#------------------------------------------------------------------------------ #$Date: 2024-07-13 05:09:47 +0300 (Sat, 13 Jul 2024) $ #$Revision: 293408 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572128.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_1572128 loop_ _publ_author_name 'Ichimaru, Yoshimi' 'Sugiura, Kirara' 'Kato, Koichi' 'Kondo, Yuki' 'Kurihara, Masaaki' 'Jin, Wanchun' 'Imai, Masanori' 'Kurosaki, Hiromasa' _publ_section_title ; [1-(Anthracen-9-ylmethyl)-1,4,7,10-tetraazacyclododecane]chloridozinc(II) nitrate ; _journal_coeditor_code WM4217 _journal_issue 7 _journal_name_full IUCrData _journal_paper_doi 10.1107/S2414314624006655 _journal_volume 9 _journal_year 2024 _chemical_formula_iupac 'C23 H30 Cl N4 Zn +, N O3 -' _chemical_formula_moiety 'C23 H30 Cl N4 Zn +, N O3 -' _chemical_formula_sum 'C23 H30 Cl N5 O3 Zn' _chemical_formula_weight 525.34 _chemical_name_systematic ; [1-(Anthracen-9-ylmethyl)-1,4,7,10-tetraazacyclododecane]chloridozinc(II) nitrate ; _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 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _cell_angle_alpha 90 _cell_angle_beta 106.1570(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.90860(10) _cell_length_b 7.80880(10) _cell_length_c 19.5342(2) _cell_measurement_reflns_used 16543 _cell_measurement_temperature 92.95 _cell_measurement_theta_max 68.3220 _cell_measurement_theta_min 2.3550 _cell_volume 2330.83(4) _computing_cell_refinement ; CrysAlisPro (Rigaku OD, 2022) ; _computing_data_collection ; CrysAlisPro (Rigaku OD, 2022) ; _computing_data_reduction ; CrysAlisPro (Rigaku OD, 2022) ; _computing_molecular_graphics ; Olex2 (Dolomanov et al., 2009) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 92.95 _diffrn_detector_area_resol_mean 10.0 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku XtaLAB Synergy-i' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_unetI/netI 0.0184 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 21217 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 68.400 _diffrn_reflns_theta_min 2.892 _exptl_absorpt_coefficient_mu 2.813 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.61854 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2022) ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.497 _exptl_crystal_description plate _exptl_crystal_F_000 1096 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _refine_diff_density_max 1.653 _refine_diff_density_min -0.675 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 298 _refine_ls_number_reflns 4271 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0414 _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^)+(0.0537P)^2^+5.0389P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1093 _refine_ls_wR_factor_ref 0.1101 _reflns_number_gt 4097 _reflns_number_total 4271 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm4217.cif _cod_data_source_block I _cod_database_code 1572128 _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 0.439 _shelx_estimated_absorpt_t_max 0.729 _shelx_hkl_file ; 0 0 -1 0.07 0.07 0 0 -1 0.24 0.09 0 0 -1 0.17 0.08 0 0 -1 0.57 0.12 0 0 -1 0.74 0.11 0 0 -2 2169.12 42.09 0 0 -2 2220.82 42.09 0 0 -2 2129.42 42.12 0 0 -2 2238.80 42.09 0 0 2 2180.83 41.49 0 0 -2 2156.24 41.89 0 0 -3 0.60 0.27 0 0 -3 0.48 0.27 0 0 -3 -0.04 0.23 0 0 -3 1.07 0.33 0 0 -3 0.76 0.29 0 0 -3 0.74 0.24 0 0 -4 5826.81 112.11 0 0 -4 5695.27 112.21 0 0 -4 5970.75 112.19 0 0 -4 5968.92 112.44 0 0 -4 5688.44 112.25 0 0 -4 5902.96 111.76 0 0 -5 1.41 0.50 0 0 -5 0.45 0.35 0 0 -5 0.82 0.47 0 0 -5 0.07 0.33 0 0 -5 0.25 0.30 0 0 -6 652.47 15.66 0 0 -6 676.83 15.42 0 0 -6 678.30 15.61 0 0 -7 0.66 0.48 0 0 -7 0.31 0.53 0 0 -8 615.14 15.94 0 0 -9 1.07 0.80 0 0 9 1.94 0.65 0 0 -10 1892.12 41.96 0 0 -11 -0.61 0.92 0 0 -12 115.14 5.61 0 0 -12 110.97 5.87 0 0 -12 105.27 6.38 0 0 -12 118.03 6.03 0 0 -12 105.69 5.51 0 0 -12 99.40 5.89 0 0 -12 96.98 5.78 0 0 -12 117.96 6.11 0 0 -12 103.31 6.28 0 0 -12 95.92 6.04 0 0 -13 0.85 0.82 0 0 -13 0.21 0.80 0 0 -13 0.27 0.93 0 0 -13 1.48 0.81 0 0 -13 -0.23 0.66 0 0 -13 0.23 0.75 0 0 -13 -0.26 0.74 0 0 -13 0.52 1.05 0 0 -14 207.51 9.06 0 0 -14 176.63 9.34 0 0 -14 195.20 8.86 0 0 -14 181.41 8.06 0 0 -14 191.69 9.01 0 0 -14 169.40 8.59 0 0 -14 171.20 9.03 0 0 -14 162.39 8.98 0 0 -15 0.25 0.82 0 0 -15 1.89 1.42 0 0 -15 0.22 0.72 0 0 -15 0.27 0.78 0 0 -15 1.38 1.21 0 0 -15 -0.31 1.13 0 0 -15 -0.31 1.10 0 0 -16 386.82 13.83 0 0 -16 369.86 12.93 0 0 -16 357.10 14.69 0 0 -16 351.55 13.82 0 0 -16 353.01 13.83 0 0 -16 310.83 13.93 0 0 -16 336.07 14.34 0 0 -17 0.94 1.03 0 0 -17 1.71 1.33 0 0 -17 1.03 1.26 0 0 -17 0.81 1.18 0 0 -18 42.25 4.80 0 0 -18 53.30 4.41 0 0 -18 40.32 4.66 0 0 -19 -0.22 0.83 0 0 -19 -0.32 1.28 0 0 -19 0.32 1.62 0 0 -20 223.96 10.43 0 0 -20 209.08 10.13 0 0 -21 -0.24 0.88 0 0 -22 10.69 1.88 0 -1 0 0.19 0.14 0 1 0 0.77 0.25 0 -1 0 0.38 0.21 0 -1 1 304.04 6.47 0 1 -1 316.69 6.73 0 1 -1 315.66 6.25 0 -1 -1 312.73 6.35 0 1 -1 314.94 6.32 