#------------------------------------------------------------------------------ #$Date: 2019-05-21 07:48:56 +0300 (Tue, 21 May 2019) $ #$Revision: 215347 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/16/2021637.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_2021637 loop_ _publ_author_name 'Han, Lizhi' 'Jin, Longyi' 'Wang, Enbo' 'Su, Zhongmin' _publ_section_title ; Synthesis and characterization of two isostructural 3d--4f coordination compounds based on pyridine-2,6-dicarboxylic acid and 4,4'-bipyridine ; _journal_coeditor_code LF3091 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first ; ; _journal_paper_doi 10.1107/S2053229619006004 _journal_volume 75 _journal_year 2019 _chemical_formula_iupac '(C10 H10 N2) [Co Tb2 (C7 H3 N O4)6 (C10 H9 N2)2 (H2 O)2], 8H2 O' _chemical_formula_moiety 'C10 H10 N2 2+, C62 H40 Co N10 O26 Tb2 2-, 16(H2 O)' _chemical_formula_sum 'C72 H82 Co N12 O42 Tb2' _chemical_formula_weight 2164.26 _chemical_name_systematic ;4,4'-Bipyridine-1,1'-diium diaquabis(\m~2~-pyridine-2,6-dicarboxylato)tetrakis(pyridine-2,6-dicarboxylato)bis[4-(pyridin-4-yl)pyridinium]cobalt(II)diterbium(III) octahydrate ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _cell_angle_alpha 98.5180(10) _cell_angle_beta 99.9010(10) _cell_angle_gamma 102.7150(10) _cell_formula_units_Z 1 _cell_length_a 11.8977(6) _cell_length_b 12.6490(6) _cell_length_c 14.8487(8) _cell_measurement_reflns_used 9945 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 25.000 _cell_measurement_theta_min 1.953 _cell_volume 2106.78(19) _computing_cell_refinement ; APEX2 (Bruker, 2005) ; _computing_data_collection ; APEX2 (Bruker, 2005) ; _computing_data_reduction ; SAINT (Bruker, 2006) ; _computing_molecular_graphics ; SHELXTL (Sheldrick, 2008) ; _computing_publication_material ; SHELXTL (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 296.02 _diffrn_detector 'charge-coupled device (CCD) area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART CCD APEXII' _diffrn_measurement_method '0.5\% \w and 0.5\% \f scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0172 _diffrn_reflns_av_unetI/netI 0.0308 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 