#------------------------------------------------------------------------------ #$Date: 2025-02-08 04:00:48 +0100 (Sat, 08 Feb 2025) $ #$Revision: 297640 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/33/2023382.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_2023382 loop_ _publ_author_name 'Kumagai, Hitoshi' 'Kawata, Satoshi' 'Ogihara, Nobuhiro' _publ_section_title ; Crystal structure of catena-poly[[[tetraaquacobalt(II)]-\m2-1,5-dihydroxynaphthalene-2,6-dicarboxylato] dimethylformamide disolvate] ; _journal_coeditor_code JP2016 _journal_issue 3 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989025000982 _journal_volume 81 _journal_year 2025 _chemical_formula_iupac '[Co (C12 H6 O6) (H2 O1)4], 2C3 H7 N1 O1' _chemical_formula_moiety 'C18 H28 Co N2 O12' _chemical_formula_sum 'C18 H28 Co N2 O12' _chemical_formula_weight 523.35 _chemical_name_systematic 'catena-Poly[[[tetraaquacobalt(II)]-\m~2~-1,5-dihydroxynaphthalene-2,6-dicarboxylato] dimethylformamide disolvate]' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 85.543(5) _cell_angle_beta 84.371(5) _cell_angle_gamma 83.981(5) _cell_formula_units_Z 1 _cell_length_a 6.8860(10) _cell_length_b 6.9450(10) _cell_length_c 12.0366(15) _cell_measurement_reflns_used 7544 _cell_measurement_temperature 110(2) _cell_measurement_theta_max 27.52 _cell_measurement_theta_min 3.31 _cell_volume 568.37(14) _computing_cell_refinement ; RAPID-AUTO (Rigaku, 2002) ; _computing_data_collection ; RAPID-AUTO (Rigaku, 2002) ; _computing_data_reduction ; RAPID-AUTO (Rigaku, 2002) ; _computing_molecular_graphics ; Yadokari-XG (Wakita, 2001) ; _computing_publication_material ; Yadokari-XG (Wakita, 2001) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014/5 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 110(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_unetI/netI 0.0223 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 9228 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.480 _diffrn_reflns_theta_min 3.302 _exptl_absorpt_coefficient_mu 0.821 _exptl_absorpt_correction_T_max 0.922 _exptl_absorpt_correction_T_min 0.760 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (ABSCOR; Rigaku, 1995) ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.529 _exptl_crystal_description Block _exptl_crystal_F_000 273 _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.621 _refine_diff_density_min -0.244 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 173 _refine_ls_number_reflns 2595 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.111 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0279 _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^)+(0.0456P)^2^+0.1029P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0721 _refine_ls_wR_factor_ref 0.0743 _reflns_number_gt 2413 _reflns_number_total 2595 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jp2016.cif _cod_data_source_block I _cod_database_code 2023382 _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 0.821 _shelx_estimated_absorpt_t_max 0.922 _shelx_hkl_file ; -1 0 -1 4168.93 95.85 1 0 1 4126.03 94.96 -1 0 -1 3901.15 90.85 1 0 1 3975.73 92.41 0 -1 -1 12.26 0.65 0 -1 -1 8.90 0.39 0 1 1 7.94 0.58 0 1 1 8.20 0.44 0 0 2 18.93 0.57 0 0 -2 19.68 0.29 0 0 2 18.62 0.37 0 0 -2 17.61 0.88 0 -1 1 527.12 7.91 0 1 -1 543.47 8.41 0 1 -1 505.11 7.91 0 -1 1 487.77 8.12 1 0 -1 7.73 0.46 1 0 -1 8.11 0.45 -1 0 1 9.38 0.67 -1 0 1 7.55 0.46 -1 -1 0 34.33 1.45 -1 -1 0 35.33 1.81 1 1 0 33.06 1.53 1 1 0 34.14 1.78 -1 -1 -1 948.31 17.42 1 1 1 908.78 16.44 -1 -1 -1 939.52 17.59 1 1 1 906.91 16.61 -1 0 -2 85.38 1.56 1 0 2 87.48 1.71 1 0 2 83.23 1.60 -1 0 -2 87.20 1.76 0 -1 -2 827.86 14.48 0 1 2 857.79 14.57 0 -1 -2 852.68 14.60 0 1 2 833.77 15.29 1 -1 0 2.60 0.37 1 -1 0 2.54 0.41 -1 1 0 2.06 0.17 -1 1 0 1.98 0.25 1 1 -1 333.29 6.14 1 1 -1 317.51 6.31 -1 -1 1 317.60 5.30 -1 -1 1 320.95 5.14 0 1 -2 1726.83 32.29 0 -1 2 1688.44 31.40 0 -1 2 1656.58 32.94 0 1 -2 1658.72 33.55 -1 1 -1 7.33 0.34 1 -1 1 6.74 0.41 -1 1 -1 7.79 0.67 1 -1 1 8.00 0.46 1 0 -2 1083.99 19.52 -1 0 2 1024.75 18.32 1 0 -2 1052.71 18.37 -1 0 2 1073.75 19.29 1 -1 -1 316.64 5.39 1 -1 -1 313.62 5.71 1 1 2 1164.79 