0 -1 -1 308.18 6.77 0 -1 1 281.52 6.63 0 1 -1 315.54 6.78 0 -1 -1 304.42 6.82 0 1 1 307.45 6.76 0 1 -1 309.52 7.00 0 -1 -1 305.56 7.04 0 1 -2 1089.53 21.97 0 1 -2 1107.78 21.86 0 1 -2 1074.99 21.49 0 -1 -2 1112.07 21.56 0 -1 -2 1113.43 21.70 0 1 -2 1073.54 21.87 0 -1 2 1095.10 21.75 0 -1 2 1021.61 21.13 0 -1 -2 1117.62 21.76 0 -1 -2 1103.62 22.22 0 1 -2 1085.99 22.06 0 1 -3 2124.74 40.82 0 1 -3 2146.10 41.57 0 -1 -3 2185.80 41.16 0 1 -3 2133.79 41.10 0 -1 -3 2155.33 41.36 0 -1 3 2101.46 40.42 0 -1 -3 2111.50 41.04 0 -1 -3 2084.52 41.53 0 1 -4 625.14 13.77 0 1 -4 615.01 12.71 0 -1 -4 652.56 13.43 0 1 -4 603.97 13.32 0 -1 -4 581.64 13.51 0 1 -4 606.53 13.51 0 -1 -4 631.05 13.10 0 -1 -4 605.52 13.80 0 -1 4 607.91 12.52 0 -1 -4 593.05 13.56 0 -1 -4 588.38 13.48 0 -1 -4 620.68 13.13 0 1 -5 377.21 9.56 0 1 -5 364.92 9.19 0 -1 -5 387.06 9.28 0 1 -5 385.55 9.41 0 -1 -5 377.26 9.54 0 1 -5 369.98 9.46 0 -1 -5 379.34 8.91 0 -1 -5 368.10 9.61 0 -1 -5 379.67 8.88 0 1 5 367.39 8.71 0 -1 -5 382.53 9.42 0 -1 -5 367.91 9.25 0 1 -6 218.34 6.80 0 1 -6 222.27 6.68 0 1 -6 212.24 6.69 0 -1 -6 214.24 6.79 0 -1 -6 225.34 6.16 0 -1 -6 214.93 6.86 0 -1 -6 216.26 6.34 0 -1 -6 221.10 6.56 0 1 -7 1963.55 40.86 0 1 -7 1953.64 40.59 0 -1 -7 1874.08 40.81 0 -1 -7 1834.90 40.62 0 -1 -7 1898.22 40.22 0 1 -8 998.27 22.75 0 -1 -8 961.92 22.98 0 1 -8 998.84 23.03 0 -1 -8 977.66 23.07 0 -1 -8 984.69 22.20 0 1 -9 332.73 10.90 0 -1 -9 362.28 11.17 0 -1 -9 349.05 11.11 0 -1 -10 9.27 1.65 0 -1 -10 7.49 1.54 0 1 -10 5.81 1.36 0 1 -11 1174.13 29.49 0 -1 -11 1198.42 29.69 0 -1 -11 1199.48 29.69 0 -1 -11 1236.94 29.23 0 1 -11 1135.87 29.24 0 -1 -11 1189.91 29.38 0 -1 -11 1222.64 28.32 0 1 -11 1270.49 29.13 0 -1 -11 1307.42 29.07 0 -1 -11 1200.10 29.41 0 -1 -11 1302.86 29.29 0 -1 -11 1206.48 28.33 0 -1 -11 1265.16 30.05 0 1 11 1229.69 28.13 0 -1 -11 1169.71 30.18 0 -1 -12 429.53 14.76 0 -1 -12 461.78 15.06 0 1 -12 439.15 14.78 0 1 -12 462.35 15.06 0 -1 -12 436.40 14.58 0 -1 -12 482.32 14.74 0 1 -12 481.52 14.71 0 -1 -12 416.72 14.40 0 1 -12 435.63 14.70 0 1 -12 503.35 14.56 0 1 -12 461.98 14.39 0 -1 -12 427.02 13.49 0 -1 -12 488.39 14.43 0 1 -12 489.46 13.79 0 -1 -12 474.28 14.43 0 -1 -12 466.61 13.91 0 1 12 435.70 13.25 0 1 -12 438.87 14.79 0 -1 -12 448.21 15.44 0 -1 -13 4.13 1.42 0 1 -13 7.32 1.84 0 -1 -13 3.98 1.52 0 -1 -13 10.17 1.83 0 1 -13 4.17 1.26 0 -1 -13 2.37 1.10 0 -1 -13 3.70 1.27 0 -1 -13 2.18 1.10 0 1 -13 2.74 1.33 0 1 -13 4.02 1.33 0 1 -13 4.57 1.40 0 -1 -13 3.30 1.34 0 -1 -13 3.64 1.19 0 1 -13 5.60 1.49 0 1 13 6.92 1.44 0 -1 -13 1.28 1.00 0 1 -13 4.64 1.60 0 1 -13 3.31 1.37 0 -1 -13 3.37 1.32 0 1 -14 161.82 8.23 0 1 -14 145.48 8.22 0 -1 -14 166.40 8.61 0 1 -14 171.28 7.70 0 -1 -14 164.88 7.70 0 -1 -14 169.90 8.12 0 1 -14 175.91 8.22 0 1 -14 140.33 8.16 0 -1 -14 149.25 8.77 0 -1 -14 182.15 8.50 0 -1 -14 156.23 7.52 0 1 -14 140.03 8.19 0 -1 -14 151.40 8.42 0 -1 -14 151.28 8.54 0 1 -14 142.41 8.18 0 -1 -14 155.60 8.28 0 1 -15 175.28 9.43 0 -1 -15 192.56 9.72 0 -1 -15 218.27 9.68 0 -1 -15 204.53 9.00 0 1 -15 218.47 9.59 0 1 -15 204.53 8.80 0 -1 -15 187.62 10.29 0 1 -15 200.75 10.07 0 -1 -15 210.86 9.08 0 1 -15 169.36 9.44 0 -1 -15 191.34 9.87 0 1 -15 172.25 9.57 0 -1 -15 203.57 10.29 0 -1 -15 203.42 9.91 0 -1 -16 43.74 4.59 0 1 -16 37.03 4.32 0 -1 -16 44.74 4.38 0 1 -16 45.14 4.38 0 1 -16 38.13 3.76 0 -1 -16 39.66 3.94 0 1 -16 41.56 4.51 0 -1 -16 37.84 4.64 0 -1 -16 37.67 3.76 0 -1 -16 40.30 4.61 0 1 -16 38.47 4.47 0 -1 -16 34.15 4.13 0 -1 -17 1.54 1.30 0 1 -17 1.27 1.05 0 -1 -17 4.58 1.61 0 1 -17 1.87 1.21 0 -1 -17 1.91 1.08 0 1 -17 0.47 1.05 0 -1 -17 1.79 1.62 0 1 -17 0.32 1.13 0 1 -17 0.99 1.40 0 -1 -17 2.99 1.73 0 -1 -17 4.05 1.59 0 -1 -18 7.38 2.18 0 1 -18 11.05 2.43 0 -1 -18 11.51 2.20 0 -1 -18 7.85 2.33 0 1 -18 11.43 2.62 0 -1 -18 9.95 2.45 0 1 -18 12.49 2.59 0 -1 -19 48.65 5.07 0 1 -19 50.55 4.90 0 -1 -19 44.39 4.67 0 1 -19 42.15 4.56 0 -1 -19 55.27 4.44 0 1 -19 52.78 4.89 0 -1 -20 27.95 3.61 0 -1 -20 26.39 3.56 0 1 -20 34.68 3.94 0 -1 -20 31.63 3.18 0 1 -20 38.08 3.94 0 -1 -21 60.12 4.80 0 -1 -21 53.34 4.46 0 1 -21 58.12 4.58 0 1 -21 55.77 4.35 0 1 -22 8.15 1.58 0 -1 -22 7.74 1.54 0 2 0 6367.49 123.99 0 -2 0 6550.67 124.14 0 2 0 6483.55 124.55 0 -2 0 6409.39 124.62 0 -2 0 6618.46 124.56 0 -2 -1 636.56 13.93 0 2 -1 659.04 13.94 0 2 -1 643.53 14.41 0 2 1 644.83 14.14 0 -2 -1 635.38 14.22 0 -2 1 652.68 14.06 0 -2 -1 636.27 14.43 0 -2 1 633.00 13.65 0 2 -1 648.15 13.44 0 2 -2 53.63 2.19 0 2 -2 48.68 2.45 0 -2 -2 52.45 2.34 0 -2 2 50.07 2.12 0 -2 -2 50.44 2.52 0 2 -2 52.57 2.24 0 -2 2 49.35 2.19 0 -2 -2 52.42 2.29 0 2 -2 51.08 2.28 0 2 -3 2356.10 46.75 0 2 -3 2384.05 47.27 0 -2 -3 2391.42 46.72 0 -2 -3 2379.65 47.43 0 2 -3 2395.56 46.73 0 2 -3 2302.00 46.86 0 -2 3 2292.68 46.54 0 2 -4 740.00 16.57 0 -2 4 710.61 16.08 0 -2 -4 728.47 16.10 0 2 -4 750.74 16.72 0 -2 -4 746.80 16.91 0 2 -4 731.18 16.34 0 2 -5 16.93 1.57 0 -2 5 15.95 1.40 0 -2 -5 16.73 1.62 0 -2 -5 19.65 1.49 0 2 -5 21.02 1.71 0 2 -5 15.99 