12081 _diffrn_reflns_theta_full 24.999 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 1.682 _diffrn_source 'microfocus sealed X-ray tube' _exptl_absorpt_coefficient_mu 1.960 _exptl_absorpt_correction_T_max 0.695 _exptl_absorpt_correction_T_min 0.619 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour pink _exptl_crystal_density_diffrn 1.706 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1091 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _refine_diff_density_max 1.097 _refine_diff_density_min -0.741 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 583 _refine_ls_number_reflns 7395 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.079 _refine_ls_R_factor_all 0.0281 _refine_ls_R_factor_gt 0.0261 _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^)+(0.0388P)^2^+2.5060P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0708 _refine_ls_wR_factor_ref 0.0722 _reflns_number_gt 6962 _reflns_number_total 7395 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file lf3091sup1.cif _cod_data_source_block Tb _cod_database_code 2021637 _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 0.651 _shelx_estimated_absorpt_t_max 0.695 _shelx_hkl_file ; -1 0 0 176.53 4.42 1 0 0 141.77 4.32 -2 0 0 92.91 2.58 2 0 0 96.26 2.56 -3 0 0 27.44 0.84 3 0 0 27.80 0.79 -4 0 0 6.30 0.31 4 0 0 7.00 0.25 -5 0 0 117.46 3.69 -5 0 0 148.34 3.78 5 0 0 140.42 3.68 -6 0 0 89.92 2.67 -6 0 0 100.90 2.76 6 0 0 96.66 2.65 -7 0 0 77.47 2.24 -7 0 0 79.48 2.33 7 0 0 79.07 2.21 -8 0 0 11.63 0.55 -8 0 0 10.96 0.47 8 0 0 10.87 0.44 -9 0 0 20.33 0.82 -9 0 0 19.20 0.73 9 0 0 20.95 0.71 -10 0 0 0.26 0.14 -10 0 0 0.62 0.22 -11 0 0 0.01 0.16 -11 0 0 -0.04 0.10 -12 0 0 25.77 1.06 -13 0 0 20.52 0.94 -14 0 0 11.93 0.70 -15 0 0 1.64 0.31 -15 1 0 4.16 0.48 -14 1 0 1.71 0.33 -13 1 0 1.44 0.28 -12 1 0 41.70 1.39 -12 1 0 43.72 1.54 -11 1 0 23.74 0.86 -11 1 0 24.36 0.98 -10 1 0 39.59 1.37 -10 1 0 50.52 1.56 9 -1 0 21.54 0.73 -9 1 0 23.16 0.91 8 -1 0 56.11 1.62 -8 1 0 56.23 1.77 7 -1 0 10.28 0.39 -7 1 0 11.31 0.53 6 -1 0 8.12 0.30 -6 1 0 7.85 0.41 5 -1 0 113.41 3.07 -5 1 0 112.52 3.18 4 -1 0 176.87 4.88 -4 1 0 178.97 4.88 -3 1 0 95.70 2.71 -3 1 0 99.56 2.64 -2 1 0 0.95 