 10 2 8.67 2.69 9 10 2 16.60 2.77 8 10 2 39.84 5.89 7 10 2 21.70 4.01 6 10 2 12.60 3.25 5 10 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90.33 6.21 2 6 7 263.70 8.92 2 7 6 46.18 4.91 1 6 7 233.98 9.61 1 7 6 20.93 3.22 0 6 7 109.94 5.70 0 7 6 14.81 3.04 -1 6 7 85.28 6.41 -1 7 6 11.99 2.68 -2 7 6 5.71 2.39 -3 7 6 3.59 2.67 -4 7 6 36.61 6.75 -5 7 6 10.96 3.32 -6 7 6 39.03 9.61 12 5 8 7.69 5.00 12 8 5 12.67 4.41 11 5 8 6.20 3.76 11 8 5 5.71 2.65 10 5 8 2.44 1.91 10 8 5 -0.47 1.71 9 5 8 20.27 2.93 9 8 5 0.96 2.34 8 8 5 3.95 2.49 7 8 5 5.99 3.02 6 8 5 7.18 3.62 5 8 5 22.13 3.93 4 8 5 11.73 3.62 3 8 5 5.79 2.40 2 8 5 0.79 1.71 1 8 5 -0.67 2.96 0 8 5 4.30 2.19 -1 8 5 12.95 3.92 -2 8 5 14.15 2.85 -3 8 5 21.99 4.57 -4 8 5 6.50 3.25 -5 8 5 6.05 3.70 11 9 4 20.77 4.74 10 9 4 9.12 3.23 9 9 4 3.41 2.45 8 9 4 16.06 3.75 7 9 4 43.57 6.51 6 9 4 21.53 4.12 5 9 4 7.39 3.59 4 9 4 -0.79 2.81 3 9 4 25.35 4.54 2 9 4 32.90 5.23 1 9 4 44.27 6.74 0 9 4 2.81 1.92 -1 9 4 9.74 3.24 -2 9 4 3.24 2.05 -3 9 4 3.27 2.30 -4 9 4 7.64 3.01 -5 9 4 2.79 2.37 11 10 3 -0.01 1.65 10 10 3 11.38 3.29 9 10 3 2.14 1.42 8 10 3 -0.41 2.08 7 10 3 5.81 2.52 6 10 3 49.10 6.62 5 10 3 93.92 10.03 4 10 3 87.43 8.73 3 10 3 21.37 5.19 2 10 3 2.42 3.02 1 10 3 2.95 2.59 0 10 3 5.76 2.35 -1 10 3 14.91 3.91 -2 10 3 5.19 2.98 -3 10 3 7.90 2.74 -4 10 3 7.80 2.08 10 11 2 5.13 2.16 9 11 2 6.88 3.03 8 11 2 3.68 2.10 7 11 2 9.90 2.95 6 11 2 24.93 6.81 5 11 2 2.34 4.24 4 11 2 5.17 2.87 3 11 2 6.41 4.31 2 11 2 3.48 2.74 1 11 2 8.18 3.36 0 11 2 22.29 4.23 -1 11 2 49.98 6.90 -2 11 2 36.20 6.02 -3 11 2 5.65 2.51 9 12 1 0.37 2.50 8 12 1 5.97 3.65 7 12 1 10.95 5.72 6 12 1 -0.93 3.98 5 12 1 2.93 3.47 4 12 1 7.48 4.14 3 12 1 28.38 7.64 2 12 1 35.80 7.48 1 12 1 36.92 8.71 0 12 1 11.51 3.25 -1 12 1 4.96 2.55 -2 12 1 4.44 2.45 6 13 0 0.28 3.64 5 13 0 0.80 3.22 4 13 0 4.54 5.90 3 13 0 5.08 4.96 2 13 0 5.22 5.03 1 13 0 3.94 6.08 12 7 7 2.35 2.89 11 7 7 4.21 4.37 10 7 7 5.86 3.29 9 7 7 1.67 2.29 8 7 7 17.24 3.99 7 7 7 40.81 4.72 6 7 7 41.51 4.95 5 7 7 36.51 4.28 4 7 7 23.33 3.12 3 7 7 33.47 4.36 2 7 7 4.19 1.38 1 7 7 84.68 7.84 -1 7 7 39.76 4.03 -2 7 7 45.33 5.90 12 6 8 1.60 5.18 12 8 6 4.26 4.11 11 6 8 8.53 5.68 11 8 6 3.72 2.39 10 6 8 10.91 6.60 10 8 6 27.27 4.82 9 6 8 12.72 4.18 9 8 6 91.45 