1.35 0 2 -6 67.14 3.32 0 2 -6 56.47 3.23 0 2 -6 55.59 2.92 0 -2 6 63.05 2.98 0 -2 -6 60.17 3.45 0 -2 -6 61.65 3.31 0 -2 -6 55.46 3.11 0 2 6 56.71 2.89 0 2 -6 57.81 3.09 0 2 -7 25.82 2.15 0 2 -7 21.92 1.94 0 -2 -7 21.67 2.17 0 -2 -7 19.25 1.92 0 -2 -7 24.60 2.11 0 2 -7 21.89 1.94 0 2 -8 117.80 5.22 0 2 -8 117.03 5.14 0 -2 -8 112.01 5.48 0 -2 -8 107.28 4.98 0 -2 -8 110.48 4.97 0 2 -9 375.80 11.34 0 2 -9 342.94 10.96 0 -2 -9 379.76 12.09 0 -2 -9 355.01 11.01 0 -2 -10 156.69 7.48 0 2 -10 149.83 6.78 0 -2 -10 154.36 6.92 0 -2 -10 161.04 6.79 0 2 -10 148.92 6.73 0 -2 -11 282.21 9.97 0 2 -11 272.63 10.18 0 -2 -11 284.52 10.77 0 2 -11 280.21 10.29 0 2 -11 262.68 10.45 0 2 -11 257.32 10.40 0 2 -11 285.87 10.08 0 -2 -11 256.26 9.52 0 -2 -11 275.93 11.30 0 -2 -11 287.22 10.21 0 -2 -11 263.58 9.58 0 -2 -11 277.36 10.32 0 -2 -11 291.16 11.11 0 -2 -12 25.68 3.18 0 2 -12 24.49 3.06 0 2 -12 22.29 2.99 0 2 -12 30.15 3.11 0 -2 -12 24.47 2.73 0 -2 -12 26.45 3.46 0 -2 -12 24.82 2.90 0 -2 -12 22.76 2.63 0 -2 -12 25.14 2.94 0 2 12 24.64 2.67 0 -2 -12 29.28 3.45 0 -2 -13 164.50 8.55 0 2 -13 156.02 8.31 0 -2 -13 153.94 8.32 0 2 -13 145.10 8.07 0 -2 -13 153.84 7.42 0 2 -13 173.66 8.17 0 -2 -13 165.22 9.13 0 -2 -13 165.94 8.06 0 -2 -13 159.33 7.51 0 -2 -13 170.36 8.32 0 2 13 150.04 7.32 0 -2 13 165.09 7.40 0 -2 -13 171.04 8.96 0 -2 -14 391.21 14.57 0 2 -14 377.77 14.28 0 2 -14 342.53 13.93 0 -2 -14 390.50 14.64 0 2 -14 373.51 13.65 0 -2 -14 353.65 12.91 0 -2 -14 364.41 15.06 0 2 -14 402.40 14.40 0 -2 -14 374.67 12.94 0 -2 -14 435.16 14.42 0 -2 -14 383.49 14.09 0 2 14 363.24 12.74 0 -2 14 369.93 12.69 0 -2 -15 347.38 14.08 0 2 -15 349.71 13.98 0 -2 -15 337.31 13.98 0 2 -15 346.26 14.15 0 -2 -15 355.92 12.95 0 -2 -15 339.67 14.79 0 2 -15 378.71 14.25 0 -2 -15 355.32 12.77 0 2 15 346.31 12.56 0 -2 -15 373.89 14.20 0 2 -16 4.52 1.69 0 -2 -16 6.03 1.89 0 -2 -16 4.96 1.62 0 2 -16 12.29 2.31 0 2 -16 4.54 1.84 0 -2 -16 2.86 1.42 0 -2 -16 12.02 2.86 0 2 -16 5.97 1.85 0 -2 -16 7.73 2.16 0 -2 -17 160.02 8.14 0 -2 -17 153.18 7.75 0 -2 -17 144.71 8.65 0 2 -17 142.10 8.57 0 2 -17 128.00 7.98 0 -2 -17 134.99 8.90 0 -2 -18 584.07 17.36 0 2 -18 546.94 18.84 0 -2 -18 581.02 19.09 0 2 -18 524.62 18.09 0 -2 -18 539.95 19.49 0 -2 -19 188.24 10.08 0 -2 -19 206.35 9.96 0 2 -19 220.38 10.33 0 -2 -19 217.17 9.00 0 -2 -20 10.61 2.28 0 2 -20 10.82 2.17 0 -2 -20 14.96 2.16 0 2 -21 57.80 4.37 0 -2 -21 58.44 4.55 0 2 -22 119.03 5.61 0 -2 -22 115.17 5.71 0 -3 0 0.32 0.36 0 -3 0 0.19 0.41 0 3 0 0.10 0.41 0 -3 0 0.40 0.54 0 3 0 0.15 0.31 0 -3 1 1717.24 36.52 0 3 -1 1759.26 36.39 0 3 1 1689.02 36.00 0 -3 -1 1729.34 36.27 0 -3 -1 1763.76 36.43 0 3 1 1765.40 35.32 0 3 -1 1727.00 35.62 0 -3 -2 1284.50 27.75 0 3 -2 1259.46 27.67 0 -3 -2 1258.79 27.28 0 3 -2 1272.49 26.78 0 3 -2 1288.98 27.05 0 -3 -2 1242.24 26.87 0 -3 -3 967.03 21.50 0 -3 -3 968.14 22.18 0 3 -3 940.40 21.96 0 3 -3 974.31 21.23 0 3 -3 963.53 21.56 0 3 -4 94.44 4.43 0 -3 -4 90.84 4.46 0 -3 -4 97.15 4.10 0 3 -4 102.79 4.19 0 3 -5 20.13 2.01 0 -3 -5 18.56 1.96 0 3 -5 17.38 1.71 0 3 -6 84.94 4.41 0 -3 -6 86.57 4.44 0 -3 -6 84.01 4.47 0 3 7 128.18 5.55 0 -3 -7 138.86 6.14 0 3 -7 137.60 6.06 0 -3 -7 136.22 6.01 0 3 -7 143.93 5.92 0 -3 -7 145.16 6.61 0 3 -8 132.23 6.11 0 -3 -8 132.67 6.16 0 -3 -8 139.71 6.35 0 3 -8 138.70 6.12 0 -3 -8 141.48 6.80 0 3 -9 337.92 12.08 0 3 -9 366.99 11.61 0 -3 -9 376.94 12.70 0 -3 -9 364.56 12.09 0 3 -9 337.97 11.98 0 -3 -9 354.56 11.66 0 3 -9 359.03 12.20 0 -3 -9 342.87 11.68 0 3 -10 41.85 3.52 0 3 -10 41.51 3.89 0 3 -10 39.68 3.63 0 3 -10 38.28 3.63 0 -3 -10 45.12 4.15 0 3 -10 37.43 3.64 0 -3 -10 42.51 3.80 0 -3 -10 37.72 3.41 0 -3 -10 46.21 3.82 0 -3 -11 907.11 25.57 0 3 -11 927.43 23.93 0 3 -11 873.15 24.76 0 3 -11 884.99 24.23 0 3 -11 890.55 24.45 0 -3 -11 942.47 24.87 0 -3 -11 933.59 25.56 0 -3 -11 900.27 23.78 0 -3 -11 889.45 24.07 0 -3 -12 137.16 8.18 0 3 -12 125.21 7.55 0 3 -12 130.37 7.04 0 3 -12 129.67 7.48 0 3 -12 130.04 7.36 0 -3 -12 130.68 6.76 0 -3 -12 126.63 7.38 0 -3 -12 137.22 8.06 0 3 12 126.23 6.67 0 -3 -12 128.03 7.02 0 -3 -12 135.18 7.36 0 3 13 181.35 8.48 0 -3 -13 202.08 10.25 0 -3 -13 191.96 9.65 0 3 -13 188.33 9.78 0 3 -13 195.88 8.89 0 3 -13 180.37 9.24 0 -3 -13 183.81 8.56 0 -3 -13 205.86 9.58 0 -3 -13 200.31 10.39 0 -3 -14 3.06 1.48 0 3 -14 1.24 1.49 0 3 -14 1.78 1.25 0 -3 -14 2.20 1.32 0 -3 -14 2.64 1.26 0 3 -14 2.23 1.16 0 -3 -14 5.63 1.77 0 -3 -14 4.71 1.36 0 -3 -14 2.34 1.36 0 3 14 3.51 1.26 0 -3 -14 1.73 1.15 0 3 -15 420.68 16.13 0 -3 -15 423.92 16.27 0 3 -15 418.79 15.83 0 -3 -15 442.70 14.92 0 -3 -15 427.12 14.30 0 -3 -15 412.68 16.72 0 -3 -15 458.15 16.07 0 3 -16 1.26 1.33 0 -3 -16 1.63 1.43 0 -3 -16 1.00 1.06 0 -3 -16 1.19 1.25 0 -3 -16 0.23 0.89 0 3 -16 2.88 1.40 0 -3 -16 0.72 1.19 0 3 -17 27.17 3.67 0 -3 -17 34.07 4.09 0 -3 -17 28.93 3.44 0 -3 -17 27.05 3.14 0 3 -17 34.60 4.12 0 -3 -17 28.30 4.01 0 -3 -18 -0.29 1.18 0 3 -18 1.44 1.39 0 -3 -18 0.62 0.72 0 -3 -18 0.32 1.39 0 3 -18 0.56 1.04 0 -3 -19 49.99 4.53 