22.11 -1 -1 -2 1151.65 22.36 -1 -1 -2 1097.99 22.38 1 1 2 1173.16 21.90 0 0 -3 518.98 8.83 0 0 -3 605.69 8.75 0 0 -3 527.18 9.30 1 -1 2 493.01 7.71 1 -1 2 483.27 7.38 -1 1 -2 482.22 8.82 -1 1 -2 461.05 7.62 1 1 -2 7.39 0.55 -1 -1 2 8.05 0.54 -1 -1 2 8.36 0.44 1 1 -2 9.19 0.75 1 -1 -2 227.17 2.94 1 -1 -2 237.73 3.13 1 -1 -2 214.57 3.78 1 -1 -2 216.85 3.68 1 0 3 23.38 0.46 1 0 3 24.36 0.84 -1 0 -3 23.15 0.44 -1 0 -3 24.99 0.90 0 1 3 104.74 1.82 0 1 3 101.10 1.74 0 -1 -3 105.29 2.14 0 -1 -3 105.02 1.83 0 2 0 5432.91 140.06 0 -2 0 5223.36 133.91 0 2 0 5210.42 135.28 0 -2 0 5246.80 136.10 -2 0 0 1.07 0.30 2 0 0 1.67 0.39 -2 0 0 1.17 0.37 0 -2 -1 2164.27 46.66 0 -2 -1 2335.08 49.62 0 2 1 2165.41 46.74 -2 0 -1 415.14 7.00 -2 0 -1 416.68 6.95 2 0 1 417.37 7.58 2 0 1 406.96 6.71 0 1 -3 539.42 9.38 0 -1 3 532.57 9.30 0 -1 3 563.77 7.98 1 1 3 816.75 15.56 -1 -1 -3 817.20 14.89 1 1 3 832.18 15.22 -1 -1 -3 755.91 14.12 1 0 -3 223.37 3.79 1 0 -3 240.40 4.02 -1 0 3 212.37 3.72 -1 0 3 232.62 3.64 0 2 -1 1.98 0.36 0 2 -1 0.93 0.55 0 -2 1 2.14 0.35 0 -2 1 0.89 0.58 1 2 0 197.76 3.55 -1 -2 0 184.79 3.33 -1 -2 0 191.64 3.55 1 2 0 195.56 4.30 2 0 -1 134.68 2.52 -2 0 1 133.07 2.48 2 0 -1 134.06 2.14 -2 0 1 137.38 2.49 -2 -1 0 6.01 0.52 -2 -1 0 5.06 0.94 2 1 0 5.25 0.90 2 1 0 7.10 0.60 -1 -2 -1 9564.93 290.93 -1 -2 -1 9999.00 304.46 1 2 1 9548.74 290.94 -2 -1 -1 3.94 0.99 -2 -1 -1 7.20 0.81 2 1 1 5.85 0.56 2 1 1 5.48 0.58 -2 0 -2 180.42 2.98 2 0 2 178.72 3.11 2 0 2 182.90 3.44 -2 0 -2 185.64 3.81 0 2 2 514.65 9.29 0 2 2 535.72 9.56 0 -2 -2 538.61 9.68 0 -2 -2 554.87 10.47 -1 1 -3 1760.87 37.04 1 -1 3 1769.69 33.31 -1 1 -3 1788.25 36.68 1 -1 3 1755.25 33.17 1 2 -1 197.77 3.46 -1 -2 1 185.96 3.40 -1 -2 1 197.13 3.35 1 2 -1 191.99 3.56 1 -1 -3 2680.23 60.02 1 -1 -3 2710.74 57.44 1 -1 -3 2662.70 59.12 1 -1 -3 2501.85 53.94 2 1 -1 51.10 1.82 -2 -1 1 53.84 1.77 2 1 -1 53.05 1.29 -2 -1 1 51.58 1.63 0 0 -4 70.82 2.02 0 0 -4 67.95 1.78 0 0 -4 68.46 0.95 0 0 -4 71.04 1.10 -1 -1 3 172.03 3.02 1 1 -3 171.80 3.02 1 1 -3 183.86 3.06 -1 -1 3 176.68 2.67 -1 2 0 227.47 3.25 -1 2 0 221.58 4.29 1 -2 0 216.08 4.19 1 -2 0 218.80 3.30 1 2 2 15.33 0.76 1 2 2 15.96 1.22 -1 -2 -2 16.72 0.83 -1 -2 -2 14.52 0.79 -2 -1 -2 24.40 0.81 2 1 2 26.33 1.27 2 1 2 23.61 0.94 -2 -1 -2 26.40 1.00 -2 1 0 101.67 1.57 2 -1 0 102.10 2.04 2 -1 0 101.34 1.55 -2 1 0 108.13 2.52 0 2 -2 133.56 2.41 0 2 -2 138.35 2.21 0 -2 2 133.66 2.87 0 -2 2 135.78 2.54 -2 1 -1 480.77 8.39 2 -1 1 494.18 8.23 2 -1 1 475.04 8.38 -2 1 -1 514.73 8.56 -1 2 1 31.87 1.33 -1 2 1 30.59 0.66 1 -2 -1 28.87 0.92 1 -2 -1 31.41 0.58 -1 2 -1 262.90 4.77 1 -2 1 249.98 3.90 1 -2 1 247.54 4.16 -1 2 -1 252.78 4.24 -2 0 2 443.78 8.29 2 0 -2 453.76 7.36 -2 0 2 428.29 6.87 2 0 -2 452.39 7.94 1 0 4 64.65 1.04 1 0 4 72.11 2.08 -1 0 -4 75.46 1.68 -2 1 1 236.67 4.25 2 -1 -1 227.52 2.90 2 -1 -1 233.56 4.77 -2 1 1 240.31 3.08 0 -1 -4 7.14 0.37 0 -1 -4 6.02 0.48 0 1 4 6.64 0.59 0 1 4 4.99 0.45 1 1 4 5.57 0.52 -1 -1 -4 4.53 0.56 1 1 4 4.15 0.37 -1 -1 -4 3.52 0.60 2 0 3 4.71 0.36 -2 0 -3 4.20 0.35 2 0 3 4.06 0.79 -2 0 -3 4.09 0.53 -1 -2 2 2.29 0.37 1 2 -2 2.14 0.48 1 2 -2 2.52 0.39 -1 -2 2 2.14 0.43 0 -2 -3 78.04 1.72 0 2 3 82.56 1.52 0 -2 -3 83.89 1.98 0 2 3 78.71 1.72 2 -1 2 673.56 12.37 -2 1 -2 683.48 12.62 2 -1 2 682.67 12.17 -2 1 -2 688.18 12.53 -2 -1 2 819.74 15.06 -2 -1 2 787.01 14.52 2 1 -2 798.79 15.70 2 1 -2 835.00 15.41 0 1 -4 1.57 0.60 0 -1 4 0.83 0.62 0 1 -4 1.83 0.13 -1 2 2 36.84 0.55 -1 2 2 34.95 1.06 1 -2 -2 36.72 1.05 1 -2 -2 37.30 0.69 1 0 -4 561.69 9.73 -1 0 4 556.52 9.70 -1 0 4 536.65 9.74 1 0 -4 544.74 9.82 -2 -1 -3 40.78 1.05 2 1 3 43.72 1.25 2 1 3 40.11 1.52 -2 -1 -3 44.22 1.32 1 2 3 5.91 0.57 -1 -2 -3 6.13 0.63 1 2 3 5.33 0.87 -1 -2 -3 5.96 0.57 -1 2 -2 283.32 5.09 -1 2 -2 273.72 4.46 1 -2 2 279.06 4.53 1 -2 2 281.21 5.09 2 -1 -2 120.42 1.60 2 -1 -2 118.75 2.42 -2 1 2 114.63 1.43 -2 1 2 121.52 2.40 -2 -2 -1 1039.28 21.89 -2 -2 -1 1038.82 21.22 2 2 1 1062.41 21.84 2 2 0 53.13 2.16 2 2 0 52.59 2.02 -2 -2 0 56.15 2.17 -2 -2 0 54.13 1.90 -1 1 -4 124.62 2.35 -1 1 -4 138.26 2.75 1 -1 4 123.24 1.48 0 -2 3 34.30 0.94 0 2 -3 35.10 0.92 0 -2 3 29.75 1.39 0 2 -3 28.82 1.37 1 -1 -4 708.03 