#------------------------------------------------------------------------------ #$Date: 2021-06-16 07:40:34 +0300 (Wed, 16 Jun 2021) $ #$Revision: 266481 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243854.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_2243854 loop_ _publ_author_name 'Zhao, Chen' 'Li, Yi' 'Xiao, Jin-Sheng' 'Zhang, Peng-Dan' 'Wu, Xue-Qian' 'Chen, Qiang' _publ_section_title ; Synthesis and crystal structure of poly[(3-amino-1,2,4-triazole)(\m~3~-1H-benzimidazole-5,6-dicarboxylato)cobalt(II)] ; _journal_coeditor_code DJ2027 _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 714 _journal_page_last 717 _journal_paper_doi 10.1107/S2056989021005867 _journal_volume 77 _journal_year 2021 _chemical_formula_iupac '[Co (C9 H4 N2 O4) (C2 H4 N4)]' _chemical_formula_moiety 'C11 H8 Co N6 O4' _chemical_formula_sum 'C11 H8 Co N6 O4' _chemical_formula_weight 347.16 _chemical_name_systematic Poly[(3-amino-1,2,4-triazole)(\m~3~-1H-benzimidazole-5,6-dicarboxylato)cobalt(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 1.3-alpha (compiled 2019.04.25 svn.r3594 for OlexSys, GUI svn.r5751) ; _cell_angle_alpha 90 _cell_angle_beta 103.478(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.3368(8) _cell_length_b 6.8727(4) _cell_length_c 13.6015(10) _cell_measurement_reflns_used 1697 _cell_measurement_temperature 279(2) _cell_measurement_theta_max 26.7370 _cell_measurement_theta_min 4.2620 _cell_volume 1212.38(14) _computing_cell_refinement ; CrysAlisPro (Rigaku OD, 2018) ; _computing_data_collection ; CrysAlisPro (Rigaku OD, 2018) ; _computing_data_reduction ; CrysAlisPro (Rigaku OD, 2018) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 279(2) _diffrn_detector_area_resol_mean 10.3376 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Rigaku Oxford Diffraction SuperNova, Dual, Cu at home/near, AtlasS2' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_unetI/netI 0.0691 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 5618 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.366 _diffrn_reflns_theta_min 3.341 _exptl_absorpt_coefficient_mu 1.448 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.97909 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlis PRO; Rigaku OD, 2018) ; _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.902 _exptl_crystal_description block _exptl_crystal_F_000 700 _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.454 _refine_diff_density_min -0.434 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 199 _refine_ls_number_reflns 2475 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.027 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0468 _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^)+(0.0319P)^2^+0.6634P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0862 _refine_ls_wR_factor_ref 0.0978 _reflns_number_gt 1839 _reflns_number_total 2475 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file dj2027sup1.cif _cod_data_source_block I _cod_database_code 2243854 _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_hkl_file ; 0 0 3 2.78 3.24 0 0 4 6.16 4.23 0 0 5 6.70 5.06 0 0 6 316.03 25.25 0 0 7 31.16 9.28 0 0 -7 46.35 12.63 0 0 8 256.45 26.47 0 0 -8 263.80 27.24 0 0 -9 -3.80 7.66 0 0 9 -0.76 6.89 0 0 -10 45.87 14.35 0 0 10 36.79 12.37 0 0 -11 6.82 9.16 0 0 -12 2.39 9.62 0 0 -13 -4.08 10.76 0 0 -14 151.21 28.82 0 0 -15 26.13 14.04 0 0 -16 356.87 47.98 0 1 -1 102.03 8.72 0 1 1 109.61 6.70 0 1 2 4317.70 51.77 0 1 -2 4202.17 62.81 0 -1 2 4182.45 63.44 0 1 3 9999.00 91.49 0 -1 3 9663.87 110.20 0 -1 -3 9865.19 93.24 0 1 4 6093.02 82.99 0 -1 -4 6031.63 83.68 0 -1 4 6130.37 97.82 0 -1 -5 803.72 34.55 0 1 5 873.98 35.55 0 -1 5 824.35 40.33 0 1 6 1560.57 53.33 0 -1 6 1556.78 59.13 0 -1 -6 1575.38 52.96 0 1 7 27.56 8.48 0 -1 7 28.35 9.39 0 -1 -7 33.12 9.50 0 1 8 148.34 19.33 0 -1 -8 122.93 18.30 0 -1 8 131.57 20.05 0 -1 9 28.06 10.51 0 1 9 13.98 7.19 0 1 -9 -2.20 7.70 0 -1 -9 17.99 9.39 0 1 10 946.73 55.32 0 -1 10 866.96 57.68 0 -1 -10 924.93 54.24 0 1 -10 775.60 53.88 0 1 11 -14.76 8.93 0 -1 -11 7.97 9.16 0 1 -11 -5.46 9.20 0 -1 -12 78.00 19.26 0 1 -12 124.94 25.09 0 1 -13 101.75 23.80 0 -1 -13 83.67 20.47 0 1 -14 56.36 20.69 0 -1 -14 11.20 11.45 0 -1 -15 -5.21 10.60 0 1 -15 -45.46 18.98 0 -1 -16 -7.17 10.70 0 1 -16 1.53 10.31 0 2 0 7663.99 83.53 0 -2 0 7925.82 85.60 0 2 -1 2925.77 57.20 0 2 1 3112.40 49.65 0 -2 -1 3165.03 50.24 0 -2 1 3040.80 58.85 0 2 -2 5254.67 84.76 0 2 2 5245.85 63.36 0 -2 -2 5332.75 65.27 0 2 3 109.93 10.92 0 -2 -3 104.02 9.95 0 2 -3 106.01 13.64 0 2 4 573.64 26.47 0 -2 -4 568.87 27.24 0 2 -4 577.32 33.41 0 2 5 146.42 14.97 0 -2 -5 138.52 15.17 0 2 -5 151.62 18.92 0 -2 5 152.33 19.47 0 -2 -6 370.05 26.32 0 -2 6 322.16 29.74 0 2 6 343.62 24.57 0 2 -6 304.37 28.94 0 -2 -7 2109.07 67.08 0 2 7 1974.16 64.18 0 -2 7 2128.10 80.04 0 2 -7 2099.83 78.45 0 -2 8 272.32 30.55 0 -2 -8 252.51 25.52 0 2 8 273.89 25.77 0 -2 9 571.45 46.97 0 2 -9 538.70 44.59 0 -2 -9 514.90 38.21 0 2 9 551.05 38.98 0 2 -9 508.81 43.57 0 2 10 9.95 7.16 0 2 -10 5.75 6.90 0 -2 -10 14.25 8.56 0 2 11 13.87 8.62 0 -2 -11 2.71 8.61 0 2 -11 3.74 8.90 0 -2 -12 45.40 14.62 0 2 -12 36.06 15.19 0 -2 -13 70.67 18.59 0 2 -13 129.73 27.97 0 2 -14 207.06 36.46 0 -2 -14 277.79 37.61 0 -2 -15 31.35 16.77 0 2 -15 38.08 17.47 0 2 -16 66.96 23.38 0 -2 -16 65.28 21.14 0 3 0 0.26 3.94 0 -3 0 0.40 3.54 0 3 -1 1288.67 45.16 0 -3 -1 1223.16 39.49 0 3 1 1247.11 39.27 0 -3 1 1318.10 45.80 0 3 2 1411.21 40.16 0 -3 -2 1384.71 40.39 0 -3 2 1354.22 49.59 0 3 -2 1410.06 50.78 0 -3 -3 286.23 18.56 0 3 -3 317.18 25.93 0 3 3 295.31 20.46 0 3 -3 329.27 26.77 0 3 4 39.88 8.56 0 -3 -4 36.58 7.58 0 3 -4 15.28 6.48 0 -3 -5 917.45 36.17 0 3 5 901.72 38.63 0 3 -5 941.54 50.49 0 3 -6 314.99 31.39 0 3 6 342.33 25.29 0 -3 -6 321.88 23.19 0 3 -6 367.57 33.54 0 3 7 32.10 8.78 0 3 -7 44.22 15.09 0 3 -7 23.24 11.39 0 -3 -7 31.19 9.13 0 3 8 959.03 47.81 0 3 -8 