9.31 8 6 8 6.02 2.23 8 8 6 76.95 8.14 7 8 6 38.66 4.55 6 8 6 6.49 2.70 5 8 6 5.44 2.45 4 8 6 3.82 2.27 3 8 6 7.73 3.21 2 8 6 38.59 4.81 1 8 6 51.40 5.21 0 8 6 56.81 6.88 -1 8 6 22.44 3.85 -2 8 6 9.09 2.34 -3 8 6 9.10 3.38 -4 8 6 6.06 3.05 -5 8 6 6.74 3.69 12 9 5 8.84 3.43 11 9 5 18.37 4.65 10 9 5 7.09 2.86 9 9 5 2.77 2.39 8 9 5 24.27 4.18 7 9 5 18.05 4.47 6 9 5 12.49 3.66 5 9 5 27.58 6.48 4 9 5 44.64 5.68 3 9 5 288.21 16.37 2 9 5 115.75 9.50 1 9 5 45.78 5.13 0 9 5 4.23 2.11 -1 9 5 9.88 3.49 -2 9 5 8.01 2.74 -3 9 5 4.15 1.90 -4 9 5 4.08 2.76 -5 9 5 5.04 2.78 11 10 4 2.32 1.96 10 10 4 7.62 2.92 9 10 4 0.43 1.30 8 10 4 3.36 2.60 7 10 4 10.13 3.09 6 10 4 70.14 8.63 5 10 4 64.18 7.19 4 10 4 10.25 3.72 3 10 4 5.73 3.96 2 10 4 28.64 5.47 1 10 4 34.44 7.25 0 10 4 34.96 6.23 -1 10 4 11.27 3.58 -2 10 4 6.03 2.59 -3 10 4 7.90 2.39 -4 10 4 8.77 3.10 10 11 3 3.53 1.76 9 11 3 0.90 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34.37 4.36 7 9 6 109.64 10.12 6 9 6 16.84 3.35 5 9 6 0.84 1.91 4 9 6 0.51 1.63 3 9 6 29.01 5.34 2 9 6 2.59 2.17 1 9 6 24.11 3.82 0 9 6 42.32 6.60 -2 9 6 27.05 4.59 -3 9 6 19.52 4.14 -4 9 6 1.94 1.81 11 10 5 6.51 2.75 10 10 5 4.49 2.71 9 10 5 5.04 2.02 8 10 5 3.26 2.96 7 10 5 0.61 2.25 6 10 5 1.96 2.91 5 10 5 5.96 3.71 4 10 5 20.99 3.82 3 10 5 131.80 11.70 2 10 5 61.86 7.19 1 10 5 68.61 6.45 0 10 5 14.80 3.49 -1 10 5 5.49 2.80 -2 10 5 4.52 2.09 -3 10 5 3.98 1.45 -4 10 5 4.67 2.74 11 11 4 2.99 1.66 10 11 4 8.90 2.54 9 11 4 1.55 2.85 8 11 4 0.64 1.88 7 11 4 2.70 3.00 6 11 4 10.79 4.90 5 11 4 16.56 4.66 4 11 4 7.35 3.38 3 11 4 29.06 6.54 2 11 4 -0.22 2.12 1 11 4 2.55 1.92 0 11 4 4.76 2.92 -1 11 4 4.18 2.36 -2 11 4 4.94 2.21 -3 11 4 3.49 1.93 9 12 3 4.74 2.59 8 12 3 4.40 2.74 7 12 3 12.50 5.53 6 12 3 0.35 3.55 5 12 3 16.34 4.49 4 12 3 6.53 3.43 3 12 3 7.32 4.50 2 12 3 1.88 2.73 1 12 3 7.47 2.48 0 12 3 4.93 2.92 -1 12 3 3.30 3.04 -2 12 3 2.71 2.48 8 13 2 11.08 5.02 7 13 2 1.32 3.42 6 13 2 6.56 3.49 5 13 2 7.24 3.34 4 13 2 21.19 5.77 3 13 2 21.19 5.06 2 13 2 14.96 4.28 1 13 2 2.85 2.07 0 13 2 6.94 3.50 12 8 8 1.94 2.71 11 8 8 4.04 2.81 10 8 8 21.92 4.54 9 8 8 0.70 1.80 8 8 8 7.80 2.36 7 8 8 49.27 6.00 12 9 7 3.62 3.26 11 9 7 3.31 2.58 10 9 7 3.11 2.18 9 9 7 1.98 2.38 8 9 7 3.23 2.98 7 9 7 5.33 2.39 6 9 7 30.23 5.07 