13.60 1 -1 -4 708.60 12.42 1 -1 -4 752.65 13.09 2 0 -3 245.77 3.96 -2 0 3 250.38 4.47 2 0 -3 250.84 4.48 -2 0 3 246.13 3.94 -1 -1 4 6.06 0.49 -1 -1 4 5.58 0.52 1 1 -4 6.98 0.46 1 1 -4 5.84 0.83 2 2 2 392.97 7.41 -2 -2 -2 410.56 7.96 -2 -2 -2 420.33 8.39 2 2 2 403.56 7.68 -2 -2 1 108.24 2.43 2 2 -1 101.63 2.79 2 2 -1 107.28 2.50 -2 -2 1 106.39 2.21 -2 1 -3 621.89 11.98 -2 1 -3 591.39 10.45 2 -1 3 610.00 11.79 2 -1 3 591.53 10.47 1 -2 -3 16.95 0.76 1 -2 -3 17.09 0.54 -1 2 3 16.50 0.52 -1 2 3 16.85 0.79 0 0 -5 23.53 0.83 0 0 -5 24.59 0.96 0 0 -5 26.02 0.61 0 0 -5 24.18 0.59 -1 -2 3 543.29 10.68 -1 -2 3 553.66 9.95 1 2 -3 535.24 10.00 1 2 -3 546.98 9.57 -2 -1 3 637.09 11.58 -2 -1 3 621.35 11.45 2 1 -3 641.19 12.06 2 1 -3 657.75 12.49 2 0 4 35.62 1.05 -2 0 -4 35.71 0.98 2 0 4 39.76 1.25 -2 0 -4 34.75 1.74 -1 2 -3 365.86 5.81 1 -2 3 377.63 7.18 1 -2 3 354.61 5.94 -1 2 -3 365.80 6.96 0 -2 -4 0.64 0.33 0 2 4 0.26 0.42 0 2 4 0.21 0.31 0 -2 -4 0.03 0.46 -1 0 -5 172.13 2.40 -1 0 -5 171.68 3.49 1 0 5 171.03 2.39 1 0 5 182.00 4.19 2 1 4 474.50 9.11 -2 -1 -4 495.54 9.53 -2 -1 -4 470.03 8.83 2 1 4 491.43 9.33 2 -1 -3 414.57 6.29 -2 1 3 422.60 6.33 2 -1 -3 411.39 7.73 -2 2 0 281.72 4.20 2 -2 0 302.56 6.27 2 -2 0 287.14 5.77 -2 2 0 282.23 3.92 -1 -2 -4 201.46 3.87 1 2 4 201.57 4.40 1 2 4 206.84 3.97 -1 -2 -4 202.35 3.99 0 1 5 21.25 0.61 0 -1 -5 21.09 1.22 0 -1 -5 20.56 0.61 0 1 5 19.32 0.81 0 3 0 7.26 0.97 0 3 0 10.56 0.68 0 -3 0 7.54 0.71 0 -3 0 8.29 0.53 0 -3 -1 276.58 4.90 0 3 1 259.98 4.71 0 3 1 261.59 5.73 0 -3 -1 270.09 5.18 -2 2 -1 1444.39 28.27 2 -2 1 1395.95 29.24 2 -2 1 1302.04 27.33 -2 2 -1 1493.83 28.26 2 2 3 391.55 7.63 -2 -2 -3 389.89 7.37 -2 -2 -3 405.52 9.00 2 2 3 397.94 7.63 -3 0 0 43.77 1.33 -3 0 0 42.11 1.11 3 0 0 38.85 1.28 -3 0 -1 17.86 1.20 -3 0 -1 17.87 0.83 3 0 1 16.74 0.71 3 0 1 17.44 0.85 -1 -1 -5 335.79 6.41 1 1 5 328.70 5.87 1 1 5 349.30 6.60 -1 -1 -5 322.85 5.41 2 -2 -1 112.00 2.49 2 -2 -1 111.17 2.87 2 2 -2 116.76 2.48 -2 -2 2 110.19 2.37 2 2 -2 116.12 2.69 -2 -2 2 112.95 2.82 1 3 1 1260.16 25.91 1 3 1 1239.84 25.70 -1 -3 -1 1242.45 25.72 -1 -3 -1 1255.61 25.97 -1 -3 0 4.18 0.98 1 3 0 4.27 1.07 1 3 0 4.18 0.65 -1 -3 0 4.06 0.65 3 1 1 92.41 2.23 -3 -1 -1 91.28 2.99 3 1 1 95.20 2.17 -3 -1 -1 97.16 2.71 0 3 -1 3.95 0.79 0 -3 1 4.00 0.56 0 3 -1 4.02 0.54 0 -3 1 3.01 0.72 -3 -1 0 176.11 4.12 3 1 0 184.53 3.69 3 1 0 179.88 3.67 -3 -1 0 180.06 4.37 0 1 -5 18.65 0.98 0 1 -5 17.75 0.27 0 1 -5 20.44 0.33 0 1 -5 20.76 0.87 3 0 -1 96.87 2.33 3 0 -1 99.24 2.23 -3 0 1 97.78 2.31 -3 0 1 99.42 2.21 0 -3 -2 124.90 2.40 0 3 2 123.13 2.43 0 3 2 122.14 2.70 0 -3 -2 126.11 3.46 1 0 -5 5139.24 133.25 1 0 -5 5069.89 135.87 1 0 -5 4917.45 129.52 1 0 -5 4981.25 128.35 -3 0 -2 25.49 1.44 3 0 2 26.21 0.93 -3 0 -2 26.18 1.37 3 0 2 24.86 0.97 0 2 -4 34.38 1.56 0 -2 4 36.39 0.83 0 -2 4 33.36 1.10 0 2 -4 37.55 0.84 1 3 2 180.62 4.52 1 3 2 173.42 3.67 -1 -3 -2 168.00 3.62 -1 -3 -2 182.69 3.86 2 -2 2 591.24 10.93 -2 2 -2 612.23 11.02 2 -2 2 600.36 10.86 -2 2 -2 607.87 10.58 -1 -3 1 396.28 7.48 -1 -3 1 406.14 7.70 1 3 -1 406.47 7.97 1 3 -1 409.12 8.48 -3 -1 -2 138.54 2.78 -3 -1 -2 136.32 3.06 3 1 2 136.75 2.87 3 1 2 130.62 2.83 -2 0 4 771.24 14.63 2 0 -4 794.51 15.52 2 0 -4 751.63 13.69 -2 0 4 765.47 13.91 2 -1 4 1774.73 39.33 2 -1 4 1938.96 39.33 -2 1 -4 1963.39 39.76 -2 1 -4 1819.03 40.20 2 -2 -2 10.62 0.71 2 -2 -2 11.75 0.79 3 1 -1 189.80 4.52 3 1 -1 193.76 3.85 -3 -1 1 194.07 4.41 -3 -1 1 180.22 4.31 -1 1 -5 2.55 0.57 -1 1 -5 2.83 0.47 1 -2 -4 28.99 1.49 -1 2 4 26.68 0.82 -1 2 4 28.53 1.44 1 -2 -4 29.57 0.86 -1 3 0 164.71 3.28 1 -3 0 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1.75 -5 -7 -7 3.60 2.30 5 7 7 1.71 1.55 5 7 7 4.84 1.52 6 0 -10 2.94 0.91 6 0 -10 2.98 1.31 6 0 -10 4.81 1.11 6 0 -10 4.29 1.32 -3 -7 7 5.17 1.48 -3 -7 7 4.11 1.06 3 7 -7 3.99 1.13 3 7 -7 6.10 1.87 -6 -7 -2 0.76 1.93 -6 -7 -2 -0.26 1.74 6 7 2 1.43 1.26 6 7 2 0.16 1.97 0 -2 -15 26.35 1.97 0 -2 -15 25.68 3.54 7 5 7 8.38 3.01 -7 -5 -7 7.97 2.74 7 5 7 8.17 1.94 -7 -5 -7 10.50 2.26 8 4 -1 19.99 2.45 -8 -4 1 16.40 3.37 -8 -4 1 18.46 2.08 8 4 -1 18.45 2.28 2 -4 -13 19.28 1.80 2 -4 -13 16.89 2.12 2 -4 -13 17.73 1.88 2 -4 -13 21.03 