874.91 58.28 0 3 -8 944.73 58.52 0 -3 -8 894.51 48.08 0 3 -9 55.66 16.24 0 3 9 64.89 14.38 0 -3 -9 56.35 14.00 0 3 -10 25.39 13.16 0 -3 -10 16.63 8.29 0 3 10 24.46 9.96 0 3 11 901.27 56.10 0 -3 -11 942.94 58.81 0 3 -11 954.94 67.96 0 -3 -12 47.35 16.64 0 3 -12 14.37 10.91 0 -3 -13 34.99 14.61 0 3 -13 7.40 10.23 0 3 -14 132.50 30.42 0 -3 -14 76.91 20.21 0 3 -15 37.05 17.28 0 -3 -15 41.13 15.17 0 -4 0 838.66 40.44 0 4 0 886.77 40.64 0 -4 1 526.99 33.45 0 4 1 522.19 29.85 0 4 -1 553.58 33.97 0 -4 -1 474.22 28.85 0 -4 -2 452.61 27.38 0 4 -2 376.45 29.86 0 -4 2 397.48 31.08 0 4 2 417.14 25.59 0 -4 -3 438.26 26.40 0 4 3 393.15 24.43 0 4 -3 462.01 34.81 0 -4 -4 418.97 26.06 0 4 -4 441.55 35.99 0 4 4 431.94 28.04 0 4 -4 410.79 34.21 0 -4 -5 1760.20 54.18 0 4 5 1739.58 58.36 0 4 -5 1863.10 77.18 0 4 -5 1964.40 79.44 0 -4 -6 11.61 6.17 0 4 -6 5.04 8.68 0 4 6 20.47 7.34 0 4 -6 11.81 9.60 0 4 -7 262.32 32.66 0 -4 -7 302.29 24.71 0 4 7 269.46 25.29 0 4 -7 304.21 34.44 0 4 8 59.86 12.83 0 -4 -8 40.26 10.58 0 4 -8 45.55 15.05 0 4 -9 287.96 37.18 0 -4 -9 367.18 30.73 0 4 9 293.99 28.94 0 4 10 91.25 17.98 0 4 -10 81.84 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-4.68 10.78 13 -4 -10 4.20 12.87 13 -4 -9 57.38 23.24 13 -4 -8 50.91 22.66 13 4 -8 25.29 12.27 13 -4 -7 247.72 41.14 13 4 -7 240.62 32.62 13 4 -6 15.90 9.28 13 -4 -6 13.85 16.17 13 4 -5 31.54 11.71 13 -4 -5 73.70 23.70 13 4 -4 6.90 6.86 13 -4 -4 -6.50 15.39 13 -4 -3 635.25 64.46 13 -4 -2 -6.49 11.79 13 -4 -1 797.35 72.59 13 -4 0 3.13 12.58 13 -4 1 340.31 48.47 13 -4 2 -22.79 16.46 13 -4 3 15.64 14.71 13 -5 -6 25.61 14.88 13 -5 -5 5.02 11.48 13 -5 -4 22.58 15.83 13 -5 -3 140.32 33.10 13 -5 -2 17.49 14.43 13 -5 -1 29.28 15.02 13 -5 0 12.35 12.55 14 0 -12 84.78 24.87 14 0 -11 17.90 13.29 14 0 -10 23.05 16.03 14 0 -9 -23.78 14.37 14 0 -8 129.58 27.30 14 0 -7 1.58 8.70 14 0 -6 -1.34 10.09 14 0 -5 2.95 10.55 14 0 -4 555.72 51.97 14 0 -3 0.29 7.65 14 0 -2 180.91 28.98 14 0 -1 -13.98 10.08 14 0 0 371.55 40.99 14 0 1 9.10 9.41 14 0 2 202.07 30.89 14 0 3 -9.79 9.54 -14 0 -4 79.05 20.81 14 0 4 58.13 18.33 -14 0 -5 26.82 13.34 14 0 5 -18.49 11.31 14 -1 -12 129.58 31.94 14 1 -12 114.62 28.13 14 -1 -11 -25.10 16.00 14 1 -11 20.11 13.42 14 1 -10 217.71 37.12 14 -1 -10 220.31 39.39 14 1 -9 12.32 13.43 14 -1 -9 4.73 9.02 14 1 -8 128.76 27.29 14 -1 -8 136.45 29.96 14 1 -7 41.08 16.87 14 -1 -7 58.37 20.26 14 1 -6 145.31 27.23 14 -1 -6 161.02 30.95 14 1 -5 -2.17 9.34 14 -1 -5 -5.46 8.93 14 1 -4 193.40 29.87 14 -1 -4 313.14 40.79 14 1 -3 140.12 25.09 14 -1 -3 172.28 30.51 14 1 -2 6.32 7.35 14 -1 -2 -1.01 8.83 14 -1 -1 49.33 17.91 14 1 -1 88.73 19.68 14 1 0 132.63 23.41 14 -1 0 151.43 29.06 14 -1 1 35.75 15.41 14 1 1 23.86 10.29 14 -1 2 118.68 25.49 14 1 2 94.84 20.00 14 -1 3 12.09 11.62 14 1 3 4.11 7.78 14 1 4 94.51 19.83 14 -1 4 128.26 26.23 14 -1 5 30.60 13.46 -14 1 -5 10.89 9.94 14 -2 -11 151.12 34.14 14 2 -11 151.04 33.14 14 -2 -10 10.40 14.19 14 2 -10 12.04 10.17 