0 3 -19 50.75 4.52 0 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-12 28.91 3.21 17 2 -12 27.58 2.90 17 2 -12 26.23 2.94 -17 -2 11 15.73 2.09 17 2 -11 14.22 2.18 17 2 -11 14.12 2.29 -17 -2 10 285.25 9.90 17 2 -10 255.60 10.44 17 2 -10 258.48 10.31 17 -2 -9 84.22 5.51 -17 -2 9 88.77 5.20 17 2 -9 87.54 5.75 17 2 -9 73.90 5.20 17 -2 -8 23.70 3.04 -17 -2 8 25.82 2.90 17 2 -8 28.12 3.29 17 2 -8 24.96 3.09 17 -2 -7 127.18 7.03 -17 -2 7 137.52 6.77 17 2 -7 124.43 7.08 17 2 -7 126.29 7.06 17 -2 -6 53.33 4.53 -17 -2 6 69.99 4.72 17 2 -6 63.38 4.97 17 -2 -5 411.28 14.00 -17 -2 5 432.98 13.62 17 2 -5 410.95 14.23 17 -2 -4 18.10 2.67 -17 -2 4 27.57 2.93 -17 -2 4 30.03 3.12 -17 2 4 22.98 2.78 17 2 -4 29.51 3.32 17 -2 -3 7.05 1.66 -17 -2 3 7.53 1.70 -17 -2 3 6.19 1.45 -17 2 3 6.12 1.68 17 2 -3 4.69 1.46 -17 -2 2 58.86 4.33 -17 2 2 48.59 4.05 17 -2 -2 47.55 3.96 -17 -2 1 136.74 6.72 -17 2 1 126.55 6.64 17 -2 -1 131.05 6.55 -17 -2 0 63.88 4.38 -17 2 0 63.88 4.48 17 -2 0 56.66 4.10 -17 -2 -1 81.01 4.81 -17 2 -1 75.08 4.75 17 -2 1 71.09 4.45 -17 -2 -2 11.60 1.79 17 -2 2 8.82 1.52 -17 2 -2 7.58 1.49 -17 -2 -2 11.77 1.75 -17 -2 -3 83.48 4.37 -17 2 -3 80.24 4.40 -17 2 -3 83.60 4.57 17 3 -13 17.25 2.07 17 -3 -13 11.35 1.74 17 3 -12 87.58 4.96 17 -3 -12 81.64 4.87 -17 -3 12 92.64 4.46 -17 -3 11 205.11 7.53 17 3 -11 187.43 8.05 17 -3 -11 191.22 8.10 17 -3 -11 211.13 8.40 -17 -3 10 11.19 1.73 17 -3 -10 7.52 1.61 17 3 -10 10.86 1.97 -17 -3 9 68.59 4.28 17 -3 -9 56.18 4.30 17 3 -9 62.97 4.55 -17 -3 8 97.30 5.24 17 -3 -8 88.47 5.55 17 3 -8 84.14 5.42 -17 -3 7 393.87 12.15 17 -3 -7 361.64 12.65 17 3 -7 361.17 12.66 -17 -3 6 1.71 0.98 17 -3 -6 0.64 1.17 17 3 -6 0.21 1.02 -17 -3 5 12.34 1.87 17 -3 -5 9.88 2.00 17 3 -5 7.75 1.76 -17 -3 4 44.69 3.45 -17 -3 4 47.41 3.69 17 -3 -4 45.39 3.90 17 3 -4 44.46 3.83 -17 -3 3 220.18 8.39 17 -3 -3 192.85 8.36 17 3 -3 198.59 8.54 -17 -3 2 35.96 3.23 -17 3 2 35.24 3.27 17 -3 -2 38.67 3.44 17 3 -2 37.04 3.34 -17 -3 1 1.01 0.79 17 -3 -1 1.07 0.86 17 -3 -1 1.13 0.85 17 3 -1 0.35 0.77 -17 -3 0 7.11 1.55 17 -3 0 8.64 1.56 17 -3 0 6.53 1.50 17 3 0 6.02 1.38 17 -3 1 185.80 7.38 17 -3 1 198.83 7.87 17 3 1 182.37 7.26 -17 -4 9 2.41 0.85 17 -4 -9 1.61 0.92 17 4 -9 0.76 0.75 -17 -4 8 4.08 1.09 17 -4 -8 4.00 1.17 17 4 -8 2.51 0.95 -17 -4 7 6.34 1.26 17 -4 -7 6.12 1.52 17 4 -7 6.07 1.34 -17 -4 6 100.34 4.69 17 -4 -6 85.68 4.97 -17 4 6 90.87 4.57 17 4 -6 87.15 4.83 -17 -4 5 313.04 9.32 17 -4 -5 289.04 10.08 17 4 -5 280.07 9.77 -17 4 5 311.29 9.58 17 -4 -4 4.11 1.28 -17 4 4 4.16 1.10 17 4 -4 4.43 1.12 -17 -4 3 56.41 3.52 17 -4 -3 48.02 3.53 -17 4 3 54.02 3.44 17 4 -3 51.10 3.49 17 -4 -2 148.33 6.37 -17 -4 2 166.36 6.37 18 0 -13 -0.34 0.73 18 0 -12 7.74 1.56 18 0 -11 0.20 0.83 -18 0 10 3.79 1.14 18 0 -10 4.56 1.43 -18 0 9 -1.15 1.19 18 0 -9 1.71 1.12 -18 0 8 86.46 4.98 18 0 -8 79.37 5.31 -18 0 7 -0.18 0.76 18 0 -7 0.22 1.02 -18 0 6 123.99 6.27 -18 0 5 0.91 0.85 -18 0 4 26.40 2.78 -18 0 4 22.43 2.64 -18 0 3 -1.19 1.25 -18 0 3 -0.18 1.03 -18 0 2 88.56 5.16 -18 0 2 97.94 5.12 -18 0 1 0.17 0.72 -18 0 1 0.18 0.65 -18 0 0 311.11 10.31 -18 0 0 306.83 10.33 -18 0 -1 0.15 0.52 -18 0 -1 0.15 0.56 18 -1 -13 51.85 3.56 18 1 -13 50.54 3.56 18 -1 -13 48.64 3.47 18 -1 -12 5.34 1.30 18 1 -12 4.65 1.28 18 -1 -12 4.72 1.25 18 -1 -11 64.98 4.39 18 1 -11 69.45 4.60 -18 -1 10 1.97 0.94 18 -1 -10 1.33 0.89 18 1 -10 1.76 1.07 -18 1 9 10.97 1.71 -18 -1 9 13.03 1.87 18 -1 -9 16.42 2.36 18 1 -9 17.24 2.46 -18 -1 8 68.82 4.37 -18 1 8 59.35 4.01 18 -1 -8 61.18 4.55 18 1 -8 58.29 4.46 -18 -1 7 102.42 5.42 -18 1 7 89.65 5.11 18 -1 -7 90.28 5.55 18 1 -7 82.70 5.39 -18 -1 6 14.06 2.03 -18 1 6 10.28 1.83 18 -1 -6 8.69 1.84 -18 -1 5 209.05 8.20 -18 1 5 191.59 7.98 -18 -1 4 150.51 6.64 -18 -1 4 142.32 6.51 -18 1 4 132.72 6.39 -18 -1 3 23.15 2.51 -18 -1 3 25.49 2.66 -18 1 3 18.46 2.35 -18 -1 2 21.08 2.44 -18 1 2 20.51 2.42 -18 -1 1 97.06 5.18 -18 1 1 97.41 5.23 -18 -1 0 80.82 4.70 -18 -1 0 97.56 4.98 -18 1 0 90.31 4.92 -18 -1 -1 1.01 0.65 -18 -1 -1 0.80 0.70 -18 1 -1 -0.14 0.55 -18 -1 -1 0.84 0.67 18 -2 -12 58.46 3.83 -18 -2 11 29.67 2.48 18 -2 -11 27.36 2.74 18 2 -11 29.95 2.70 -18 -2 10 24.52 2.36 18 2 -10 28.09 2.71 -18 -2 9 82.28 4.51 18 2 -9 79.05 4.70 -18 -2 8 33.98 2.92 18 2 -8 32.08 3.01 -18 -2 7 4.27 1.21 18 2 -7 2.73 1.23 18 2 -7 2.86 1.01 -18 -2 6 1.57 0.86 18 2 -6 -0.17 1.16 18 2 -6 1.61 0.94 -18 -2 5 33.97 2.90 18 2 -5 27.91 2.81 18 2 -5 25.77 2.74 -18 -2 4 4.24 1.12 18 2 -4 3.78 1.14 -18 2 3 1.27 0.76 -18 -2 3 0.77 0.74 18 2 -3 0.17 0.61 -18 -2 2 0.76 0.66 18 2 -2 1.25 0.80 -18 -2 1 56.18 3.61 -18 2 1 53.00 3.57 -18 -2 1 50.11 3.45 -18 -2 0 68.07 3.84 -18 2 0 58.80 3.69 18 3 -9 4.32 1.13 -18 -3 9 4.26 1.02 18 3 -8 39.39 3.11 -18 -3 8 44.65 3.04 18 3 -7 213.86 8.03 18 -3 -7 211.93 7.93 18 3 -6 15.94 2.00 18 -3 -6 18.38 2.21 -18 -3 6 18.45 1.97 18 3 -5 4.18 1.13 18 -3 -5 3.39 1.17 18 3 -4 101.87 5.03 19 0 -8 210.03 7.95 -19 0 8 217.15 7.49 -19 0 7 0.93 0.68 19 0 -6 18.41 2.25 -19 0 6 20.05 2.09 19 