1.17 3 -5 -11 11.03 2.94 3 -5 -11 14.92 1.94 -2 -2 -15 69.90 3.33 -2 -2 -15 70.31 5.67 6 7 1 0.00 0.98 -6 -7 -1 0.37 1.37 -6 -7 -1 -0.23 0.86 6 7 1 0.44 0.97 -5 4 -10 5.31 1.37 -5 4 -10 0.00 1.79 7 6 2 -0.20 1.12 7 6 2 -0.48 1.75 -7 -6 -2 1.06 0.98 -7 -6 -2 0.24 1.13 -1 1 -15 51.37 4.96 -1 1 -15 48.75 4.30 -4 7 -4 1.70 1.18 4 -7 4 1.61 0.86 4 -7 4 0.73 1.56 -4 7 -4 1.79 0.75 -1 4 -13 7.94 1.90 -1 4 -13 9.14 1.75 0 7 10 7.23 1.67 0 -7 -10 8.14 2.93 0 7 10 9.10 1.66 0 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4.30 7 -2 -7 102.13 4.21 6 -5 -5 16.92 3.44 6 -5 -5 16.55 2.08 3 -3 -13 17.57 1.66 3 -3 -13 14.34 2.55 -7 0 8 14.06 1.91 7 0 -8 10.98 3.08 -5 -7 4 101.73 5.90 5 7 -4 94.02 4.43 5 7 -4 93.32 5.02 -5 -7 4 91.15 5.45 -3 2 -14 5.14 2.28 -3 2 -14 4.59 1.72 -8 2 -5 15.60 1.60 8 -2 5 16.41 1.77 8 -2 5 16.02 2.87 -2 -6 -12 144.60 5.64 2 6 12 132.01 6.19 2 6 12 136.36 6.59 -2 -6 -12 137.90 5.27 1 0 -15 52.08 3.15 1 0 -15 48.95 2.70 -2 -8 5 64.21 3.37 -2 -8 5 54.39 2.80 2 8 -5 64.55 4.02 2 8 -5 55.12 2.96 1 -1 -15 20.35 2.67 1 -1 -15 20.43 2.14 -4 -8 2 15.37 3.19 4 8 -2 16.39 2.64 4 8 -2 14.31 2.23 -4 -8 2 17.23 2.06 6 7 0 9.13 2.20 -6 -7 0 9.69 2.94 -6 -7 0 10.25 2.83 6 7 0 9.95 3.19 -7 -1 8 21.60 2.07 -7 -1 8 21.97 2.28 7 1 -8 20.43 2.32 7 1 -8 22.14 1.69 0 3 -14 201.60 6.78 0 3 -14 198.17 7.23 2 -8 -5 2.40 1.32 -2 8 5 -0.09 1.10 -4 -4 11 54.89 2.71 4 4 -11 55.80 5.14 4 4 -11 49.87 2.89 -4 -4 11 57.69 4.37 -8 -4 -5 0.87 1.87 -8 -4 -5 1.71 1.47 8 4 5 1.83 1.29 8 4 5 0.10 2.17 1 -8 5 11.28 1.58 -1 8 -5 13.79 1.95 1 -8 5 15.64 1.63 -1 8 -5 13.79 2.18 3 8 -4 20.34 2.17 3 8 -4 22.52 4.39 -3 -8 4 26.37 2.33 -3 -8 4 21.60 3.10 8 -2 -3 9.67 1.93 8 -2 -3 12.11 1.85 0 5 -12 4.17 1.46 0 5 -12 2.21 2.54 4 7 -6 51.02 5.69 -4 -7 6 58.79 3.33 -4 -7 6 49.92 3.71 4 7 -6 56.17 4.19 -1 3 -14 79.20 3.87 -1 3 -14 87.61 4.41 2 2 -14 38.45 3.90 2 2 -14 37.84 2.85 2 7 -8 2.38 0.78 -2 -7 8 1.58 0.75 2 7 -8 4.14 2.33 -2 -7 8 0.02 1.21 8 1 -5 74.66 5.69 -8 -1 5 72.41 5.51 -8 -1 5 75.49 2.61 8 1 -5 74.24 2.83 7 6 0 113.78 5.40 -7 -6 0 123.08 5.09 7 6 0 118.90 5.43 -7 -6 0 108.25 6.46 6 -1 -10 1.20 1.08 6 -1 -10 0.83 0.90 7 -4 5 2.99 0.95 7 -4 5 0.00 0.98 2 6 -10 13.34 2.03 -2 -6 10 0.03 2.60 -6 -4 -11 96.85 7.29 -6 -4 -11 90.62 3.66 6 4 11 88.00 3.76 6 4 11 87.65 4.43 -5 -3 -13 35.64 3.28 -5 -3 -13 31.99 1.72 5 3 13 31.45 2.52 5 3 13 35.92 2.90 4 -3 -12 39.18 2.39 4 -3 -12 34.94 3.53 5 -5 -8 4.11 2.48 5 -5 -8 4.37 2.37 -5 1 -13 89.15 3.91 -5 1 -13 82.14 4.44 1 4 -13 70.47 3.69 1 4 -13 65.20 4.01 8 0 -5 55.81 3.51 -8 0 5 61.94 3.62 7 4 9 2.27 1.30 -7 -4 -9 1.96 1.15 -7 -4 -9 2.07 2.62 7 4 9 2.15 1.41 3 -8 0 68.96 5.24 3 -8 0 71.67 5.38 -7 -5 4 5.83 1.60 7 5 -4 6.24 1.90 -7 -5 4 5.58 2.37 7 5 -4 4.83 1.79 3 -8 -1 49.69 4.81 3 -8 -1 57.77 3.46 -4 -7 -9 21.72 3.70 4 7 9 22.36 2.43 4 7 9 23.20 2.49 -4 -7 -9 22.31 4.21 4 6 11 9.73 1.91 -4 -6 -11 10.21 3.49 4 6 11 12.20 2.66 -4 -6 -11 11.21 1.81 4 -6 -8 0.94 1.93 4 -6 -8 1.16 1.24 -7 -3 7 9.29 2.60 -7 -3 7 8.96 1.45 7 3 -7 9.18 2.73 7 3 -7 10.59 1.88 4 0 -13 39.37 2.80 4 0 -13 41.05 2.15 4 0 -13 44.38 3.25 4 0 -13 38.87 1.87 -6 -7 -4 28.96 2.67 6 7 4 31.37 4.48 6 7 4 29.73 3.05 -6 -7 -4 28.94 3.05 -6 -6 -8 15.12 2.58 6 6 8 11.59 3.38 6 6 8 15.23 3.40 -6 -6 -8 12.95 2.04 3 8 7 18.85 2.28 -3 -8 -7 14.10 2.33 -3 -8 -7 14.21 3.39 3 8 7 16.41 2.02 -6 2 -11 0.26 2.11 -6 2 -11 11.61 2.52 3 5 13 16.81 2.07 -3 -5 -13 16.51 2.51 -3 -5 -13 16.34 1.74 3 5 13 14.42 2.17 7 -3 -6 26.13 2.54 7 -3 -6 24.25 2.34 7 6 4 -0.55 2.03 7 6 4 1.27 1.27 -7 -6 -4 0.63 1.33 -7 -6 -4 1.04 1.14 -6 5 -6 0.87 0.95 6 -5 6 1.33 1.17 -6 5 -6 0.15 1.09 6 -5 6 0.67 1.18 0 -6 -12 13.17 2.25 0 -6 -12 10.13 2.93 0 6 12 11.20 1.64 0 6 12 7.76 1.99 -3 5 -11 29.20 2.69 -3 5 -11 26.53 3.41 -2 8 -4 0.40 1.00 2 -8 4 3.67 1.10 2 -8 4 0.44 0.90 -2 8 -4 4.83 1.13 -4 5 -10 7.79 2.07 -4 5 -10 0.91 1.21 -3 -4 12 44.92 2.86 3 4 -12 38.31 3.29 -2 1 -15 28.32 4.37 -2 1 -15 33.82 3.71 -8 -3 -7 1.74 2.14 -8 -3 -7 -0.13 1.07 8 3 7 1.59 1.87 8 3 7 1.90 1.19 -2 6 -10 3.15 2.06 -2 6 -10 1.67 1.22 -1 5 -12 1.90 2.00 -1 5 -12 0.96 1.15 -7 -3 -10 -0.56 1.74 7 3 10 0.11 0.91 -7 -3 -10 -0.08 1.06 7 3 10 0.35 0.75 -3 -1 -15 73.35 