14 2 -9 71.51 21.27 14 -2 -9 99.14 26.98 14 2 -8 19.62 13.01 14 -2 -8 28.34 16.30 14 2 -7 18.13 12.76 14 -2 -7 23.45 14.99 14 2 -6 6.47 7.27 14 -2 -6 5.50 9.13 14 2 -5 122.60 23.20 14 -2 -5 139.21 29.97 14 2 -4 100.29 20.60 14 -2 -4 154.11 30.58 14 2 -3 3.68 7.07 14 -2 -3 -8.09 10.57 14 2 -2 189.75 26.20 14 -2 -2 205.39 36.03 14 -2 -1 22.78 15.21 14 2 -1 0.94 6.58 14 2 0 104.65 19.47 14 -2 0 131.31 26.97 14 -2 1 -15.03 12.64 14 2 1 -2.07 6.95 14 -2 2 55.29 19.60 14 -2 3 24.03 16.59 14 -2 4 27.16 15.16 14 -3 -10 66.16 25.53 14 3 -10 68.67 20.77 14 -3 -9 37.30 19.77 14 3 -9 3.26 8.69 14 3 -8 10.79 11.46 14 -3 -8 36.67 18.77 14 3 -7 13.11 10.33 14 -3 -7 2.32 10.98 14 3 -6 64.98 17.41 14 -3 -6 79.89 24.39 14 3 -5 110.00 21.71 14 -3 -5 122.26 29.37 14 3 -4 88.74 18.18 14 -3 -4 108.04 27.22 14 3 -3 296.69 31.64 14 -3 -3 315.09 45.08 14 -3 -2 42.12 18.34 14 3 -2 44.63 13.26 14 -3 -1 296.98 43.52 14 -3 0 5.64 12.17 14 -3 1 96.29 26.04 14 -3 2 -12.41 13.23 14 -3 3 200.77 38.06 14 4 -7 118.69 24.02 14 -4 -7 68.31 24.22 14 4 -6 -11.08 8.95 14 -4 -6 24.72 16.22 14 -4 -5 83.64 25.33 14 -4 -4 7.53 16.25 14 -4 -3 11.32 13.95 14 -4 -2 45.87 22.67 14 -4 -1 78.75 22.59 14 -4 0 14.55 12.92 14 -4 1 34.04 19.45 15 0 -10 175.89 34.49 15 0 -9 -0.31 8.83 15 0 -8 300.94 43.34 15 0 -7 4.09 12.26 15 0 -6 572.93 56.68 15 0 -5 -11.41 10.85 15 0 -4 169.70 30.66 15 0 -3 1.76 8.62 15 0 -2 35.30 14.03 15 0 -1 22.11 12.44 15 0 0 13.10 11.24 15 0 1 5.64 13.03 15 0 2 162.08 28.97 15 0 3 16.04 11.55 15 1 -10 41.25 21.01 15 -1 -10 37.10 18.02 15 1 -9 111.79 27.01 15 -1 -9 78.35 26.13 15 1 -8 135.10 28.28 15 -1 -8 105.88 27.41 15 1 -7 23.30 12.09 15 -1 -7 50.75 19.71 15 1 -6 359.30 43.30 15 -1 -6 450.89 52.07 15 1 -5 8.71 10.23 15 -1 -5 22.34 14.84 15 1 -4 366.86 42.01 15 -1 -4 416.59 49.74 15 1 -3 1.14 9.16 15 -1 -3 20.22 12.15 15 1 -2 249.37 34.22 15 -1 -2 263.31 39.08 15 1 -1 12.53 10.41 15 -1 -1 -1.30 12.40 15 1 0 145.10 25.75 15 -1 0 158.03 30.04 15 -1 1 14.31 10.74 15 1 1 25.79 12.34 15 1 2 64.32 18.26 15 -1 2 47.16 16.39 15 -1 3 -25.00 14.52 15 2 -9 25.83 12.94 15 -2 -9 6.25 11.76 15 2 -8 24.04 14.08 15 -2 -8 52.53 22.81 15 2 -7 5.34 9.07 15 -2 -7 -17.05 13.93 15 2 -6 224.33 33.48 15 -2 -6 260.18 41.45 15 2 -5 272.76 35.97 15 -2 -5 290.73 43.63 15 2 -4 -1.79 8.70 15 -2 -4 1.93 9.52 15 2 -3 193.09 28.57 15 -2 -3 243.15 40.32 15 -2 -2 13.77 11.95 15 2 -2 -8.07 8.44 15 2 -1 51.77 15.48 15 -2 -1 104.91 26.12 15 -2 0 131.07 29.57 15 -2 1 58.57 18.80 15 -2 2 163.50 33.04 15 3 -7 142.43 27.31 15 -3 -7 267.43 44.46 15 3 -6 109.81 22.86 15 -3 -6 148.03 32.78 15 3 -5 17.67 10.25 15 -3 -5 46.34 20.69 15 3 -4 138.39 27.15 15 -3 -4 156.39 34.08 15 -3 -3 29.77 15.83 15 -3 -2 21.39 13.48 15 -3 -1 164.33 34.00 15 -3 0 89.11 25.64 16 0 -8 97.90 26.33 16 0 -7 -4.48 9.70 16 0 -6 21.77 16.58 16 0 -5 6.99 11.05 16 0 -4 290.02 40.16 16 0 -3 21.85 13.25 16 0 -2 307.84 41.09 16 0 -1 22.39 12.73 16 0 0 170.59 30.70 16 1 -8 154.53 35.30 16 -1 -8 91.90 