5 9 7 19.37 3.89 4 9 7 84.45 7.02 3 9 7 37.63 5.00 2 9 7 2.73 1.51 1 9 7 6.24 2.75 0 9 7 58.12 7.48 -1 9 7 9.75 2.14 -2 9 7 4.49 2.50 12 10 6 3.83 2.32 11 10 6 5.43 2.81 10 10 6 1.30 2.35 9 10 6 1.58 1.47 8 10 6 3.92 3.17 7 10 6 3.50 2.42 6 10 6 31.29 6.83 5 10 6 11.16 3.67 4 10 6 3.42 2.32 3 10 6 1.52 1.87 2 10 6 10.25 4.12 1 10 6 5.68 2.11 0 10 6 15.78 4.31 -1 10 6 19.48 4.06 -2 10 6 20.86 3.81 -3 10 6 15.30 3.60 11 11 5 -1.44 1.23 10 11 5 4.47 2.50 9 11 5 4.86 3.09 8 11 5 26.52 5.12 7 11 5 24.87 5.52 6 11 5 36.33 5.77 5 11 5 20.56 4.56 4 11 5 1.65 2.83 3 11 5 21.16 4.75 2 11 5 5.50 2.91 1 11 5 12.95 3.16 0 11 5 15.92 4.22 -1 11 5 13.68 3.97 -2 11 5 3.72 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-3 -13 -9 0.36 2.42 -3 -9 -13 2.28 2.30 -6 -14 -8 2.57 5.41 -6 -8 -14 3.43 3.19 -5 -14 -8 18.58 9.02 -5 -8 -14 9.62 4.45 -4 -8 -14 2.89 2.70 -7 -12 -11 21.62 5.21 -7 -11 -12 1.57 2.16 -6 -12 -11 6.67 3.10 -6 -11 -12 2.81 2.17 -5 -12 -11 -0.04 1.86 -5 -11 -12 1.57 1.71 -4 -12 -11 0.79 1.68 -4 -11 -12 2.29 2.28 -3 -12 -11 1.48 1.54 -3 -11 -12 2.15 1.88 -8 -13 -10 4.90 5.50 -7 -13 -10 8.70 6.43 -7 -10 -13 3.63 2.63 -6 -13 -10 -0.61 2.49 -6 -10 -13 3.24 2.42 -5 -13 -10 2.30 2.75 -5 -10 -13 4.89 2.49 -4 -13 -10 3.42 2.57 -4 -10 -13 0.50 1.89 -7 -14 -9 -2.58 4.83 -6 -14 -9 23.83 9.20 -6 -9 -14 6.60 5.11 -5 -9 -14 2.69 2.49 -7 -12 -12 -0.16 2.28 -6 -12 -12 2.30 2.72 -5 -12 -12 4.70 2.24 -7 -13 -11 10.04 4.28 -7 -11 -13 1.30 2.52 -6 -13 -11 8.12 3.69 -6 -11 -13 4.99 2.97 -5 -11 -13 1.72 2.40 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 43232 _shelx_res_file ; TITL 131202a1 in P-1 4.res created by SHELXL-2018/1 at 15:44:18 on 19-Jan-2019 CELL 0.71073 9.8038 11.3496 11.3496 69.430 65.912 65.912 ZERR 2.00 0.0126 0.0143 0.0143 0.014 0.018 0.018 LATT 1 SFAC C H N Cl Zn I UNIT 26 22 12 6 2 4 OMIT -1.00 50.10 L.S. 8 ACTA BOND FMAP 2 PLAN 20 size 0.18 0.15 0.11 dfix 2.84 0.02 cl1' cl2' cl2' cl3' cl3' cl1' dfix 1.72 0.01 c13' cl1' c13' cl2' c13' cl3' simu 0.01 0.02 2.9 c13 cl1 cl2 cl3 dfix 2.84 0.02 cl1 cl2 cl2 cl3 cl3 cl1 dfix 1.72 0.01 c13 cl1 c13 cl2 c13 cl3 eadp cl1 cl1' eadp cl2 cl2' eadp cl3 cl3' eadp c13 c13' FREE N1 N3 TEMP 25 WGHT 0.172000 FVAR 0.18660 0.76412 MOLE 1 ZN1 5 0.584057 1.360957 0.326981 11.00000 0.04108 