4.20 -3 -1 -15 78.95 3.64 -4 1 -14 32.49 3.67 -4 1 -14 32.82 4.48 -7 2 -9 -0.10 1.83 -7 2 -9 0.33 1.44 7 -2 9 2.31 1.08 7 -2 9 1.85 1.17 4 -7 -5 19.12 2.48 4 -7 -5 22.43 3.80 -6 3 -10 -0.25 0.77 -6 3 -10 2.25 1.42 3 -8 1 19.02 3.44 3 -8 1 23.19 2.36 7 -4 -4 65.47 3.45 7 -4 -4 60.05 3.60 -3 -7 -10 24.97 2.54 3 7 10 24.30 2.41 -3 -7 -10 28.11 2.69 3 7 10 21.19 2.28 8 1 8 9.17 2.32 -8 -1 -8 -0.18 2.21 8 1 8 0.44 2.52 -8 -1 -8 19.30 2.98 3 -8 -2 22.51 2.54 3 -8 -2 19.43 2.43 -8 -4 2 3.75 1.31 -8 -4 2 4.14 1.44 8 4 -2 -0.10 1.50 8 4 -2 4.74 1.63 -4 -3 12 55.19 3.06 4 3 -12 60.08 3.52 -4 6 -8 -0.13 1.11 -4 6 -8 0.27 0.98 7 4 -6 84.30 4.21 7 4 -6 86.50 4.32 -7 -4 6 84.54 5.43 -7 -4 6 89.13 5.12 4 5 -10 3.94 3.75 -4 -5 10 16.45 3.11 4 5 -10 15.62 1.41 -4 -5 10 17.04 1.34 4 -1 -13 45.76 2.15 4 -1 -13 45.29 2.06 4 -1 -13 47.07 2.29 4 -1 -13 48.43 2.95 -6 -5 -10 4.57 1.44 6 5 10 5.29 1.52 6 5 10 5.41 1.72 -6 -5 -10 6.71 3.14 3 0 -14 15.38 1.58 3 0 -14 11.70 2.56 8 -3 1 2.56 1.35 8 -3 1 2.17 2.03 -5 -6 -10 8.14 1.78 5 6 10 7.66 3.02 5 6 10 10.34 1.84 -5 -6 -10 10.91 3.54 4 -5 -10 27.30 2.52 -1 -8 -8 0.25 1.95 1 8 8 6.08 1.82 1 8 8 6.72 2.45 -1 -8 -8 6.70 2.81 -8 1 -7 0.28 1.74 -8 1 -7 0.23 1.91 8 -1 7 5.33 1.11 8 -1 7 0.52 1.15 -5 -6 7 30.47 2.52 5 6 -7 23.89 3.47 -5 -6 7 25.45 2.04 5 6 -7 28.45 3.12 1 5 -12 21.19 2.27 1 5 -12 17.60 3.90 -4 -3 -14 25.95 2.96 4 3 14 24.60 2.67 -6 -7 1 3.58 2.17 -6 -7 1 2.50 1.40 6 7 -1 4.04 1.66 6 7 -1 1.10 1.57 7 -1 -8 10.62 1.94 7 -1 -8 11.15 1.72 -7 1 -10 0.44 0.61 7 -1 10 -0.48 0.63 -7 1 -10 -0.22 0.73 7 -1 10 0.14 0.68 8 -3 0 18.70 2.34 8 -3 0 23.75 3.37 5 -6 6 17.71 1.60 -5 6 -6 20.25 1.48 5 -6 6 18.10 1.56 -5 6 -6 19.19 1.57 2 -3 -14 42.07 3.12 2 -3 -14 44.60 1.95 2 -3 -14 42.03 2.22 2 -3 -14 42.49 2.27 -1 -3 -15 39.95 2.98 -1 -3 -15 39.38 3.36 3 4 14 11.11 1.22 -3 -4 -14 12.50 3.60 -3 -4 -14 9.34 2.03 3 4 14 17.07 2.09 -2 4 -13 0.75 1.05 -2 4 -13 0.52 1.21 8 -3 2 160.95 7.15 8 -3 2 145.11 7.25 8 3 -4 4.25 1.60 8 3 -4 -0.67 2.16 -8 -3 4 3.06 1.77 -8 -3 4 4.35 1.48 -5 -4 10 20.92 1.67 5 4 -10 24.88 3.88 5 4 -10 20.83 2.75 -5 -4 10 22.24 2.14 -3 0 -15 71.54 5.98 -3 0 -15 71.62 3.58 -1 8 7 2.78 2.57 1 -8 -7 8.02 1.94 4 1 -13 1.02 1.38 4 1 -13 0.08 0.94 4 1 -13 0.39 0.85 4 1 -13 0.56 0.53 -7 -6 1 9.56 1.90 -7 -6 1 10.98 1.92 7 6 -1 8.37 2.22 7 6 -1 10.46 2.22 -3 -5 11 -0.33 0.86 3 5 -11 0.02 1.05 3 -1 -14 6.25 1.64 3 -1 -14 3.05 0.84 3 -1 -14 2.95 1.48 3 -1 -14 2.95 0.84 6 5 -7 10.91 2.17 -6 -5 7 10.46 2.62 6 5 -7 8.02 2.79 -6 -5 7 7.69 1.56 1 3 -14 1.41 1.13 1 3 -14 0.57 1.25 1 1 -15 11.12 2.04 1 1 -15 11.88 1.76 -8 -2 -8 8.17 3.15 8 2 8 7.64 1.77 8 2 8 9.40 1.64 -8 -2 -8 -0.24 2.27 1 -2 -15 23.33 2.12 1 -2 -15 24.76 2.61 6 6 -5 77.86 4.46 6 6 -5 74.56 4.02 -6 -6 5 68.96 4.90 -6 -6 5 79.43 3.94 1 -5 -13 0.13 0.66 1 -5 -13 0.22 0.71 1 -5 -13 -0.48 1.18 1 -5 -13 0.06 0.57 -2 -8 -8 9.20 2.61 2 8 8 0.03 2.37 -2 -8 -8 10.88 2.06 2 8 8 10.52 1.87 -8 -2 5 2.72 0.87 -8 -2 5 2.44 1.37 8 2 -5 2.03 1.51 8 2 -5 2.49 1.74 -6 -2 10 1.42 1.50 -6 -2 10 2.22 1.12 6 2 -10 2.86 1.82 6 2 -10 2.11 1.20 6 3 12 28.92 2.83 -6 -3 -12 32.63 3.25 -6 -3 -12 28.68 2.71 6 3 12 28.30 2.71 4 8 6 0.00 1.76 -4 -8 -6 8.85 1.87 -4 -8 -6 7.64 2.75 4 8 6 6.93 1.80 -3 -2 -15 0.88 2.33 -3 -2 -15 1.75 1.17 -7 -2 8 0.17 1.59 7 2 -8 -0.85 1.48 7 2 -8 0.75 1.10 -7 -2 8 1.37 0.70 5 0 -12 71.76 3.73 5 0 -12 76.15 3.11 5 0 -12 71.74 2.93 5 0 -12 72.12 2.81 2 -7 -9 152.60 6.17 2 -7 -9 133.90 5.85 0 -8 6 10.28 1.66 0 -8 6 6.63 1.27 0 8 -6 8.41 1.25 0 8 -6 10.35 1.98 1 9 1 0.02 1.67 -1 -9 -1 0.81 0.87 1 9 1 0.31 1.03 -1 -9 -1 1.34 1.21 -2 3 -14 101.15 5.05 -2 3 -14 116.35 4.60 5 -6 -6 13.25 2.09 5 -6 -6 11.40 3.25 3 3 -13 64.50 3.48 3 3 -13 65.04 3.73 1 8 -6 9.70 1.97 -1 -8 6 -0.06 1.57 1 8 -6 9.28 1.86 -1 -8 6 6.71 1.19 -6 -7 -5 11.44 3.11 -6 -7 -5 12.12 3.63 6 7 5 10.53 3.44 6 7 5 10.95 2.30 4 -7 5 0.25 1.10 4 -7 5 0.68 1.16 -4 7 -5 0.30 0.66 -4 7 -5 0.15 1.03 2 -6 -11 27.86 2.67 2 -6 -11 31.04 2.77 6 -3 -9 66.92 3.68 -2 7 -8 3.67 2.02 -2 7 -8 3.08 2.16 -8 0 -8 2.13 1.28 -8 0 -8 0.52 1.12 8 0 8 0.51 0.96 8 0 8 0.00 0.78 6 -6 0 13.16 3.07 6 -6 0 13.89 3.04 3 -8 2 -0.58 0.94 3 -8 2 -0.12 1.54 -1 -9 -2 5.98 1.94 -1 -9 -2 8.32 1.42 1 9 2 4.95 2.52 1 9 2 8.04 2.63 7 6 5 8.26 1.96 -7 -6 -5 6.60 3.44 7 6 5 7.78 2.08 -7 -6 -5 6.72 1.81 3 -8 -3 13.64 3.29 8 4 6 5.03 1.67 -8 -4 -6 4.21 1.91 -8 -4 -6 5.45 2.33 8 4 6 3.39 1.74 8 -3 -1 27.21 3.98 -3 -6 -12 8.25 2.03 -3 -6 -12 8.10 2.46 3 6 12 6.26 1.46 6 -6 1 1.69 1.27 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 87670 _shelx_res_file ; TITL User-defined CIF.res created by SHELXL-2018/3 at 11:20:45 on 31-Jan-2025 REM Yadorkari-X generated CELL 0.71075 6.8860 6.9450 12.0366 85.5429 84.3712 83.9811 ZERR 1.0 0.0010 0.0010 0.0015 0.0046 0.0045 0.0049 LATT 1 REM SPGR P-1 triclinic SFAC C H Co N O UNIT 18 28 1 2 12 SIZE 0.25 0.25 0.10 TEMP -163.0 L.S. 50 FMAP 2 PLAN -50 ACTA CONF HTAB LIST 4 WPDB -1 BOND $H MERG 2 OMIT 0 8 4 OMIT 7 -1 9 OMIT 7 0 10 EQIV $1 1-X, 2-Y, 1-Z EQIV $2 2-X, 1-Y, 1-Z EQIV $3 1-X, 1-Y, 1-Z HTAB O3 O1 HTAB C7 O4_$1 HTAB O4 O6 HTAB O4 O2_$2 HTAB O5 O2_$3 HTAB O5 O6_$1 WGHT 0.045600 0.102900 FVAR 0.64961 CO1 3 0.500000 0.500000 0.500000 10.50000 0.01037 0.02391 = 0.00905 -0.00044 0.00171 -0.00095 O1 5 0.673056 0.467994 0.350202 11.00000 0.01309 0.03145 = 0.01116 -0.00105 0.00272 0.00025 O2 5 0.960076 0.333483 0.403628 11.00000 0.01251 0.03593 = 0.01311 0.00258 0.00079 -0.00047 O3 5 0.623847 0.543039 0.146355 11.00000 0.01058 0.03202 = 0.01020 -0.00151 0.00250 -0.00083 H3 2 0.597470 0.534912 0.211045 11.00000 0.03027 O4 5 0.665790 0.720054 0.535286 11.00000 0.01283 0.02690 = 0.01749 -0.00319 -0.00098 -0.00010 O5 5 0.305725 0.699994 0.415162 11.00000 0.01418 0.02767 = 0.01614 0.00242 0.00180 -0.00037 O6 5 0.502384 0.987235 0.682578 11.00000 0.02472 0.02755 = 0.02730 -0.00186 0.00601 -0.00202 N1 4 0.223278 1.017670 0.800101 11.00000 0.02681 0.02176 = 0.02315 -0.00236 0.00584 -0.00442 C1 1 0.856130 0.412091 0.330483 11.00000 0.01329 0.02064 = 0.01309 -0.00283 0.00177 -0.00458 C2 1 0.818609 0.500969 0.127071 11.00000 0.01115 0.01759 = 0.01392 -0.00360 0.00246 -0.00340 C3 1 0.940736 0.442281 0.211774 11.00000 0.01286 0.01725 = 0.01205 -0.00271 0.00228 -0.00234 C4 1 1.145405 0.408848 0.183531 11.00000 0.01333 0.02149 = 0.01337 -0.00089 -0.00078 -0.00242 AFIX 43 H4 2 1.229079 0.371976 0.241383 11.00000 -1.20000 AFIX 0 C5 1 1.225987 0.428198 0.075174 11.00000 0.01096 0.02173 = 0.01524 -0.00267 0.00095 -0.00173 AFIX 43 H5 2 1.363922 0.406279 0.058549 11.00000 -1.20000 AFIX 0 C6 1 1.102187 0.481312 -0.012500 11.00000 0.01222 0.01653 = 0.01279 -0.00291 0.00164 -0.00285 C7 1 0.321938 1.021675 0.700105 11.00000 0.02718 0.02524 = 0.02222 -0.00091 0.00213 -0.00489 AFIX 43 H7 2 0.249193 1.053293 0.636960 11.00000 -1.20000 AFIX 0 C8 1 0.011527 1.058688 0.814761 11.00000 0.02721 0.03036 = 0.04634 -0.00983 0.01305 -0.00848 AFIX 137 H8A 2 -0.039095 1.089840 0.741516 11.00000 -1.20000 H8B 2 -0.022584 1.169262 0.861194 11.00000 -1.20000 H8C 2 -0.046646 0.944645 0.851466 11.00000 -1.20000 AFIX 0 C9 1 0.325671 0.972550 0.900748 11.00000 0.05038 0.02907 = 0.02196 -0.00139 0.00235 0.00009 AFIX 137 H9A 2 0.299710 1.081591 0.948870 11.00000 -1.20000 H9B 2 0.466950 0.950019 0.879845 11.00000 -1.20000 H9C 2 0.279186 0.855710 0.941191 11.00000 -1.20000 AFIX 0 H1 2 0.619432 0.795450 0.574664 11.00000 0.03449 H2 2 0.768995 0.689586 0.556082 11.00000 0.02834 H6 2 0.214257 0.727666 0.458180 11.00000 0.05682 H10 2 0.351173 0.806380 0.392822 11.00000 0.03677 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM User-defined REM wR2 = 0.0743, GooF = S = 1.111, Restrained GooF = 1.111 for all data REM R1 = 0.0279 for 2413 Fo > 4sig(Fo) and 0.0303 for all 2595 data REM 173 parameters refined using 0 restraints END WGHT 0.0456 0.1029 REM Instructions for potential hydrogen bonds HTAB O3 O1 HTAB C7 O4_$1 HTAB O4 O6 HTAB O4 O2_$2 HTAB O5 O2_$3 HTAB O5 O6_$1 REM Highest difference peak 0.621, deepest hole -0.244, 1-sigma level 0.104 Q1 1 1.0000 0.5000 0.0000 10.50000 0.05 0.62 Q2 1 0.8370 0.5471 -0.0266 11.00000 0.05 0.57 Q3 1 0.4399 0.3950 0.4925 11.00000 0.05 0.54 Q4 1 0.9059 0.4263 0.2644 11.00000 0.05 0.51 Q5 1 0.8632 0.5033 0.0627 11.00000 0.05 0.50 Q6 1 1.0370 0.4238 0.2004 11.00000 0.05 0.49 Q7 1 0.8788 0.4834 0.1731 11.00000 0.05 0.47 Q8 1 0.2616 0.9848 0.8354 11.00000 