0.06 -2 1 0 1.35 0.12 -1 1 0 41.21 1.14 -1 1 0 42.70 1.16 0 -1 0 133.61 3.68 0 1 0 132.39 3.65 -1 -1 0 167.83 4.65 -1 -1 0 174.66 4.70 1 1 0 167.03 4.67 -2 -1 0 259.14 7.03 -2 -1 0 248.65 6.90 -3 -1 0 7.18 0.28 -3 -1 0 7.17 0.28 -4 -1 0 25.57 0.79 -4 -1 0 26.40 0.82 4 1 0 26.25 0.78 -5 -1 0 13.80 0.49 -5 -1 0 13.77 0.52 5 1 0 13.61 0.48 -6 -1 0 4.38 0.29 -6 -1 0 4.35 0.26 6 1 0 4.21 0.25 -7 -1 0 56.51 1.71 -7 -1 0 57.03 1.67 7 1 0 54.97 1.64 -8 -1 0 72.00 2.11 -8 -1 0 71.72 2.17 8 1 0 71.64 2.08 -9 -1 0 57.47 1.81 -9 -1 0 56.85 1.74 9 1 0 56.90 1.71 -10 -1 0 59.69 1.90 -10 -1 0 60.64 1.84 10 1 0 58.33 1.79 -11 -1 0 36.81 1.27 -11 -1 0 38.81 1.36 -12 -1 0 0.28 0.20 -12 -1 0 -0.07 0.16 -13 -1 0 0.03 0.17 -13 -1 0 0.24 0.21 -14 -1 0 14.39 0.77 -15 2 0 10.26 0.69 -14 2 0 10.53 0.67 -13 2 0 9.74 0.64 -12 2 0 0.43 0.16 -12 2 0 1.11 0.29 -11 2 0 -0.14 0.12 -11 2 0 -0.29 0.19 -10 2 0 19.80 0.73 -10 2 0 20.95 0.89 9 -2 0 12.93 0.47 -9 2 0 12.46 0.50 -9 2 0 13.19 0.64 8 -2 0 123.07 3.40 -8 2 0 123.63 3.58 -8 2 0 124.18 3.44 7 -2 0 1.52 0.14 -7 2 0 1.20 0.21 -7 2 0 1.63 0.15 6 -2 0 22.08 0.67 -6 2 0 22.45 0.81 -5 2 0 83.20 2.41 -5 2 0 83.89 2.29 -4 2 0 149.89 4.13 -4 2 0 149.46 4.03 -2 2 0 34.61 1.00 -2 2 0 34.12 0.96 -1 2 0 121.84 3.30 0 -2 0 33.61 0.93 0 2 0 32.89 0.94 0 2 0 33.17 0.91 -1 -2 0 35.25 1.04 1 2 0 37.68 1.05 -2 -2 0 0.25 0.08 -2 -2 0 0.04 0.05 2 2 0 0.08 0.09 -3 -2 0 11.78 0.43 -3 -2 0 12.54 0.41 3 2 0 12.39 0.43 -4 -2 0 204.68 5.50 -4 -2 0 200.82 5.51 -5 -2 0 216.05 5.93 -5 -2 0 219.62 5.94 -6 -2 0 132.82 3.67 -6 -2 0 131.92 3.67 6 2 0 129.59 3.65 -7 -2 0 28.65 0.94 -7 -2 0 28.38 0.95 7 2 0 26.90 0.92 -8 -2 0 12.23 0.54 -8 -2 0 11.83 0.54 8 2 0 12.08 0.52 -9 -2 0 11.43 0.54 -9 -2 0 11.39 0.56 9 2 0 11.52 0.52 -10 -2 0 37.13 1.25 -10 -2 0 36.97 1.28 10 2 0 35.72 1.21 -11 -2 0 63.00 2.00 -11 -2 0 65.81 2.06 -12 -2 0 11.16 0.62 -12 -2 0 10.42 0.57 -13 -2 0 12.77 0.66 -13 -2 0 12.61 0.67 -15 3 0 1.16 0.33 -14 3 0 5.33 0.49 -13 3 0 18.41 0.89 -12 3 0 18.99 0.77 -12 3 0 19.09 0.89 -11 3 0 53.19 1.63 -11 3 0 54.36 1.82 -10 3 0 9.26 0.42 -10 3 0 9.16 0.57 9 -3 0 32.13 0.97 -9 3 0 31.47 1.00 -9 3 0 31.78 1.17 8 -3 0 24.09 0.73 -8 3 0 22.35 0.90 7 -3 0 