0 -5 -0.75 1.07 -19 0 5 -0.39 0.92 19 0 -4 71.48 4.17 -19 -1 8 31.24 2.54 -19 -1 7 1.02 0.68 19 1 -6 117.01 5.48 -19 -1 6 125.65 5.34 0 0 0 0.00 0.00 TITL atcycleneZn_autored in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 15.908644 7.808752 19.534188 90.0000 106.1567 90.0000 ZERR 10.00 0.000134 0.000052 0.000155 0.0000 0.0009 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O UNIT 110.00 100.00 10.00 10.00 SIZE 0.12 0.25 0.35 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 93240 _shelx_res_file ; TITL atcyclenezn_autored_a.res in P2(1)/c atcyclenezn_autored.res created by SHELXL-2019/3 at 10:32:12 on 17-Jun-2024 REM Old TITL atcyclenezn_autored_a.res in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.193, Rweak 0.007, Alpha 0.030 REM 1.138 for 346 systematic absences, Orientation as input REM Formula found by SHELXT: C23 N5 O4 Br CELL 1.54184 15.9086 7.8088 19.5342 90 106.157 90 ZERR 4 0.0001 0.0001 0.0002 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl N O Zn UNIT 92 120 4 20 12 4 L.S. 4 PLAN 1 SIZE 0.12 0.25 0.35 TEMP -180.2 CONF list 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.053700 5.038900 FVAR 0.44499 ZN1 6 0.387311 0.456594 0.359226 11.00000 0.01667 0.01153 = 0.02232 0.00115 0.00709 -0.00095 CL1 3 0.489087 0.663485 0.389265 11.00000 0.02818 0.02167 = 0.02847 0.00030 0.00610 -0.00341 O1 5 0.386177 0.662748 0.164110 11.00000 0.02273 0.03078 = 0.01921 -0.00078 0.00229 -0.00424 O2 5 0.357991 0.679750 0.048908 11.00000 0.03080 0.03389 = 0.02072 0.00649 0.00783 -0.00044 N1 4 0.247370 0.575130 0.326272 11.00000 0.01665 0.01254 = 0.02418 0.00220 0.00532 0.00071 N2 4 0.344281 0.381539 0.252617 11.00000 0.02263 0.01880 = 0.02333 0.00018 0.00918 -0.00270 AFIX 13 H2 2 0.354759 0.475940 0.221385 11.00000 -1.20000 AFIX 0 N3 4 0.442975 0.206903 0.373405 11.00000 0.01748 0.01713 = 0.03288 -0.00251 0.00259 0.00242 AFIX 13 H3 2 0.507715 0.216524 0.381655 11.00000 -1.20000 AFIX 0 O3 5 0.275922 0.525769 0.096799 11.00000 0.02922 0.06659 = 0.02791 0.00315 0.00171 -0.02458 N4 4 0.346139 0.389697 0.449432 11.00000 0.02452 0.02164 = 0.02439 0.00469 0.00787 0.00234 AFIX 13 H4 2 0.393328 0.423402 0.492937 11.00000 -1.20000 AFIX 0 N5 4 0.339656 0.622526 0.102713 11.00000 0.01950 0.02421 = 0.02292 0.00046 0.00523 0.00110 C1 1 0.182908 0.882348 0.301900 11.00000 0.01611 0.01058 = 0.02587 -0.00075 0.00430 -0.00265 C2 1 0.134916 0.948698 0.347345 11.00000 0.01443 0.01383 = 0.02526 -0.00154 0.00330 -0.00241 C7 1 0.061985 1.061984 0.318474 11.00000 0.01536 0.01380 = 0.02719 -0.00193 0.00271 -0.00214 C17 1 0.249310 0.350272 0.237848 11.00000 0.02238 0.01628 = 0.02461 0.00128 0.00555 -0.00228 AFIX 23 H17A 2 0.238613 0.257067 0.268744 11.00000 -1.20000 H17B 2 0.224518 0.315513 0.187516 11.00000 -1.20000 AFIX 0 C15 1 0.261338 0.764507 0.331428 11.00000 0.01516 0.01230 = 0.02459 0.00151 0.00557 0.00032 AFIX 23 H15A 2 0.306094 0.792998 0.306741 11.00000 -1.20000 H15B 2 0.286579 0.793243 0.382389 11.00000 -1.20000 AFIX 0 C8 1 0.038662 1.104641 0.246728 11.00000 0.01646 0.01325 = 0.03091 0.00145 0.00289 0.00041 AFIX 43 H8 2 -0.010901 1.175629 0.227958 11.00000 -1.20000 AFIX 0 C9 1 0.086445 1.045491 0.201663 11.00000 0.01902 0.01366 = 0.02668 0.00261 0.00300 -0.00246 C14 1 0.161581 0.937234 0.229779 11.00000 0.01954 0.01094 = 0.02684 -0.00047 0.00599 -0.00315 C6 1 0.015627 1.133539 0.365093 11.00000 0.01761 0.01729 = 0.03427 -0.00369 0.00558 0.00124 AFIX 43 H6 2 -0.033418 1.205501 0.345867 11.00000 -1.20000 AFIX 0 C16 1 0.206436 0.513302 0.252383 11.00000 0.02235 0.01644 = 0.02770 0.00101 -0.00019 0.00039 AFIX 23 H16A 2 0.212198 0.602408 0.217920 11.00000 -1.20000 H16B 2 0.143295 0.492520 0.245818 11.00000 -1.20000 AFIX 0 C10 1 0.062878 1.095159 0.128066 11.00000 0.02577 0.02232 = 0.03089 0.00770 0.00474 0.00046 AFIX 43 H10 2 0.012570 1.164427 0.109607 11.00000 -1.20000 AFIX 0 C13 1 0.212877 0.896135 0.181986 11.00000 0.02889 0.01529 = 0.02996 0.00361 0.01110 0.00287 AFIX 43 H13 2 0.265276 0.832090 0.199311 11.00000 -1.20000 AFIX 0 C3 1 0.157660 0.917957 0.422584 11.00000 0.01566 0.02262 = 0.02493 -0.00061 0.00219 0.00099 AFIX 43 H3A 2 0.205360 0.844130 0.443490 11.00000 -1.20000 AFIX 0 C5 1 0.040216 1.100771 0.435431 11.00000 0.02078 0.02766 = 0.03237 -0.00858 0.00835 0.00110 AFIX 43 H5 2 0.009087 1.150559 0.465472 11.00000 -1.20000 AFIX 0 C19 1 0.405748 0.110500 0.307217 11.00000 0.02159 0.01840 = 0.03631 -0.00662 0.00664 0.00235 AFIX 23 H19A 2 0.348153 0.062604 0.307287 11.00000 -1.20000 H19B 2 0.444945 0.014239 0.303947 11.00000 -1.20000 AFIX 0 C4 1 0.112874 0.991507 0.464887 11.00000 0.02155 0.03084 = 0.02438 -0.00300 0.00322 0.00041 AFIX 43 H4A 2 0.130287 0.969705 0.514699 11.00000 -1.20000 AFIX 0 C20 1 0.425170 0.130097 0.437124 11.00000 0.03311 0.01730 = 0.02970 0.00329 -0.00118 0.00341 AFIX 23 H20A 2 0.474231 0.155658 0.479727 11.00000 -1.20000 H20B 2 0.420519 0.004167 0.431476 11.00000 -1.20000 AFIX 0 C21 1 0.340518 0.201017 0.447465 11.00000 0.03032 