26.13 16 1 -7 40.38 16.92 16 -1 -7 30.53 17.08 16 1 -6 96.87 23.07 16 -1 -6 93.87 25.90 16 1 -5 21.92 11.49 16 -1 -5 34.26 17.37 16 1 -4 51.61 17.89 16 -1 -4 62.24 22.69 16 1 -3 9.68 10.82 16 -1 -3 14.23 11.68 16 -1 -2 34.18 15.09 16 1 -2 56.13 18.11 16 1 -1 9.80 17.34 16 -1 -1 18.05 14.41 16 1 0 61.91 18.13 16 -1 0 54.21 18.36 16 2 -6 166.39 30.21 16 -2 -6 175.92 36.37 16 2 -5 51.08 15.99 16 -2 -5 31.52 17.05 16 2 -4 133.90 24.73 16 -2 -4 95.01 27.33 16 -2 -3 -4.13 10.10 16 2 -3 3.27 9.41 16 -2 -2 158.85 32.43 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 619 _shelx_res_file ; TITL w_a.res in P2(1)/c w.res created by SHELXL-2018/3 at 09:36:50 on 13-Sep-2019 REM Old TITL W in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.119, Rweak 0.005, Alpha 0.032, Orientation as input REM Formula found by SHELXT: C14 N5 O2 Co CELL 0.71073 13.3368 6.8727 13.6015 90 103.478 90 ZERR 4 0.0008 0.0004 0.001 0 0.007 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Co N O UNIT 44 32 4 24 16 L.S. 20 PLAN 5 BOND $H list 4 fmap 2 53 acta REM REM REM WGHT 0.031900 0.663400 FVAR 0.59403 CO1 3 0.753596 0.694506 0.527453 11.00000 0.01562 0.02248 = 0.02726 -0.00205 0.00539 -0.00139 O2 5 0.769172 -0.184674 0.400669 11.00000 0.02476 0.03460 = 0.03149 0.01259 0.00965 0.01176 O1 5 0.741575 0.017122 0.272111 11.00000 0.02734 0.03160 = 0.03692 0.01211 0.01776 0.00872 O4 5 0.661125 0.478450 0.492001 11.00000 0.02340 0.02699 = 0.04809 -0.01141 0.00833 -0.00548 O3 5 0.774864 0.275388 0.453743 11.00000 0.01461 0.05188 = 0.06127 -0.02086 0.01345 -0.00662 N2 4 0.315408 0.124017 0.392188 11.00000 0.01514 0.02495 = 0.02143 -0.00095 0.00573 -0.00294 N1 4 0.339867 -0.155172 0.318805 11.00000 0.02061 0.02591 = 0.03070 -0.00876 0.00796 -0.00531 AFIX 43 H1 2 0.326047 -0.266046 0.289464 11.00000 -1.20000 AFIX 0 N4 4 0.900413 0.692751 0.605281 11.00000 0.01415 0.03207 = 0.03265 0.00322 0.00468 -0.00102 C4 1 0.686189 0.318802 0.454433 11.00000 0.01967 0.02326 = 0.02282 -0.00141 0.00678 -0.00687 C7 1 0.435050 -0.065518 0.343194 11.00000 0.02004 0.01991 = 0.01965 -0.00016 0.00552 -0.00348 C6 1 0.418829 0.111012 0.389215 11.00000 0.01750 0.02004 = 0.02012 0.00197 0.00598 -0.00075 C8 1 0.531938 -0.121525 0.332152 11.00000 0.02288 0.01857 = 0.02615 -0.00327 0.00693 0.00304 AFIX 43 H8 2 0.541882 -0.239926 0.302707 11.00000 -1.20000 AFIX 0 N3 4 1.066746 0.720560 0.651118 11.00000 0.01592 0.06212 = 0.04310 0.00889 0.00826 -0.00360 AFIX 43 H3 2 1.129713 0.736543 0.647408 11.00000 -1.20000 AFIX 0 C1 1 0.715752 -0.054599 0.345628 11.00000 0.02218 0.01750 = 0.02385 -0.00531 0.00668 -0.00183 C3 1 0.598617 0.184799 0.413225 11.00000 0.01838 0.02328 = 0.01992 0.00047 0.00463 -0.00122 C9 1 0.273108 -0.037644 0.349263 11.00000 0.01903 0.02923 = 0.02795 -0.00120 0.00524 -0.00193 AFIX 43 H9 2 0.203572 -0.067057 0.340978 11.00000 -1.20000 AFIX 0 C2 1 0.612905 0.005101 0.366509 11.00000 0.01781 0.02232 = 0.01869 0.00409 0.00297 0.00240 C5 1 