0.05 0.45 Q9 1 0.1315 1.0316 0.8076 11.00000 0.05 0.43 Q10 1 0.5066 0.4611 0.5574 11.00000 0.05 0.42 Q11 1 0.7378 0.5343 0.1425 11.00000 0.05 0.41 Q12 1 0.2650 0.5564 0.6538 11.00000 0.05 0.39 Q13 1 0.3891 0.5147 0.5082 11.00000 0.05 0.38 Q14 1 0.4390 0.9817 0.6753 11.00000 0.05 0.38 Q15 1 0.2715 0.9872 0.7638 11.00000 0.05 0.37 Q16 1 0.2250 1.0741 0.7958 11.00000 0.05 0.35 Q17 1 1.1788 0.4106 0.1314 11.00000 0.05 0.34 Q18 1 0.3900 0.6504 0.4617 11.00000 0.05 0.33 Q19 1 0.6588 0.4972 0.2986 11.00000 0.05 0.31 Q20 1 1.0359 0.3111 0.4034 11.00000 0.05 0.31 Q21 1 0.5317 0.9065 0.7124 11.00000 0.05 0.30 Q22 1 0.9363 0.4135 0.3829 11.00000 0.05 0.30 Q23 1 -0.0635 0.9897 0.7983 11.00000 0.05 0.30 Q24 1 -0.0293 1.1123 0.8164 11.00000 0.05 0.27 Q25 1 0.5525 0.9353 0.6670 11.00000 0.05 0.27 Q26 1 0.9402 0.3120 0.4378 11.00000 0.05 0.27 Q27 1 1.2573 0.3812 0.0629 11.00000 0.05 0.25 Q28 1 0.6181 0.5595 0.0999 11.00000 0.05 0.24 Q29 1 1.1589 0.3660 0.2007 11.00000 0.05 0.23 Q30 1 0.6726 0.6404 0.1353 11.00000 0.05 0.22 Q31 1 0.1628 0.9819 0.8955 11.00000 0.05 0.22 Q32 1 0.2627 0.6019 0.4202 11.00000 0.05 0.21 Q33 1 0.3943 0.8584 0.8927 11.00000 0.05 0.21 Q34 1 0.1622 0.9403 1.0351 11.00000 0.05 0.20 Q35 1 0.1986 0.9420 0.9666 11.00000 0.05 0.20 Q36 1 0.1722 1.0758 0.6408 11.00000 0.05 0.18 Q37 1 0.3898 0.2707 0.5108 11.00000 0.05 0.18 Q38 1 0.0784 0.9986 1.0168 11.00000 0.05 0.18 Q39 1 0.6603 0.9580 0.5280 11.00000 0.05 0.17 Q40 1 0.5700 0.4380 0.1283 11.00000 0.05 0.16 Q41 1 0.7508 0.8468 0.5350 11.00000 0.05 0.15 Q42 1 1.2415 0.2769 0.2621 11.00000 0.05 0.15 Q43 1 -0.0271 1.0195 0.9217 11.00000 0.05 0.14 Q44 1 -0.0903 1.0671 0.9016 11.00000 0.05 0.14 Q45 1 0.6455 0.7846 0.7435 11.00000 0.05 0.13 Q46 1 0.2748 1.0768 0.6723 11.00000 0.05 0.13 Q47 1 0.3938 1.0756 0.9035 11.00000 0.05 0.13 Q48 1 0.4359 0.5640 0.2998 11.00000 0.05 0.13 Q49 1 0.5045 0.6026 0.2858 11.00000 0.05 0.12 Q50 1 0.0700 1.0540 0.6025 11.00000 0.05 0.11 ; _shelx_res_checksum 22031 loop_ _space_group_symop_operation_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 Co Co1 0.500000 0.500000 0.500000 0.01471(10) Uani d 1 . . O O1 0.67306(14) 0.46799(15) 0.35020(7) 0.0190(2) Uani d 1 . . O O2 0.96008(13) 0.33348(15) 0.40363(8) 0.0210(2) Uani d 1 . . O O3 0.62385(13) 0.54304(15) 0.14635(8) 0.0179(2) Uani d 1 . . H H3 0.597(3) 0.535(3) 0.2110(17) 0.030(5) Uiso d 1 . . O O4 0.66579(15) 0.72005(16) 0.53529(8) 0.0191(2) Uani d 1 . . O O5 0.30573(15) 0.69999(16) 0.41516(8) 0.0199(2) Uani d 1 . . O O6 0.50238(16) 0.98724(16) 0.68258(9) 0.0271(2) Uani d 1 . . N N1 0.22328(19) 1.01767(18) 0.80010(10) 0.0243(3) Uani d 1 . . C C1 0.85613(19) 0.41209(19) 0.33048(10) 0.0156(3) Uani d 1 . . C C2 0.81861(18) 0.50097(18) 0.12707(10) 0.0142(2) Uani d 1 . . C C3 0.94074(18) 0.44228(18) 0.21177(10) 0.0141(2) Uani d 1 . . C C4 1.14541(18) 0.40885(19) 0.18353(10) 0.0161(3) Uani d 1 . . H H4 1.229079 0.371976 0.241383 0.019 Uiso calc 1 . . C C5 1.22599(18) 0.42820(19) 0.07517(11) 0.0160(3) Uani d 1 . . H H5 1.363922 0.406279 0.058549 0.019 Uiso calc 1 . . C C6 1.10219(17) 0.48131(18) -0.01250(10) 0.0138(2) Uani d 1 . . C C7 0.3219(2) 1.0217(2) 0.70011(12) 0.0250(3) Uani d 1 . . H H7 0.249193 1.053293 0.636960 0.030 Uiso calc 1 . . C C8 0.0115(2) 1.0587(2) 0.81476(16) 0.0349(4) Uani d 1 . . H H8A -0.039095 1.089840 0.741516 0.042 Uiso calc 1 . . H H8B -0.022584 1.169262 0.861194 0.042 Uiso calc 1 . . H H8C -0.046646 0.944645 0.851466 0.042 Uiso calc 1 . . C C9 0.3257(3) 0.9726(2) 0.90075(13) 0.0345(4) Uani d 1 . . H H9A 0.299710 1.081591 0.948870 0.041 Uiso calc 1 . . H H9B 0.466950 0.950019 0.879845 0.041 Uiso calc 1 . . H H9C 0.279186 0.855710 0.941191 0.041 Uiso calc 1 . . H H1 0.619(3) 0.795(3) 0.5747(18) 0.034(6) Uiso d 1 . . H H2 0.769(3) 0.690(3) 0.5561(16) 0.028(5) Uiso d 1 . . H H6 0.214(4) 0.728(4) 0.458(2) 0.057(7) Uiso d 1 . . H H10 0.351(3) 0.806(3) 0.3928(17) 0.037(5) Uiso d 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 0.01037(14) 0.02391(15) 0.00905(13) -0.00095(9) 0.00171(8) -0.00044(9) O1 0.0131(4) 0.0315(5) 0.0112(4) 0.0002(4) 0.0027(3) -0.0011(4) O2 0.0125(4) 0.0359(6) 0.0131(4) -0.0005(4) 0.0008(3) 0.0026(4) O3 0.0106(4) 