0.04289 = 0.06292 -0.01784 -0.02771 -0.01052 PART 1 CL1 4 0.362165 0.138635 0.268811 21.00000 0.09930 0.10851 = 0.24907 -0.05392 -0.05494 -0.03372 CL2 4 0.110101 0.046028 0.346707 21.00000 0.09156 0.09936 = 0.23018 -0.03305 -0.04234 -0.03526 CL3 4 0.399617 -0.083481 0.180403 21.00000 0.14618 0.08806 = 0.18173 -0.05518 -0.07099 0.01420 PART 2 CL1' 4 0.339608 0.093156 0.374565 -21.00000 0.09930 0.10851 = 0.24907 -0.05392 -0.05494 -0.03372 CL2' 4 0.181160 -0.008415 0.289452 -21.00000 0.09156 0.09936 = 0.23018 -0.03305 -0.04234 -0.03526 CL3' 4 0.365751 0.157789 0.103551 -21.00000 0.14618 0.08806 = 0.18173 -0.05518 -0.07099 0.01420 PART 0 I1 6 0.502729 1.565250 0.155596 11.00000 0.07198 0.05351 = 0.06818 -0.00954 -0.04495 -0.00972 I2 6 0.386466 1.292403 0.539990 11.00000 0.04684 0.06243 = 0.07346 -0.01881 -0.01604 -0.01537 N1 3 0.992927 0.720233 0.193560 11.00000 0.03416 0.04193 = 0.06312 -0.01730 -0.02129 -0.00538 N2 3 1.032185 0.628702 0.128105 11.00000 0.04106 0.06347 = 0.06066 -0.03297 -0.00438 -0.02316 N3 3 0.972665 0.680602 0.028314 11.00000 0.10428 0.07555 = 0.05922 -0.01257 -0.02890 -0.05243 N4 3 0.896283 0.807225 0.024622 11.00000 0.11776 0.03778 = 0.10117 -0.00867 -0.06411 -0.03320 N5 3 0.764029 0.370469 0.365029 11.00000 0.02869 0.05612 = 0.05783 -0.01292 -0.01895 -0.02155 N6 3 0.698417 1.197019 0.245276 11.00000 0.04617 0.05012 = 0.06165 -0.01990 -0.02931 -0.01051 C1 1 0.903686 0.828089 0.132968 11.00000 0.04723 0.04592 = 0.04970 -0.02263 -0.01580 -0.01414 C2 1 1.107784 0.493474 0.170930 11.00000 0.02815 0.03734 = 0.08257 -0.03658 0.00333 -0.00972 AFIX 23 H2A 2 1.195411 0.484101 0.196510 11.00000 -1.20000 H2B 2 1.149015 0.449294 0.098640 11.00000 -1.20000 AFIX 0 C3 1 0.869634 0.416294 0.267997 11.00000 0.07015 0.03164 = 0.07071 -0.01768 -0.04118 -0.01237 AFIX 43 H3 2 0.862289 0.441904 0.182900 11.00000 -1.20000 AFIX 0 C4 1 0.995266 0.428580 0.287255 11.00000 0.01759 0.05955 = 0.05704 -0.03272 -0.01096 -0.00063 C5 1 1.008327 0.388728 0.410427 11.00000 0.02923 0.05638 = 0.09387 -0.04798 -0.02106 0.01079 AFIX 43 H5 2 1.092389 0.394268 0.424452 11.00000 -1.20000 AFIX 0 C6 1 0.901953 0.342470 0.509313 11.00000 0.07498 0.06140 = 0.04658 -0.03525 -0.01553 -0.00580 AFIX 43 H6 2 0.911978 0.314510 0.593672 11.00000 -1.20000 AFIX 