0.02280 = 0.02852 0.00789 0.00623 -0.00334 AFIX 23 H21A 2 0.290232 0.163987 0.407747 11.00000 -1.20000 H21B 2 0.331815 0.157511 0.492607 11.00000 -1.20000 AFIX 0 C18 1 0.395188 0.228296 0.244058 11.00000 0.02617 0.02632 = 0.03274 -0.00809 0.01508 -0.00184 AFIX 23 H18A 2 0.453501 0.263582 0.240278 11.00000 -1.20000 H18B 2 0.364569 0.167201 0.199724 11.00000 -1.20000 AFIX 0 C22 1 0.265061 0.480471 0.450827 11.00000 0.02948 0.02200 = 0.02839 0.00088 0.01456 -0.00029 AFIX 23 H22A 2 0.280205 0.594958 0.472524 11.00000 -1.20000 H22B 2 0.235127 0.415636 0.480764 11.00000 -1.20000 AFIX 0 C23 1 0.203800 0.500638 0.376701 11.00000 0.01935 0.01880 = 0.03558 0.00349 0.01376 -0.00014 AFIX 23 H23A 2 0.179688 0.387098 0.358880 11.00000 -1.20000 H23B 2 0.154274 0.575060 0.378989 11.00000 -1.20000 AFIX 0 C12 1 0.188468 0.946351 0.112810 11.00000 0.04135 0.02601 = 0.03205 0.00508 0.01775 0.00365 AFIX 43 H12 2 0.223574 0.915233 0.082604 11.00000 -1.20000 AFIX 0 C11 1 0.111150 1.044937 0.084512 11.00000 0.04151 0.02968 = 0.02602 0.00918 0.00835 0.00246 AFIX 43 H11 2 0.093660 1.075128 0.035468 11.00000 -1.20000 AFIX 0 HKLF 4 REM atcyclenezn_autored_a.res in P2(1)/c REM wR2 = 0.1101, GooF = S = 1.050, Restrained GooF = 1.050 for all data REM R1 = 0.0414 for 4097 Fo > 4sig(Fo) and 0.0427 for all 4271 data REM 298 parameters refined using 0 restraints END WGHT 0.0524 5.2892 REM Highest difference peak 1.653, deepest hole -0.675, 1-sigma level 0.079 Q1 1 0.4488 0.6683 0.3381 11.00000 0.05 1.65 ; _shelx_res_checksum 38711 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 Zn Zn1 0.38731(2) 0.45659(4) 0.35923(2) 0.01650(12) Uani d 1 . . Cl Cl1 0.48909(4) 0.66348(8) 0.38926(4) 0.02646(17) Uani d 1 . . O O1 0.38618(12) 0.6627(3) 0.16411(10) 0.0250(4) Uani d 1 . . O O2 0.35799(13) 0.6797(3) 0.04891(10) 0.0283(4) Uani d 1 . . N N1 0.24737(14) 0.5751(3) 0.32627(12) 0.0179(4) Uani d 1 . . N N2 0.34428(15) 0.3815(3) 0.25262(12) 0.0210(5) Uani d 1 . . H H2 0.354759 0.475940 0.221385 0.025 Uiso calc 1 . . N N3 0.44297(14) 0.2069(3) 0.37340(13) 0.0234(5) Uani d 1 . . H H3 0.507715 0.216524 0.381655 0.028 Uiso calc 1 . . O O3 0.27592(15) 0.5258(4) 0.09680(12) 0.0425(6) Uani d 1 . . N N4 0.34614(15) 0.3897(3) 0.44943(12) 0.0233(5) Uani d 1 . . H H4 0.393328 0.423402 0.492937 0.028 Uiso calc 1 . . N N5 0.33966(14) 0.6225(3) 0.10271(12) 0.0223(5) Uani d 1 . . C C1 0.18291(16) 0.8823(3) 0.30190(14) 0.0178(5) Uani d 1 . . C C2 0.13492(16) 0.9487(3) 0.34735(14) 0.0183(5) Uani d 1 . . C C7 0.06198(17) 1.0620(3) 0.31847(15) 0.0194(5) Uani d 1 . . C C17 0.24931(17) 0.3503(3) 0.23785(15) 0.0213(5) Uani d 1 . . H H17A 0.238613 0.257067 0.268744 0.026 Uiso calc 1 . . H H17B 0.224518 0.315513 0.187516 0.026 Uiso calc 1 . . C C15 0.26134(16) 0.7645(3) 0.33143(14) 0.0173(5) Uani d 1 . . H H15A 0.306094 0.792998 0.306741 0.021 Uiso calc 1 . . H H15B 0.286579 0.793243 0.382389 0.021 Uiso calc 1 . . C C8 0.03866(17) 1.1046(3) 0.24673(15) 0.0209(5) Uani d 1 . . H H8 -0.010901 1.175629 0.227958 0.025 Uiso calc 1 . . C C9 0.08644(17) 1.0455(3) 0.20166(15) 0.0205(5) Uani d 1 . . C C14 0.16158(17) 0.9372(3) 0.22978(14) 0.0192(5) Uani d 1 . . C C6 0.01563(17) 1.1335(3) 0.36509(15) 0.0234(6) Uani d 1 . . H H6 -0.033418 1.205501 0.345867 0.028 Uiso calc 1 . . C C16 0.20644(18) 0.5133(4) 0.25238(15) 0.0236(6) Uani d 1 . . H H16A 0.212198 0.602408 0.217920 0.028 Uiso calc 1 . . H H16B 0.143295 0.492520 0.245818 0.028 Uiso calc 1 . . C C10 0.06288(19) 1.0952(4) 0.12807(15) 0.0270(6) Uani d 1 . . H H10 0.012570 1.164427 0.109607 0.032 Uiso calc 1 . . C C13 0.21288(19) 0.8961(3) 0.18199(15) 0.0241(6) Uani d 1 . . H H13 0.265276 0.832090 0.199311 0.029 Uiso calc 1 . . C C3 0.15766(17) 0.9180(4) 0.42258(14) 0.0218(5) Uani d 1 . . H H3A 0.205360 0.844130 0.443490 0.026 Uiso calc 1 . . C C5 0.04022(18) 1.1008(4) 0.43543(16) 0.0267(6) Uani d 1 . . H H5 0.009087 1.150559 0.465472 0.032 Uiso calc 1 . . C C19 0.40575(18) 0.1105(4) 0.30722(16) 0.0257(6) Uani d 1 . . H H19A 0.348153 0.062604 0.307287 0.031 Uiso calc 1 . . H H19B 0.444945 0.014239 0.303947 0.031 Uiso calc 1 . . C C4 0.11287(18) 0.9915(4) 0.46489(15) 0.0262(6) Uani d 1 . . H H4A 0.130287 0.969705 0.514699 0.031 Uiso calc 1 . . C C20 0.4252(2) 0.1301(4) 0.43712(16) 0.0287(6) Uani d 1 . . H H20A 0.474231 0.155658 0.479727 0.034 Uiso calc 1 . . H H20B 0.420519 0.004167 0.431476 0.034 Uiso calc 1 . . C C21 0.34052(19) 0.2010(4) 0.44747(16) 0.0276(6) Uani d 1 . . H H21A 0.290232 0.163987 0.407747 0.033 Uiso calc 1 . . H H21B 0.331815 0.157511 0.492607 0.033 Uiso calc 1 . . C C18 0.39519(19) 0.2283(4) 0.24406(16) 0.0270(6) Uani d 1 . . H H18A 0.453501 0.263582 0.240278 0.032 Uiso calc 1 . . H H18B 0.364569 0.167201 0.199724 0.032 Uiso calc 1 . . C C22 0.26506(19) 0.4805(4) 0.45083(15) 0.0253(6) Uani d 1 . . H H22A 0.280205 0.594958 0.472524 0.030 Uiso calc 1 . . H H22B 0.235127 0.415636 0.480764 0.030 Uiso calc 1 . . C C23 0.20380(17) 0.5006(4) 0.37670(16) 0.0233(6) Uani d 1 . . H H23A 0.179688 