0.0320(5) 0.0102(4) -0.0008(4) 0.0025(3) -0.0015(4) O4 0.0128(5) 0.0269(5) 0.0175(5) -0.0001(4) -0.0010(4) -0.0032(4) O5 0.0142(5) 0.0277(5) 0.0161(5) -0.0004(4) 0.0018(4) 0.0024(4) O6 0.0247(5) 0.0275(5) 0.0273(6) -0.0020(4) 0.0060(4) -0.0019(4) N1 0.0268(7) 0.0218(6) 0.0231(6) -0.0044(5) 0.0058(5) -0.0024(5) C1 0.0133(6) 0.0206(6) 0.0131(6) -0.0046(5) 0.0018(4) -0.0028(5) C2 0.0112(6) 0.0176(6) 0.0139(6) -0.0034(4) 0.0025(4) -0.0036(5) C3 0.0129(6) 0.0172(6) 0.0121(6) -0.0023(5) 0.0023(4) -0.0027(4) C4 0.0133(6) 0.0215(6) 0.0134(6) -0.0024(5) -0.0008(4) -0.0009(5) C5 0.0110(6) 0.0217(6) 0.0152(6) -0.0017(5) 0.0009(4) -0.0027(5) C6 0.0122(6) 0.0165(6) 0.0128(6) -0.0028(5) 0.0016(4) -0.0029(5) C7 0.0272(8) 0.0252(7) 0.0222(7) -0.0049(6) 0.0021(6) -0.0009(6) C8 0.0272(8) 0.0304(8) 0.0463(10) -0.0085(7) 0.0131(7) -0.0098(7) C9 0.0504(11) 0.0291(8) 0.0220(8) 0.0001(7) 0.0024(7) -0.0014(6) 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 O1 Co1 O1 2_666 . 180.0 ? O1 Co1 O4 2_666 2_666 89.40(4) ? O1 Co1 O4 . 2_666 90.60(4) ? O1 Co1 O4 2_666 . 90.60(4) ? O1 Co1 O4 . . 89.40(4) ? O4 Co1 O4 2_666 . 180.0 ? O1 Co1 O5 2_666 . 91.09(4) ? O1 Co1 O5 . . 88.91(4) ? O4 Co1 O5 2_666 . 88.28(4) ? O4 Co1 O5 . . 91.72(4) ? O1 Co1 O5 2_666 2_666 88.91(4) ? O1 Co1 O5 . 2_666 91.09(4) ? O4 Co1 O5 2_666 2_666 91.72(4) ? O4 Co1 O5 . 2_666 88.28(4) ? O5 Co1 O5 . 2_666 180.00(8) ? C1 O1 Co1 . . 130.95(8) ? C2 O3 H3 . . 107.8(14) ? Co1 O4 H1 . . 118.7(16) ? Co1 O4 H2 . . 117.9(14) ? H1 O4 H2 . . 104(2) ? Co1 O5 H6 . . 107.4(18) ? Co1 O5 H10 . . 114.6(14) ? H6 O5 H10 . . 105(2) ? C7 N1 C8 . . 122.13(14) ? C7 N1 C9 . . 120.50(14) ? C8 N1 C9 . . 117.37(13) ? O2 C1 O1 . . 123.35(11) ? O2 C1 C3 . . 120.55(12) ? O1 C1 C3 . . 116.08(11) ? O3 C2 C3 . . 123.22(11) ? O3 C2 C6 . 2_765 116.24(11) ? C3 C2 C6 . 2_765 120.54(11) ? C2 C3 C4 . . 119.02(11) ? C2 C3 C1 . . 120.40(11) ? C4 C3 C1 . . 120.57(11) ? C5 C4 C3 . . 121.81(12) ? C5 C4 H4 . . 119.1 ? C3 C4 H4 . . 119.1 ? C4 C5 C6 . . 119.71(12) ? C4 C5 H5 . . 120.1 ? C6 C5 H5 . . 120.1 ? C6 C6 C5 2_765 . 120.13(14) ? C6 C6 C2 2_765 2_765 118.74(14) ? C5 C6 C2 . 2_765 121.14(11) ? O6 C7 N1 . . 124.91(14) ? O6 C7 H7 . . 117.5 ? N1 C7 H7 . . 117.5 ? N1 C8 H8A . . 109.5 ? N1 C8 H8B . . 109.5 ? H8A C8 H8B . . 109.5 ? N1 C8 H8C . . 109.5 ? H8A C8 H8C . . 109.5 ? H8B C8 H8C . . 109.5 ? N1 C9 H9A . . 109.5 ? N1 C9 H9B . . 109.5 ? H9A C9 H9B . . 109.5 ? N1 C9 H9C . . 109.5 ? H9A C9 H9C . . 109.5 ? H9B C9 H9C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 O1 2_666 2.0750(9) ? Co1 O1 . 2.0750(9) ? Co1 O4 2_666 2.0931(10) ? Co1 O4 . 2.0931(10) ? Co1 O5 . 2.1023(10) ? Co1 O5 2_666 2.1023(10) ? O1 C1 . 1.2842(16) ? O2 C1 . 1.2460(17) ? O3 C2 . 1.3436(15) ? O3 H3 . 0.78(2) ? O4 H1 . 0.76(2) ? O4 H2 . 0.78(2) ? O5 H6 . 0.79(3) ? O5 H10 . 0.85(2) ? O6 C7 . 1.2409(19) ? N1 C7 . 1.3226(19) ? N1 C8 . 1.452(2) ? N1 C9 . 1.458(2) ? C1 C3 . 1.4969(17) ? C2 C3 . 1.3945(18) ? C2 C6 2_765 1.4334(17) ? C3 C4 . 1.4161(17) ? C4 C5 . 1.3687(17) ? C4 H4 . 0.9500 ? C5 C6 . 1.4235(18) ? C5 H5 . 0.9500 ? C6 C6 2_765 1.411(2) ? C7 H7 . 0.9500 ? C8 H8A . 0.9800 ? C8 H8B . 0.9800 ? C8 H8C . 0.9800 ? C9 H9A . 0.9800 ? C9 H9B . 0.9800 ? C9 H9C . 0.9800 ? 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 O3 H3 O1 . 0.78(2) 1.81(2) 2.5168(13) 149.1(19) yes C7 H7 O4 2_676 0.95 2.56 3.2322(18) 127.7 no O4 H1 O6 . 0.76(2) 1.99(2) 2.7449(16) 178(2) yes O4 H2 O2 2_766 0.78(2) 1.96(2) 2.7284(15) 168(2) yes O5 H6 O2 2_666 0.79(3) 2.00(3) 2.7182(14) 151(2) yes O5 H10 O6 2_676 0.85(2) 1.95(2) 2.7836(15) 166(2) 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 O1 C1 O2 . . . . 12.6(2) ? Co1 O1 C1 C3 . . . . -168.77(8) ? O3 C2 C3 C4 . . . . -177.43(11) ? C6 C2 C3 C4 2_765 . . . 2.82(19) ? O3 C2 C3 C1 . . . . 3.5(2) ? C6 C2 C3 C1 2_765 . . . -176.22(11) ? O2 C1 C3 C2 . . . . 169.63(12) ? O1 C1 C3 C2 . . . . -9.05(18) ? O2 C1 C3 C4 . . . . -9.39(19) ? O1 C1 C3 C4 . . . . 171.94(11) ? C2 C3 C4 C5 . . . . -1.54(19) ? C1 C3 C4 C5 . . . . 177.49(12) ? C3 C4 C5 C6 . . . . -0.7(2) ? C4 C5 C6 C6 . . . 2_765 1.6(2) ? C4 C5 C6 C2 . . . 2_765 -178.74(12) ? C8 N1 C7 O6 . . . . -179.71(14) ? C9 N1 C7 O6 . . . . 0.7(2) ?