32.61 0.97 -7 3 0 33.22 1.14 -6 3 0 127.03 3.57 -6 3 0 123.63 3.41 -5 3 0 49.70 1.39 -5 3 0 48.93 1.50 -4 3 0 171.89 4.68 -4 3 0 175.42 4.77 -3 3 0 71.64 1.98 -3 3 0 72.46 2.04 -2 3 0 13.01 0.45 -2 3 0 13.41 0.42 -1 3 0 21.83 0.66 0 -3 0 1.37 0.13 0 3 0 1.08 0.08 0 3 0 0.95 0.12 -1 -3 0 135.82 3.77 1 3 0 140.65 3.79 -2 -3 0 151.81 4.24 -2 -3 0 156.71 4.19 2 3 0 158.01 4.25 -3 -3 0 0.52 0.07 -3 -3 0 0.70 0.11 3 3 0 0.85 0.14 -4 -3 0 13.68 0.51 -4 -3 0 13.66 0.47 4 3 0 13.97 0.51 -5 -3 0 44.61 1.34 -5 -3 0 43.84 1.30 5 3 0 44.09 1.34 -6 -3 0 105.65 2.97 -6 -3 0 105.25 3.00 -7 -3 0 41.99 1.30 -7 -3 0 40.88 1.32 -8 -3 0 52.96 1.63 -8 -3 0 51.87 1.61 8 3 0 51.10 1.61 -9 -3 0 1.06 0.20 -9 -3 0 1.25 0.24 9 3 0 1.24 0.23 -10 -3 0 8.90 0.49 -10 -3 0 8.71 0.49 10 3 0 8.32 0.50 -11 -3 0 9.66 0.56 -11 -3 0 9.35 0.53 -12 -3 0 0.75 0.22 -12 -3 0 0.76 0.22 -13 -3 0 8.42 0.56 -15 4 0 7.41 0.60 -14 4 0 4.57 0.51 -13 4 0 0.01 0.21 -12 4 0 0.32 0.22 -11 4 0 46.48 1.61 -11 4 0 43.53 1.38 -10 4 0 12.54 0.67 -10 4 0 12.29 0.50 9 -4 0 65.66 1.84 -9 4 0 62.91 2.05 -8 4 0 34.85 1.25 -8 4 0 36.12 1.06 -7 4 0 0.54 0.10 -7 4 0 0.16 0.18 -6 4 0 129.48 3.67 -6 4 0 128.66 3.53 -5 4 0 6.85 0.27 -5 4 0 6.19 0.36 -4 4 0 153.83 4.19 -4 4 0 155.44 4.27 -3 4 0 129.34 3.61 -3 4 0 136.25 3.67 -2 4 0 11.24 0.42 -2 4 0 13.57 0.43 -1 4 0 60.30 1.72 -1 4 0 61.93 1.70 0 -4 0 4.96 0.24 0 4 0 5.05 0.19 0 4 0 4.91 0.25 -1 -4 0 104.98 2.94 1 4 0 107.58 2.96 -2 -4 0 128.06 3.53 2 4 0 127.75 3.54 -3 -4 0 55.68 1.52 -3 -4 0 52.97 1.59 3 4 0 53.79 1.60 -4 -4 0 90.40 2.55 -4 -4 0 87.87 2.47 4 4 0 89.83 2.56 -5 -4 0 94.14 2.66 -5 -4 0 91.95 2.58 5 4 0 90.94 2.65 -6 -4 0 0.15 0.10 -6 -4 0 0.12 0.14 6 4 0 0.11 0.15 -7 -4 0 5.03 0.36 -7 -4 0 5.01 0.30 7 4 0 5.16 0.36 -8 -4 0 29.41 1.04 -8 -4 0 27.50 0.96 -9 -4 0 6.37 0.43 -9 -4 0 6.15 0.38 9 4 0 6.54 0.43 -10 -4 0 13.41 0.66 -10 -4 0 12.63 0.59 10 4 0 12.22 0.63 -11 -4 0 5.49 0.43 -12 -4 0 8.99 0.58 -13 -4 0 0.25 0.22 -15 5 0 4.37 0.52 -14 5 0 17.64 0.93 -13 5 0 11.14 0.69 -12 5 0 16.30 0.83 -11 5 0 -0.01 0.21 -11 5 0 0.14 0.12 -10 5 0 1.16 0.28 -9 5 0 14.39 0.51 -9 5 0 13.35 0.70 -8 5 0 55.36 1.59 -8 5 0 54.64 1.79 -7 5 0 129.58 3.70 -7 5 0 127.30 3.53 -6 