0 C7 1 0.774963 0.333779 0.492492 11.00000 0.06781 0.03337 = 0.08323 -0.01390 -0.04316 -0.01101 AFIX 43 H7 2 0.698048 0.303990 0.564855 11.00000 -1.20000 AFIX 0 C8 1 0.708424 1.189551 0.127779 11.00000 0.08357 0.06356 = 0.05451 0.01033 -0.02541 -0.05079 AFIX 43 H8 2 0.667647 1.265823 0.070595 11.00000 -1.20000 AFIX 0 C9 1 0.777953 1.071135 0.089227 11.00000 0.06232 0.04045 = 0.06526 -0.01339 -0.03051 -0.01813 AFIX 43 H9 2 0.781346 1.070513 0.006349 11.00000 -1.20000 AFIX 0 C10 1 0.841518 0.955850 0.164411 11.00000 0.03520 0.02139 = 0.07243 -0.01914 -0.02714 0.01078 C11 1 0.836812 0.962065 0.286960 11.00000 0.08526 0.03827 = 0.06522 -0.01027 -0.05451 -0.00011 AFIX 43 H11 2 0.884030 0.887863 0.342255 11.00000 -1.20000 AFIX 0 C12 1 0.759868 1.081827 0.322303 11.00000 0.06632 0.05143 = 0.06234 -0.02166 -0.03427 -0.00941 AFIX 43 H12 2 0.749025 1.083913 0.406926 11.00000 -1.20000 PART 1 AFIX 0 C13 1 0.276955 0.066204 0.218811 21.00000 0.10682 0.08307 = 0.21800 -0.04341 -0.05298 -0.02349 AFIX 13 H13 2 0.246658 0.126195 0.140874 21.00000 -1.20000 PART 2 AFIX 0 C13' 1 0.247442 0.120057 0.262965 -21.00000 0.10682 0.08307 = 0.21800 -0.04341 -0.05298 -0.02349 AFIX 13 H13' 2 0.154749 0.198219 0.276621 -21.00000 -1.20000 PART 0 AFIX 0 HKLF 4 REM 131202a1 in P-1 REM R1 = 0.1308 for 2424 Fo > 4sig(Fo) and 0.1638 for all 3598 data REM 239 parameters refined using 48 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 2.403, deepest hole -1.890, 1-sigma level 0.381 Q1 1 0.2846 1.3187 0.5960 11.00000 0.05 2.40 Q2 1 0.3487 0.1806 0.1457 11.00000 0.05 1.96 Q3 1 0.4752 1.3810 0.3602 11.00000 0.05 1.88 Q4 1 0.3269 -0.0979 0.2043 11.00000 0.05 1.83 Q5 1 0.5870 1.4417 0.2824 11.00000 0.05 1.77 Q6 1 0.1537 0.0820 0.3641 11.00000 0.05 1.76 Q7 1 0.4737 1.3127 0.4386 11.00000 0.05 1.74 Q8 1 0.4951 1.6547 0.1001 11.00000 0.05 1.73 Q9 1 0.4952 1.2581 0.5013 11.00000 0.05 1.65 Q10 1 0.3934 1.5964 0.1958 11.00000 0.05 1.60 Q11 1 0.5925 1.5638 0.0670 11.00000 0.05 1.58 Q12 1 0.3751 1.3758 0.4982 11.00000 0.05 1.57 Q13 1 0.6141 1.5416 0.1199 11.00000 0.05 1.57 Q14 1 0.5021 1.4932 0.2010 11.00000 0.05 1.56 Q15 1 0.6916 1.3350 0.2613 11.00000 0.05 1.56 Q16 1 0.5903 1.2781 0.3600 11.00000 0.05 1.52 Q17 1 0.3968 1.2055 0.5947 11.00000 0.05 1.47 Q18 1 0.3796 