0.500793 0.236102 0.424002 11.00000 0.02034 0.01958 = 0.02401 -0.00029 0.00409 -0.00112 AFIX 43 H5 2 0.490570 0.353422 0.454314 11.00000 -1.20000 AFIX 0 N5 4 1.036104 0.688800 0.739282 11.00000 0.02597 0.06781 = 0.03886 0.00829 0.00324 -0.00590 N6 4 0.992080 0.748990 0.475992 11.00000 0.02973 0.08364 = 0.03788 0.01043 0.01611 0.00134 AFIX 93 H6A 2 1.051093 0.765185 0.461830 11.00000 -1.20000 H6B 2 0.936808 0.749236 0.428430 11.00000 -1.20000 AFIX 0 C10 1 0.986256 0.723396 0.572078 11.00000 0.02280 0.03108 = 0.03752 0.00633 0.00986 0.00271 C11 1 0.936704 0.673424 0.707344 11.00000 0.02561 0.05471 = 0.03364 0.01020 0.00661 -0.00150 AFIX 43 H11 2 0.893449 0.650912 0.750793 11.00000 -1.20000 AFIX 0 HKLF 4 REM w_a.res in P2(1)/c REM wR2 = 0.0978, GooF = S = 1.027, Restrained GooF = 1.027 for all data REM R1 = 0.0468 for 1839 Fo > 4sig(Fo) and 0.0712 for all 2475 data REM 199 parameters refined using 0 restraints END WGHT 0.0319 0.6634 REM Highest difference peak 0.454, deepest hole -0.434, 1-sigma level 0.093 Q1 1 0.7090 0.8006 0.5049 11.00000 0.05 0.42 Q2 1 0.9952 0.8202 0.7385 11.00000 0.05 0.41 Q3 1 0.8365 0.6667 0.5682 11.00000 0.05 0.40 Q4 1 0.7388 -0.2982 0.4157 11.00000 0.05 0.38 Q5 1 0.4659 -0.0844 0.2976 11.00000 0.05 0.37 ; _shelx_res_checksum 55129 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 Co Co1 0.75360(3) 0.69451(6) 0.52745(4) 0.02172(16) Uani d 1 . . O O2 0.76917(18) -0.1847(3) 0.40067(19) 0.0298(6) Uani d 1 . . O O1 0.74157(18) 0.0171(3) 0.27211(19) 0.0303(6) Uani d 1 . . O O4 0.66113(18) 0.4785(3) 0.4920(2) 0.0328(6) Uani d 1 . . O O3 0.77486(18) 0.2754(4) 0.4537(2) 0.0418(7) Uani d 1 . . N N2 0.3154(2) 0.1240(4) 0.3922(2) 0.0203(6) Uani d 1 . . N N1 0.3399(2) -0.1552(4) 0.3188(2) 0.0254(7) Uani d 1 . . H H1 0.326047 -0.266046 0.289464 0.030 Uiso calc 1 . . N N4 0.9004(2) 0.6928(4) 0.6053(2) 0.0264(7) Uani d 1 . . C C4 0.6862(3) 0.3188(5) 0.4544(3) 0.0216(8) Uani d 1 . . C C7 0.4351(2) -0.0655(5) 0.3432(2) 0.0197(7) Uani d 1 . . C C6 0.4188(2) 0.1110(5) 0.3892(2) 0.0190(7) Uani d 1 . . C C8 0.5319(2) -0.1215(5) 0.3322(3) 0.0223(8) Uani d 1 . . H H8 0.541882 -0.239926 0.302707 0.027 Uiso calc 1 . . N N3 1.0667(2) 0.7206(5) 0.6511(3) 0.0402(9) Uani d 1 . . H H3 1.129713 0.736543 0.647408 0.048 Uiso calc 1 . . C C1 0.7158(3) -0.0546(5) 0.3456(3) 0.0210(8) Uani d 1 . . C C3 0.5986(2) 0.1848(5) 0.4132(2) 0.0205(7) Uani d 1 . . C C9 0.2731(3) -0.0376(5) 0.3493(3) 0.0254(8) Uani d 1 . . H H9 0.203572 -0.067057 0.340978 0.031 Uiso calc 1 . . C C2 0.6129(2) 0.0051(5) 0.3665(2) 0.0198(7) Uani d 1 . . C C5 0.5008(2) 0.2361(5) 0.4240(3) 0.0215(8) Uani d 1 . . H H5 0.490570 0.353422 0.454314 0.026 Uiso calc 1 . . N N5 1.0361(2) 0.6888(5) 0.7393(3) 0.0449(9) Uani d 1 . . N N6 0.9921(3) 0.7490(5) 0.4760(3) 0.0491(10) Uani d 1 . . H H6A 1.051093 0.765185 0.461830 0.059 Uiso calc 1 . . H H6B 0.936808 0.749236 0.428430 0.059 Uiso calc 1 . . C C10 0.9863(3) 0.7234(5) 0.5721(3) 0.0300(9) Uani d 