5 0 66.52 2.00 -6 5 0 65.55 1.87 -5 5 0 72.25 2.03 -5 5 0 72.41 2.13 -4 5 0 8.71 0.41 -4 5 0 8.24 0.33 -3 5 0 7.23 0.30 -3 5 0 7.61 0.33 -2 5 0 55.45 1.59 -1 5 0 114.44 3.07 -1 5 0 109.44 3.10 0 -5 0 150.72 4.11 0 5 0 149.54 4.13 0 5 0 149.65 4.06 -1 -5 0 106.49 2.92 1 5 0 101.85 2.92 -2 -5 0 52.60 1.57 2 5 0 53.70 1.59 -3 -5 0 5.79 0.32 3 5 0 5.81 0.35 -4 -5 0 1.26 0.18 4 5 0 1.08 0.20 -5 -5 0 55.12 1.58 -5 -5 0 55.27 1.68 5 5 0 53.04 1.67 -6 -5 0 30.06 0.94 -6 -5 0 29.72 1.04 6 5 0 29.46 1.04 -7 -5 0 101.14 2.95 -7 -5 0 100.56 2.84 7 5 0 98.45 2.93 -8 -5 0 3.34 0.36 -8 -5 0 3.44 0.27 8 5 0 3.36 0.34 -9 -5 0 18.42 0.77 9 5 0 13.73 0.68 -10 -5 0 0.09 0.18 10 5 0 0.24 0.19 -11 -5 0 5.86 0.46 -12 -5 0 32.31 1.26 -13 -5 0 4.64 0.47 -15 6 0 2.11 0.40 -14 6 0 1.05 0.31 -13 6 0 0.28 0.24 -12 6 0 12.57 0.73 -11 6 0 14.54 0.77 -10 6 0 15.86 0.79 -9 6 0 0.17 0.24 -9 6 0 0.09 0.10 -8 6 0 5.64 0.29 -8 6 0 5.75 0.45 -7 6 0 2.67 0.20 -7 6 0 2.59 0.33 -6 6 0 18.52 0.72 -6 6 0 17.09 0.59 -5 6 0 55.33 1.62 -5 6 0 57.67 1.73 -4 6 0 133.14 3.72 -4 6 0 137.52 3.79 -3 6 0 123.33 3.50 -3 6 0 128.58 3.48 -2 6 0 18.27 0.64 -2 6 0 19.64 0.64 -1 6 0 3.54 0.25 -1 6 0 3.73 0.20 0 6 0 30.59 0.88 0 6 0 28.76 0.96 -1 -6 0 52.35 1.58 1 6 0 54.63 1.61 1 6 0 52.52 1.49 -2 -6 0 278.56 7.61 2 6 0 280.29 7.64 -3 -6 0 72.05 2.13 3 6 0 72.96 2.15 -4 -6 0 29.02 1.01 4 6 0 30.04 1.04 -5 -6 0 1.76 0.26 5 6 0 1.33 0.24 -6 -6 0 6.10 0.31 -6 -6 0 6.75 0.45 6 6 0 5.92 0.45 -7 -6 0 7.56 0.44 -7 -6 0 7.65 0.47 7 6 0 8.17 0.51 -8 -6 0 19.78 0.83 8 6 0 19.98 0.84 -9 -6 0 21.40 0.91 9 6 0 20.64 0.89 -10 -6 0 9.12 0.58 10 6 0 8.52 0.55 -11 -6 0 5.57 0.50 -12 -6 0 0.26 0.25 -15 7 0 11.89 0.79 -14 7 0 7.95 0.63 -13 7 0 5.51 0.53 -12 7 0 0.87 0.31 -11 7 0 -0.04 0.20 -10 7 0 41.98 1.53 -9 7 0 44.88 1.58 -9 7 0 43.94 1.41 -8 7 0 5.08 0.47 -8 7 0 4.95 0.28 -7 7 0 13.77 0.52 -7 7 0 13.89 0.66 -6 7 0 26.64 0.86 -6 7 0 26.06 0.96 -5 7 0 5.02 0.36 -5 7 0 4.74 0.27 -4 7 0 10.11 0.42 -4 7 0 9.98 0.46 -3 7 0 150.75 4.17 -2 7 0 49.09 1.49 -2 7 0 49.69 1.46 -1 7 0 104.23 2.94 -1 7 0 102.53 2.86 0 7 0 21.32 0.66 0 7 0 20.52 0.76 -1 -7 0 31.20 1.00 1 7 0 30.26 0.89 1 7 0 29.27 1.02 -2 -7 0 36.45 1.19 2 7 0 37.67 