0.387098 0.358880 0.028 Uiso calc 1 . . H H23B 0.154274 0.575060 0.378989 0.028 Uiso calc 1 . . C C12 0.1885(2) 0.9464(4) 0.11281(17) 0.0316(7) Uani d 1 . . H H12 0.223574 0.915233 0.082604 0.038 Uiso calc 1 . . C C11 0.1111(2) 1.0449(4) 0.08451(17) 0.0326(7) Uani d 1 . . H H11 0.093660 1.075128 0.035468 0.039 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 Zn1 0.01667(19) 0.01153(19) 0.0223(2) -0.00095(12) 0.00709(14) 0.00115(12) Cl1 0.0282(3) 0.0217(3) 0.0285(3) -0.0034(3) 0.0061(3) 0.0003(3) O1 0.0227(9) 0.0308(11) 0.0192(9) -0.0042(8) 0.0023(8) -0.0008(8) O2 0.0308(11) 0.0339(11) 0.0207(10) -0.0004(9) 0.0078(8) 0.0065(8) N1 0.0166(10) 0.0125(10) 0.0242(11) 0.0007(8) 0.0053(9) 0.0022(9) N2 0.0226(11) 0.0188(11) 0.0233(11) -0.0027(9) 0.0092(9) 0.0002(9) N3 0.0175(11) 0.0171(11) 0.0329(13) 0.0024(9) 0.0026(9) -0.0025(10) O3 0.0292(12) 0.0666(17) 0.0279(11) -0.0246(11) 0.0017(9) 0.0031(11) N4 0.0245(12) 0.0216(12) 0.0244(12) 0.0023(10) 0.0079(9) 0.0047(9) N5 0.0195(11) 0.0242(12) 0.0229(12) 0.0011(9) 0.0052(9) 0.0005(9) C1 0.0161(12) 0.0106(11) 0.0259(13) -0.0026(9) 0.0043(10) -0.0008(10) C2 0.0144(12) 0.0138(12) 0.0253(13) -0.0024(9) 0.0033(10) -0.0015(10) C7 0.0154(12) 0.0138(12) 0.0272(14) -0.0021(10) 0.0027(10) -0.0019(10) C17 0.0224(13) 0.0163(13) 0.0246(13) -0.0023(10) 0.0055(11) 0.0013(10) C15 0.0152(11) 0.0123(12) 0.0246(13) 0.0003(9) 0.0056(10) 0.0015(10) C8 0.0165(12) 0.0133(12) 0.0309(14) 0.0004(10) 0.0029(10) 0.0015(11) C9 0.0190(13) 0.0137(12) 0.0267(14) -0.0025(10) 0.0030(11) 0.0026(10) C14 0.0195(12) 0.0109(11) 0.0268(14) -0.0032(10) 0.0060(11) -0.0005(10) C6 0.0176(12) 0.0173(13) 0.0343(15) 0.0012(10) 0.0056(11) -0.0037(11) C16 0.0223(13) 0.0164(13) 0.0277(14) 0.0004(11) -0.0002(11) 0.0010(11) C10 0.0258(14) 0.0223(14) 0.0309(15) 0.0005(11) 0.0047(12) 0.0077(12) C13 0.0289(14) 0.0153(13) 0.0300(15) 0.0029(11) 0.0111(12) 0.0036(11) C3 0.0157(12) 0.0226(13) 0.0249(14) 0.0010(10) 0.0022(10) -0.0006(11) C5 0.0208(13) 0.0277(15) 0.0324(15) 0.0011(12) 0.0084(11) -0.0086(12) C19 0.0216(13) 0.0184(13) 0.0363(16) 0.0023(11) 0.0066(12) -0.0066(12) C4 0.0215(14) 0.0308(15) 0.0244(14) 0.0004(12) 0.0032(11) -0.0030(12) C20 0.0331(15) 0.0173(13) 0.0297(15) 0.0034(12) -0.0012(12) 0.0033(11) C21 0.0303(15) 0.0228(14) 0.0285(15) -0.0033(12) 0.0062(12) 0.0079(12) C18 0.0262(14) 0.0263(15) 0.0327(15) -0.0018(12) 0.0151(12) -0.0081(12) C22 0.0295(15) 0.0220(14) 0.0284(15) -0.0003(11) 0.0146(12) 0.0009(11) C23 0.0193(13) 0.0188(13) 0.0356(15) -0.0001(11) 0.0138(12) 0.0035(12) C12 0.0414(18) 0.0260(15) 0.0320(16) 0.0036(13) 0.0177(14) 0.0051(12) C11 0.0415(18) 0.0297(16) 0.0260(15) 0.0025(13) 0.0084(13) 0.0092(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 5 0 -12 0.1487 -10 -1 1 0.0807 -3 0 13 0.1852 -10 0 0 0.0665 -10 0 2 0.0802 3 2 -12 0.1710 2 -1 -13 0.1519 -8 0 11 0.1729 4 1 10 0.1493 9 1 3 0.0912 10 0 0 0.0513 5 -4 2 0.0705 -3 0 -10 0.1411 -6 -4 3 0.1107 -2 -5 2 0.0996 1 -5 2 0.0860 5 -2 -11 0.1586 -2 5 0 0.1302 5 4 1 0.1076 2 5 1 0.1226 0 0 12 0.1587 -10 0 0 0.0571 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 Cl1 Zn1 N1 . . 110.50(6) ? N2 Zn1 Cl1 . . 118.36(6) ? N2 Zn1 N1 . . 79.22(8) ? N2 Zn1 N3 . . 83.20(9) ? N2 Zn1 N4 . . 132.23(9) ? N3 Zn1 Cl1 . . 112.42(6) ? N3 Zn1 N1 . . 136.98(8) ? N4 Zn1 Cl1 . . 109.19(7) ? N4 Zn1 N1 . . 80.46(8) ? N4 Zn1 N3 . . 83.05(9) ? C15 N1 Zn1 . . 105.17(14) ? C16 N1 Zn1 . . 105.40(15) ? C16 N1 C15 . . 113.8(2) ? C23 N1 Zn1 . . 104.45(15) ? C23 N1 C15 . . 115.8(2) ? C23 N1 C16 . . 111.1(2) ? Zn1 N2 H2 . . 109.7 ? C17 N2 Zn1 . . 105.96(16) ? C17 N2 H2 . . 109.7 ? C17 N2 C18 . . 114.0(2) ? C18 N2 Zn1 . . 107.57(17) ? C18 N2 H2 . . 109.7 ? Zn1 N3 H3 . . 109.0 ? C19 N3 Zn1 . . 107.67(16) ? C19 N3 H3 . . 109.0 ? C19 N3 C20 . . 114.1(2) ? C20 N3 Zn1 . . 108.13(17) ? C20 N3 H3 . . 109.0 ? Zn1 N4 H4 . . 108.1 ? C21 N4 Zn1 . . 104.84(17) ? C21 N4 H4 . . 108.1 ? C21 N4 C22 . . 115.6(2) ? C22 N4 Zn1 . . 111.83(17) ? C22 N4 H4 . . 108.1 ? O2 N5 O1 . . 119.9(2) ? O3 N5 O1 . . 119.1(2) ? O3 N5 O2 . . 121.0(2) ? C2 C1 C15 . . 120.5(2) ? C2 C1 C14 . . 119.2(2) ? C14 C1 C15 . . 120.0(2) ? C1 C2 C7 . . 119.5(2) ? C1 C2 C3 . . 123.6(2) ? C3 C2 C7 . . 116.7(2) ? C8 C7 C2 . . 120.1(2) ? C8 C7 C6 . . 120.5(2) ? C6 C7 C2 . . 119.3(2) ? N2 C17 H17A . . 110.0 ? N2 C17 H17B . . 110.0 ? N2 C17 C16 . . 108.4(2) ? H17A C17 H17B . . 108.4 ? C16 C17 H17A . . 110.0 ? C16 C17 H17B . . 110.0 ? N1 C15 C1 . . 118.7(2) ? N1 C15 H15A . . 107.6 ? N1 C15 H15B . . 107.6 ? C1 C15 H15A . . 107.6 ? C1 C15 H15B . . 107.6 ? H15A C15 H15B . . 107.1 ? C7 C8 H8 . . 119.3 ? C7 C8 C9 . . 121.3(2) ? C9 C8 H8 . . 119.3 ? C8 C9 C14 . . 119.6(2) ? C8 C9 C10 . . 120.5(2) ? C10 C9 C14 . . 119.9(3) ? C1 C14 C9 . . 119.9(2) ? C1 C14 C13 . . 123.7(2) ? C13 C14 C9 . . 116.4(2) ? C7 C6 H6 . . 119.3 ? C5 C6 C7 . . 121.3(3) ? C5 C6 H6 . . 119.3 ? N1 C16 C17 . . 110.9(2) ? N1 C16 H16A . . 109.4 ? N1 C16 H16B . . 109.5 ? C17 C16 H16A . . 109.4 ? C17 C16 H16B . . 109.4 ? H16A C16 H16B . . 