1.4955 0.2790 11.00000 0.05 1.30 Q19 1 0.9417 0.4396 0.3771 11.00000 0.05 1.25 Q20 1 1.2868 0.3637 -0.0793 11.00000 0.05 1.23 ; _shelx_res_checksum 50701 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 Zn Zn1 0.5841(2) 1.3610(2) 0.3270(2) 0.0439(7) Uani d 1 . . Cl Cl1 0.3622(15) 0.1386(14) 0.269(2) 0.147(5) Uani d 0.764(11) A 1 Cl Cl2 0.1101(13) 0.0460(13) 0.3467(18) 0.142(5) Uani d 0.764(11) A 1 Cl Cl3 0.3996(17) -0.0835(12) 0.1804(15) 0.142(5) Uani d 0.764(11) A 1 Cl Cl1' 0.340(6) 0.093(5) 0.375(4) 0.147(5) Uani d 0.236(11) A 2 Cl Cl2' 0.181(5) -0.008(4) 0.289(5) 0.142(5) Uani d 0.236(11) A 2 Cl Cl3' 0.366(5) 0.158(3) 0.104(4) 0.142(5) Uani d 0.236(11) A 2 I I1 0.50273(18) 1.56525(14) 0.15560(15) 0.0610(6) Uani d 1 . . I I2 0.38647(17) 1.29240(15) 0.53999(15) 0.0613(6) Uani d 1 . . N N1 0.9929(17) 0.7202(15) 0.1936(16) 0.045(4) Uani d 1 . . N N2 1.0322(19) 0.6287(18) 0.1281(18) 0.051(4) Uani d 1 . . N N3 0.973(3) 0.681(2) 0.0283(19) 0.070(6) Uani d 1 . . N N4 0.896(3) 0.8072(18) 0.025(2) 0.074(6) Uani d 1 . . N N5 0.7640(17) 0.3705(16) 0.3650(15) 0.043(4) Uani d 1 . . N N6 0.6984(18) 1.1970(16) 0.2453(17) 0.048(4) Uani d 1 . . C C1 0.904(2) 0.8281(19) 0.1330(19) 0.044(4) Uani d 1 . . C C2 1.108(2) 0.4935(18) 0.171(2) 0.050(5) Uani d 1 . . H H2A 1.195411 0.484101 0.196510 0.060 Uiso calc 1 . . H H2B 1.149015 0.449294 0.098640 0.060 Uiso calc 1 . . C C3 0.870(3) 0.4163(18) 0.268(2) 0.050(5) Uani d 1 . . H H3 0.862289 0.441904 0.182900 0.060 Uiso calc 1 . . C C4 0.9953(19) 0.4286(19) 0.287(2) 0.043(4) Uani d 1 . . C C5 1.008(2) 0.389(2) 0.410(3) 0.058(6) Uani d 1 . . H H5 1.092389 0.394268 0.424452 0.070 Uiso calc 1 . . C C6 0.902(3) 0.342(2) 0.509(2) 0.061(6) Uani d 1 . . H H6 0.911978 0.314510 0.593672 0.073 Uiso calc 1 . . C C7 0.775(3) 0.3338(18) 0.492(2) 0.056(5) Uani d 1 . . H H7 0.698048 0.303990 0.564855 0.067 Uiso calc 1 . . C C8 0.708(3) 1.190(2) 0.128(2) 0.063(6) Uani d 1 . . H H8 0.667647 1.265823 0.070595 0.075 Uiso calc 1 . . C C9 0.778(2) 1.0711(19) 0.089(2) 0.051(5) Uani d 1 . . H H9 0.781346 1.070513 0.006349 0.061 Uiso calc 1 . . C C10 0.842(2) 0.9558(16) 0.164(2) 0.044(4) Uani d 1 . . C C11 0.837(3) 0.962(2) 0.287(2) 0.059(6) Uani d 1 . . H H11 0.884030 0.887863 0.342255 0.071 Uiso calc 1 . . C C12 