1 . . C C11 0.9367(3) 0.6734(6) 0.7073(3) 0.0380(10) Uani d 1 . . H H11 0.893449 0.650912 0.750793 0.046 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 Co1 0.0156(3) 0.0225(3) 0.0273(3) -0.0014(2) 0.00539(19) -0.0020(2) O2 0.0248(13) 0.0346(14) 0.0315(15) 0.0118(12) 0.0097(11) 0.0126(12) O1 0.0273(14) 0.0316(14) 0.0369(16) 0.0087(12) 0.0178(12) 0.0121(12) O4 0.0234(14) 0.0270(14) 0.0481(17) -0.0055(12) 0.0083(12) -0.0114(13) O3 0.0146(13) 0.0519(18) 0.061(2) -0.0066(13) 0.0135(13) -0.0209(15) N2 0.0151(14) 0.0249(15) 0.0214(16) -0.0029(13) 0.0057(12) -0.0010(13) N1 0.0206(15) 0.0259(16) 0.0307(18) -0.0053(13) 0.0080(13) -0.0088(13) N4 0.0142(14) 0.0321(17) 0.0327(18) -0.0010(13) 0.0047(13) 0.0032(14) C4 0.0197(18) 0.0233(18) 0.0228(19) -0.0069(15) 0.0068(14) -0.0014(15) C7 0.0200(18) 0.0199(17) 0.0197(18) -0.0035(15) 0.0055(14) -0.0002(14) C6 0.0175(17) 0.0200(17) 0.0201(18) -0.0007(15) 0.0060(14) 0.0020(14) C8 0.0229(18) 0.0186(17) 0.026(2) 0.0030(16) 0.0069(15) -0.0033(15) N3 0.0159(16) 0.062(2) 0.043(2) -0.0036(16) 0.0083(15) 0.0089(18) C1 0.0222(18) 0.0175(17) 0.0239(19) -0.0018(15) 0.0067(15) -0.0053(15) C3 0.0184(17) 0.0233(18) 0.0199(18) -0.0012(15) 0.0046(14) 0.0005(15) C9 0.0190(18) 0.0292(19) 0.028(2) -0.0019(16) 0.0052(15) -0.0012(16) C2 0.0178(17) 0.0223(18) 0.0187(18) 0.0024(15) 0.0030(14) 0.0041(15) C5 0.0203(18) 0.0196(17) 0.0240(19) -0.0011(15) 0.0041(15) -0.0003(15) N5 0.0260(18) 0.068(3) 0.039(2) -0.0059(17) 0.0032(16) 0.0083(19) N6 0.0297(19) 0.084(3) 0.038(2) 0.0013(19) 0.0161(16) 0.010(2) C10 0.0228(19) 0.031(2) 0.038(2) 0.0027(17) 0.0099(17) 0.0063(18) C11 0.026(2) 0.055(3) 0.034(2) -0.001(2) 0.0066(17) 0.010(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' Co Co 0.3494 0.9721 '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 O2 Co1 N2 1_565 3_666 111.64(11) ? O2 Co1 N4 1_565 . 100.15(11) ? O4 Co1 O2 . 1_565 107.41(11) ? O4 Co1 N2 . 3_666 105.49(11) ? O4 Co1 N4 . . 128.46(11) ? N4 Co1 N2 . 3_666 103.38(11) ? C1 O2 Co1 . 1_545 130.8(2) ? C4 O4 Co1 . . 123.3(2) ? C6 N2 Co1 . 3_666 129.5(2) ? C9 N2 Co1 . 3_666 124.0(2) ? C9 N2 C6 . . 104.9(3) ? C7 N1 H1 . . 126.4 ? C9 N1 H1 . . 126.4 ? C9 N1 C7 . . 107.3(3) ? C10 N4 Co1 . . 129.0(3) ? C10 N4 C11 . . 103.3(3) ? C11 N4 Co1 . . 127.6(3) ? O4 C4 C3 . . 115.0(3) ? O3 C4 O4 . . 123.5(3) ? O3 C4 C3 . . 121.4(3) ? N1 C7 C6 . . 105.3(3) ? N1 C7 C8 . . 132.6(3) ? C8 C7 C6 . . 122.1(3) ? N2 C6 C7 . . 109.0(3) ? C5 C6 N2 . . 131.2(3) ? C5 C6 C7 . . 119.8(3) ? C7 C8 H8 . . 121.2 ? C2 C8 C7 . . 117.5(3) ? C2 C8 H8 . . 121.2 ? N5 N3 H3 . . 124.4 ? C10 N3 H3 . . 124.4 ? C10 N3 N5 . . 111.1(3) ? O2 C1 C2 . . 119.0(3) ? O1 C1 O2 . . 122.3(3) ? O1 C1 C2 . . 118.6(3) ? C2 C3 C4 . . 122.0(3) ? C5 C3 C4 . . 118.4(3) ? C5 C3 C2 . . 119.6(3) ? N2 C9 N1 . . 113.5(3) ? N2 C9 H9 . . 123.2 ? N1 C9 H9 . . 123.2 ? C8 C2 C1 . . 115.8(3) ? C8 C2 C3 . . 121.5(3) ? C3 C2 C1 . . 122.6(3) ? C6 C5 C3 . . 119.4(3) ? C6 C5 H5 . . 120.3 ? C3 C5 H5 . . 