108.0 ? C9 C10 H10 . . 119.5 ? C11 C10 C9 . . 121.1(3) ? C11 C10 H10 . . 119.5 ? C14 C13 H13 . . 119.1 ? C12 C13 C14 . . 121.7(3) ? C12 C13 H13 . . 119.1 ? C2 C3 H3A . . 119.1 ? C4 C3 C2 . . 121.8(3) ? C4 C3 H3A . . 119.1 ? C6 C5 H5 . . 120.0 ? C6 C5 C4 . . 120.0(3) ? C4 C5 H5 . . 120.0 ? N3 C19 H19A . . 109.8 ? N3 C19 H19B . . 109.8 ? N3 C19 C18 . . 109.4(2) ? H19A C19 H19B . . 108.2 ? C18 C19 H19A . . 109.8 ? C18 C19 H19B . . 109.8 ? C3 C4 C5 . . 120.8(3) ? C3 C4 H4A . . 119.6 ? C5 C4 H4A . . 119.6 ? N3 C20 H20A . . 109.6 ? N3 C20 H20B . . 109.6 ? N3 C20 C21 . . 110.4(2) ? H20A C20 H20B . . 108.1 ? C21 C20 H20A . . 109.6 ? C21 C20 H20B . . 109.6 ? N4 C21 C20 . . 108.5(2) ? N4 C21 H21A . . 110.0 ? N4 C21 H21B . . 110.0 ? C20 C21 H21A . . 110.0 ? C20 C21 H21B . . 110.0 ? H21A C21 H21B . . 108.4 ? N2 C18 C19 . . 109.9(2) ? N2 C18 H18A . . 109.7 ? N2 C18 H18B . . 109.7 ? C19 C18 H18A . . 109.7 ? C19 C18 H18B . . 109.7 ? H18A C18 H18B . . 108.2 ? N4 C22 H22A . . 109.3 ? N4 C22 H22B . . 109.3 ? N4 C22 C23 . . 111.4(2) ? H22A C22 H22B . . 108.0 ? C23 C22 H22A . . 109.3 ? C23 C22 H22B . . 109.3 ? N1 C23 C22 . . 112.6(2) ? N1 C23 H23A . . 109.1 ? N1 C23 H23B . . 109.1 ? C22 C23 H23A . . 109.1 ? C22 C23 H23B . . 109.1 ? H23A C23 H23B . . 107.8 ? C13 C12 H12 . . 119.4 ? C13 C12 C11 . . 121.3(3) ? C11 C12 H12 . . 119.4 ? C10 C11 C12 . . 119.5(3) ? C10 C11 H11 . . 120.3 ? C12 C11 H11 . . 120.3 ? 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 Cl1 . 2.2466(7) ? Zn1 N1 . 2.330(2) ? Zn1 N2 . 2.087(2) ? Zn1 N3 . 2.127(2) ? Zn1 N4 . 2.109(2) ? O1 N5 . 1.261(3) ? O2 N5 . 1.249(3) ? N1 C15 . 1.495(3) ? N1 C16 . 1.489(3) ? N1 C23 . 1.473(3) ? N2 H2 . 1.0000 ? N2 C17 . 1.477(3) ? N2 C18 . 1.480(4) ? N3 H3 . 1.0000 ? N3 C19 . 1.471(4) ? N3 C20 . 1.478(4) ? O3 N5 . 1.244(3) ? N4 H4 . 1.0000 ? N4 C21 . 1.476(4) ? N4 C22 . 1.479(4) ? C1 C2 . 1.420(4) ? C1 C15 . 1.528(3) ? C1 C14 . 1.420(4) ? C2 C7 . 1.443(4) ? C2 C3 . 1.433(4) ? C7 C8 . 1.387(4) ? C7 C6 . 1.435(4) ? C17 H17A . 0.9900 ? C17 H17B . 0.9900 ? C17 C16 . 1.508(4) ? C15 H15A . 0.9900 ? C15 H15B . 0.9900 ? C8 H8 . 0.9500 ? C8 C9 . 1.392(4) ? C9 C14 . 1.442(4) ? C9 C10 . 1.435(4) ? C14 C13 . 1.437(4) ? C6 H6 . 0.9500 ? C6 C5 . 1.344(4) ? C16 H16A . 0.9900 ? C16 H16B . 0.9900 ? C10 H10 . 0.9500 ? C10 C11 . 1.353(4) ? C13 H13 . 0.9500 ? C13 C12 . 1.356(4) ? C3 H3A . 0.9500 ? C3 C4 . 1.359(4) ? C5 H5 . 0.9500 ? C5 C4 . 1.423(4) ? C19 H19A . 0.9900 ? C19 H19B . 0.9900 ? C19 C18 . 1.510(4) ? C4 H4A . 0.9500 ? C20 H20A . 0.9900 ? C20 H20B . 0.9900 ? C20 C21 . 1.521(4) ? C21 H21A . 0.9900 ? C21 H21B . 0.9900 ? C18 H18A . 0.9900 ? C18 H18B . 0.9900 ? C22 H22A . 0.9900 ? C22 H22B . 0.9900 ? C22 C23 . 1.512(4) ? C23 H23A . 0.9900 ? C23 H23B . 0.9900 ? C12 H12 . 0.9500 ? C12 C11 . 1.426(4) ? C11 H11 . 0.9500 ? 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 N2 H2 O1 1_555 1.00 1.98 2.983(3) 175 yes N3 H3 O1 2_645 1.00 2.16 3.025(3) 144 yes 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 Zn1 N1 C15 C1 . . . . 170.33(18) ? Zn1 N1 C16 C17 . . . . 23.5(2) ? Zn1 N1 C23 C22 . . . . 37.1(2) ? Zn1 N2 C17 C16 . . . . 58.9(2) ? Zn1 N2 C18 C19 . . . . 40.9(2) ? Zn1 N3 C19 C18 . . . . 37.5(2) ? Zn1 N3 C20 C21 . . . . 29.3(3) ? Zn1 N4 C21 C20 . . . . 49.6(2) ? Zn1 N4 C22 C23 . . . . 36.5(3) ? N2 C17 C16 N1 . . . . -55.4(3) ? N3 C19 C18 N2 . . . . -53.5(3) ? N3 C20 C21 N4 . . . . -54.3(3) ? N4 C22 C23 N1 . . . . -51.2(3) ? C1 C2 C7 C8 . . . . 0.4(4) ? C1 C2 C7 C6 . . . . -177.8(2) ? C1 C2 C3 C4 . . . . 176.3(3) ? C1 C14 C13 C12 . . . . 177.7(3) ? C2 C1 C15 N1 . . . . 94.8(3) ? C2 C1 C14 C9 . . . . -6.2(4) ? C2 C1 C14 C13 . . . . 171.5(2) ? C2 C7 C8 C9 . . . . -2.5(4) ? C2 C7 C6 C5 . . . . 1.8(4) ? C2 C3 C4 C5 . . . . 1.0(4) ? C7 C2 C3 C4 . . . . 0.1(4) ? C7 C8 C9 C14 . . . . 0.2(4) ? C7 C8 C9 C10 . . . . -178.1(2) ? C7 C6 C5 C4 . . . . -0.8(4) ? C17 N2 C18 C19 . . . . -76.3(3) ? C15 N1 C16 C17 . . . . 138.2(2) ? C15 N1 C23 C22 . . . . -78.0(3) ? C15 C1 C2 C7 . . . . 179.0(2) ? C15 C1 C2 C3 . . . . 2.8(4) ? C15 C1 C14 C9 . . . . 178.7(2) ? C15 C1 C14 C13 . . . . -3.6(4) ? C8 C7 C6 C5 . . . . -176.5(3) ? C8 C9 C14 C1 . . . . 4.2(4) ? C8 C9 C14 C13 . . . . -173.7(2) ? C8 C9 C10 C11 . . . . 176.9(3) ? C9 C14 C13 C12 . . . . -4.5(4) ? C9 C10 C11 C12 . . . . -2.3(5) ? C14 C1 C2 C7 . . . . 3.9(4) ? C14 C1 C2 C3 . . . . -172.3(2) ? C14 C1 C15 N1 . . . . -90.1(3) ? C14 C9 C10 C11 . . . . -1.4(4) ? C14 C13 C12 C11 . . . . 1.0(5) ? C6 C7 C8 C9 . . . . 175.7(2) ? C6 C5 C4 C3 . . . . -0.6(5) ? C16 N1 C15 C1 . . . . 55.5(3) ? C16 N1 C23 C22 . . . . 150.2(2) ? C10 C9 C14 C1 . . . . -177.5(2) ? C10 C9 C14 C13 . . . . 4.7(4) ? C13 C12 C11 C10 . . . . 2.6(5) ? C3 C2 C7 C8 . . . . 176.9(2) ? C3 C2 C7 C6 . . . . -1.4(4) ? C19 N3 C20 C21 . . . . -90.4(3) ? C20 N3 C19 C18 . . . . 157.5(2) ? C21 N4 C22 C23 . . . . -83.4(3) ? C18 N2 C17 C16 . . . . 177.0(2) ? C22 N4 C21 C20 . . . . 173.2(2) ? C23 N1 C15 C1 . . . . -75.0(3) ? C23 N1 C16 C17 . . . . -89.0(3) ?