0.760(3) 1.082(2) 0.322(2) 0.055(5) Uani d 1 . . H H12 0.749025 1.083913 0.406926 0.066 Uiso calc 1 . . C C13 0.2770(18) 0.0662(17) 0.219(2) 0.134(9) Uani d 0.764(11) A 1 H H13 0.246658 0.126195 0.140874 0.161 Uiso calc 0.764(11) A 1 C C13' 0.247(4) 0.120(4) 0.263(4) 0.134(9) Uani d 0.236(11) A 2 H H13' 0.154749 0.198219 0.276621 0.161 Uiso calc 0.236(11) A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zn1 0.0411(13) 0.0429(13) 0.0629(15) -0.0105(9) -0.0277(11) -0.0178(10) Cl1 0.099(7) 0.109(8) 0.249(13) -0.034(6) -0.055(9) -0.054(9) Cl2 0.092(8) 0.099(8) 0.230(12) -0.035(6) -0.042(8) -0.033(8) Cl3 0.146(9) 0.088(7) 0.182(11) 0.014(6) -0.071(8) -0.055(7) Cl1' 0.099(7) 0.109(8) 0.249(13) -0.034(6) -0.055(9) -0.054(9) Cl2' 0.092(8) 0.099(8) 0.230(12) -0.035(6) -0.042(8) -0.033(8) Cl3' 0.146(9) 0.088(7) 0.182(11) 0.014(6) -0.071(8) -0.055(7) I1 0.0720(11) 0.0535(9) 0.0682(10) -0.0097(7) -0.0450(8) -0.0095(7) I2 0.0468(9) 0.0624(10) 0.0735(11) -0.0154(6) -0.0160(7) -0.0188(7) N1 0.034(9) 0.042(9) 0.063(10) -0.005(6) -0.021(8) -0.017(7) N2 0.041(10) 0.063(11) 0.061(11) -0.023(8) -0.004(8) -0.033(9) N3 0.104(17) 0.076(15) 0.059(12) -0.052(13) -0.029(11) -0.013(10) N4 0.118(18) 0.038(11) 0.101(16) -0.033(11) -0.064(14) -0.009(10) N5 0.029(8) 0.056(10) 0.058(10) -0.022(7) -0.019(7) -0.013(8) N6 0.046(10) 0.050(10) 0.062(10) -0.011(7) -0.029(8) -0.020(8) C1 0.047(12) 0.046(11) 0.050(11) -0.014(8) -0.016(9) -0.023(9) C2 0.028(10) 0.037(10) 0.083(15) -0.010(7) 0.003(9) -0.037(10) C3 0.070(14) 0.032(10) 0.071(13) -0.012(9) -0.041(11) -0.018(9) C4 0.018(9) 0.060(12) 0.057(12) -0.001(7) -0.011(8) -0.033(9) C5 0.029(11) 0.056(13) 0.094(18) 0.011(9) -0.021(11) -0.048(12) C6 0.075(17) 0.061(14) 0.047(12) -0.006(11) -0.016(11) -0.035(10) C7 0.068(15) 0.033(11) 0.083(16) -0.011(9) -0.043(12) -0.014(10) C8 0.084(17) 0.064(14) 0.055(13) -0.051(13) -0.025(12) 0.010(11) C9 0.062(13) 0.040(11) 0.065(13) -0.018(9) -0.031(11) -0.013(9) C10 0.035(10) 0.021(9) 0.072(13) 0.011(7) -0.027(9) -0.019(8) C11 0.085(16) 0.038(11) 0.065(14) 0.000(10) -0.055(12) -0.010(9) C12 0.066(14) 0.051(13) 0.062(13) -0.009(10) -0.034(11) -0.022(10) C13 0.107(12) 0.083(12) 0.218(15) -0.023(11) -0.053(12) -0.043(12) C13' 0.107(12) 0.083(12) 0.218(15) -0.023(11) -0.053(12) -0.043(12) 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' N N 0.0061 0.0033 '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' Zn Zn 0.2839 1.4301 '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' 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 N5 Zn1 N6 1_565 . 