120.3 ? C11 N5 N3 . . 102.1(3) ? H6A N6 H6B . . 120.0 ? C10 N6 H6A . . 120.0 ? C10 N6 H6B . . 120.0 ? N3 C10 N4 . . 108.5(3) ? N3 C10 N6 . . 124.8(4) ? N6 C10 N4 . . 126.7(3) ? N4 C11 H11 . . 122.5 ? N5 C11 N4 . . 115.1(4) ? N5 C11 H11 . . 122.5 ? 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 Co1 O2 1_565 1.968(2) ? Co1 O4 . 1.919(2) ? Co1 N2 3_666 2.016(3) ? Co1 N4 . 1.997(3) ? O2 C1 . 1.272(4) ? O1 C1 . 1.234(4) ? O4 C4 . 1.287(4) ? O3 C4 . 1.222(4) ? N2 C6 . 1.392(4) ? N2 C9 . 1.319(4) ? N1 H1 . 0.8600 ? N1 C7 . 1.380(4) ? N1 C9 . 1.337(4) ? N4 C10 . 1.342(5) ? N4 C11 . 1.366(5) ? C4 C3 . 1.490(5) ? C7 C6 . 1.405(5) ? C7 C8 . 1.390(4) ? C6 C5 . 1.384(4) ? C8 H8 . 0.9300 ? C8 C2 . 1.381(5) ? N3 H3 . 0.8600 ? N3 N5 . 1.372(5) ? N3 C10 . 1.331(5) ? C1 C2 . 1.521(5) ? C3 C2 . 1.422(5) ? C3 C5 . 1.392(5) ? C9 H9 . 0.9300 ? C5 H5 . 0.9300 ? N5 C11 . 1.300(5) ? N6 H6A . 0.8600 ? N6 H6B . 0.8600 ? N6 C10 . 1.339(5) ? C11 H11 . 0.9300 ? 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 N1 H1 O1 2_645 0.86 1.84 2.675(4) 163 yes N3 H3 O1 3_766 0.86 2.48 3.104(4) 130 yes N3 H3 O3 3_766 0.86 2.08 2.811(4) 142 yes N6 H6A O3 3_766 0.86 2.35 3.036(5) 136 yes N6 H6B O2 1_565 0.86 2.23 2.946(5) 141 yes C5 H5 O4 3_666 0.93 2.58 3.312(4) 136 yes C5 H5 O4 . 0.93 2.37 2.698(4) 100 no C9 H9 N5 4_465 0.93 2.48 3.332(5) 152 yes C11 H11 O1 4_566 0.93 2.41 3.215(5) 145 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 Co1 O4 C4 O3 . . . . 13.1(5) ? Co1 O4 C4 C3 . . . . -168.4(2) ? C9 N1 C7 C8 . . . . 178.0(4) ? C9 N1 C7 C6 . . . . -0.2(4) ? C9 N2 C6 C5 . . . . -179.1(4) ? Co1 N2 C6 C5 3_666 . . . -13.5(5) ? C9 N2 C6 C7 . . . . -0.3(4) ? Co1 N2 C6 C7 3_666 . . . 165.4(2) ? N1 C7 C6 C5 . . . . 179.3(3) ? C8 C7 C6 C5 . . . . 0.8(5) ? N1 C7 C6 N2 . . . . 0.3(4) ? C8 C7 C6 N2 . . . . -178.2(3) ? N1 C7 C8 C2 . . . . -179.2(3) ? C6 C7 C8 C2 . . . . -1.2(5) ? Co1 O2 C1 O1 1_545 . . . 173.7(2) ? Co1 O2 C1 C2 1_545 . . . -10.5(4) ? O3 C4 C3 C5 . . . . 174.7(3) ? O4 C4 C3 C5 . . . . -3.8(5) ? O3 C4 C3 C2 . . . . -3.3(5) ? O4 C4 C3 C2 . . . . 178.2(3) ? C6 N2 C9 N1 . . . . 0.2(4) ? Co1 N2 C9 N1 3_666 . . . -166.5(2) ? C7 N1 C9 N2 . . . . 0.0(4) ? C7 C8 C2 C3 . . . . 1.1(5) ? C7 C8 C2 C1 . . . . -175.4(3) ? C5 C3 C2 C8 . . . . -0.6(5) ? C4 C3 C2 C8 . . . . 177.4(3) ? C5 C3 C2 C1 . . . . 175.7(3) ? C4 C3 C2 C1 . . . . -6.3(5) ? O1 C1 C2 C8 . . . . 98.3(4) ? O2 C1 C2 C8 . . . . -77.6(4) ? O1 C1 C2 C3 . . . . -78.3(4) ? O2 C1 C2 C3 . . . . 105.8(4) ? N2 C6 C5 C3 . . . . 178.5(3) ? C7 C6 C5 C3 . . . . -0.2(5) ? C2 C3 C5 C6 . . . . 0.1(5) ? C4 C3 C5 C6 . . . . -177.9(3) ? C10 N3 N5 C11 . . . . 0.2(4) ? N5 N3 C10 N6 . . . . -179.1(4) ? N5 N3 C10 N4 . . . . -0.3(4) ? C11 N4 C10 N3 . . . . 0.3(4) ? Co1 N4 C10 N3 . . . . 176.1(2) ? C11 N4 C10 N6 . . . . 179.1(4) ? Co1 N4 C10 N6 . . . . -5.1(6) ? N3 N5 C11 N4 . . . . 0.0(5) ? C10 N4 C11 N5 . . . . -0.2(5) ? Co1 N4 C11 N5 . . . . -176.1(3) ? _cod_database_fobs_code 2243854