99.7(6) ? N5 Zn1 I2 1_565 . 109.9(5) ? N6 Zn1 I2 . . 105.0(5) ? N5 Zn1 I1 1_565 . 108.5(4) ? N6 Zn1 I1 . . 110.4(5) ? I2 Zn1 I1 . . 121.28(12) ? N2 N1 C1 . . 104.6(17) ? N3 N2 N1 . . 110.0(18) ? N3 N2 C2 . . 125.7(18) ? N1 N2 C2 . . 123.7(19) ? N4 N3 N2 . . 109.5(18) ? N3 N4 C1 . . 104.3(19) ? C3 N5 C7 . . 118.7(16) ? C3 N5 Zn1 . 1_545 118.6(13) ? C7 N5 Zn1 . 1_545 122.6(12) ? C8 N6 C12 . . 115.7(18) ? C8 N6 Zn1 . . 127.0(15) ? C12 N6 Zn1 . . 117.2(14) ? N1 C1 N4 . . 111.2(17) ? N1 C1 C10 . . 124.7(18) ? N4 C1 C10 . . 123.5(19) ? N2 C2 C4 . . 111.0(15) ? N5 C3 C4 . . 121.8(19) ? C5 C4 C3 . . 119.3(19) ? C5 C4 C2 . . 121.5(19) ? C3 C4 C2 . . 119.1(19) ? C6 C5 C4 . . 119(2) ? C5 C6 C7 . . 122(2) ? C6 C7 N5 . . 119(2) ? N6 C8 C9 . . 121(2) ? C10 C9 C8 . . 124(2) ? C9 C10 C11 . . 116.1(17) ? C9 C10 C1 . . 126(2) ? C11 C10 C1 . . 118.1(17) ? C12 C11 C10 . . 117.3(18) ? N6 C12 C11 . . 126(2) ? Cl3 C13 Cl2 . . 110.1(11) ? Cl3 C13 Cl1 . . 112.9(11) ? Cl2 C13 Cl1 . . 107.0(10) ? Cl2' C13' Cl3' . . 112.6(14) ? Cl2' C13' Cl1' . . 112.4(14) ? Cl3' C13' Cl1' . . 110.7(14) ? 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 Zn1 N5 1_565 2.030(14) ? Zn1 N6 . 2.059(16) ? Zn1 I2 . 2.508(3) ? Zn1 I1 . 2.526(3) ? Cl1 C13 . 1.724(10) ? Cl2 C13 . 1.723(10) ? Cl3 C13 . 1.717(10) ? Cl1' C13' . 1.718(10) ? Cl2' C13' . 1.716(10) ? Cl3' C13' . 1.718(10) ? N1 N2 . 1.33(2) ? N1 C1 . 1.33(2) ? N2 N3 . 1.33(3) ? N2 C2 . 1.41(3) ? N3 N4 . 1.32(3) ? N4 C1 . 1.37(3) ? N5 C3 . 1.29(3) ? N5 C7 . 1.39(3) ? N6 C8 . 1.33(3) ? N6 C12 . 1.35(3) ? C1 C10 . 1.44(2) ? C2 C4 . 1.51(3) ? C3 C4 . 1.40(3) ? C4 C5 . 1.35(3) ? C5 C6 . 1.30(3) ? C6 C7 . 1.38(3) ? C8 C9 . 1.37(3) ? C9 C10 . 1.35(3) ? C10 C11 . 1.40(3) ? C11 C12 . 1.37(3) ? 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 _geom_hbond_publ_flag C6 H6 N1^iii^ 2_766 0.93 2.75 3.64(2) 160 yes C13 H13 N4^iv^ 2_665 0.98 2.57 3.45(3) 150 yes C13 Cl1 Cg1 . 1.714(9) 3.559(16) 4.799(16) 127 yes _cod_database_fobs_code 2022306