1.23 -3 -7 0 19.71 0.76 3 7 0 20.71 0.79 -4 -7 0 110.69 3.22 4 7 0 112.10 3.24 -5 -7 0 8.44 0.48 5 7 0 7.82 0.49 -6 -7 0 116.18 3.32 6 7 0 109.76 3.31 -7 -7 0 13.43 0.67 7 7 0 12.59 0.66 -8 -7 0 4.39 0.42 8 7 0 4.95 0.45 -9 -7 0 5.38 0.45 9 7 0 4.82 0.45 -10 -7 0 15.95 0.78 10 7 0 14.10 0.74 -11 -7 0 20.51 0.97 -12 -7 0 11.12 0.71 -15 8 0 1.31 0.36 -14 8 0 2.51 0.43 -13 8 0 14.13 0.86 -12 8 0 5.94 0.54 -11 8 0 23.41 1.05 -10 8 0 3.61 0.44 -9 8 0 0.83 0.30 -8 8 0 25.14 1.03 -8 8 0 24.41 0.83 -7 8 0 22.41 0.77 -7 8 0 22.96 0.93 -6 8 0 77.24 2.21 -6 8 0 75.83 2.31 -5 8 0 22.94 0.86 -5 8 0 22.92 0.79 -4 8 0 106.21 3.04 -4 8 0 106.09 3.00 -3 8 0 3.70 0.27 -3 8 0 3.62 0.28 -2 8 0 4.12 0.29 -2 8 0 4.40 0.27 -1 8 0 14.46 0.60 -1 8 0 13.55 0.50 0 8 0 23.69 0.75 0 8 0 24.66 0.87 -1 -8 0 63.19 1.92 1 8 0 64.78 1.80 1 8 0 63.52 1.94 -2 -8 0 21.30 0.80 2 8 0 20.84 0.66 2 8 0 21.59 0.83 -3 -8 0 48.15 1.57 3 8 0 51.04 1.62 -4 -8 0 4.32 0.39 4 8 0 3.16 0.35 -5 -8 0 5.06 0.43 5 8 0 4.76 0.41 -6 -8 0 11.52 0.60 6 8 0 11.37 0.63 -7 -8 0 20.90 0.89 7 8 0 20.85 0.89 -8 -8 0 40.25 1.43 8 8 0 37.64 1.40 -9 -8 0 9.90 0.64 9 8 0 10.32 0.64 -10 -8 0 -0.11 0.22 10 8 0 -0.05 0.22 -11 -8 0 0.86 0.32 -14 9 0 4.64 0.56 -13 9 0 0.27 0.27 -12 9 0 1.98 0.41 -11 9 0 8.29 0.62 -10 9 0 16.65 0.86 -9 9 0 50.51 1.76 -8 9 0 10.15 0.63 -8 9 0 10.43 0.47 -7 9 0 1.93 0.22 -7 9 0 2.16 0.31 -6 9 0 20.04 0.73 -6 9 0 19.70 0.83 -5 9 0 9.92 0.46 -5 9 0 9.74 0.52 -4 9 0 114.23 3.25 -3 9 0 34.34 1.10 -3 9 0 32.70 1.11 -2 9 0 37.91 1.18 -2 9 0 38.17 1.24 -1 9 0 1.50 0.23 -1 9 0 1.70 0.18 0 9 0 1.76 0.27 0 9 0 1.99 0.18 1 9 0 30.61 1.10 1 9 0 31.36 0.94 -2 -9 0 24.78 0.92 2 9 0 24.89 0.96 -3 -9 0 162.70 4.64 3 9 0 164.43 4.67 -4 -9 0 48.71 1.61 4 9 0 48.33 1.64 -5 -9 0 37.06 1.32 5 9 0 37.00 1.35 -6 -9 0 0.22 0.22 6 9 0 -0.02 0.20 -7 -9 0 2.00 0.32 7 9 0 2.15 0.35 -8 -9 0 23.91 1.04 8 9 0 23.20 1.03 -9 -9 0 9.02 0.64 9 9 0 8.40 0.60 -10 -9 0 16.94 0.89 10 9 0 14.78 0.81 -14 10 0 10.15 0.79 -13 10 0 3.99 0.54 -12 10 0 12.94 0.82 -11 10 0 -0.07 0.23 -10 10 0 0.52 0.27 -9 10 0 21.45 0.97 -8 10 0 31.67 1.07 -8 10 0 32.56 1.25 -7 10 0 61.36 1.86 -7 10 0 61.29 1.98 -6 10 0 39.29 1.26 -6 10 0 37.45 1.32 -5 10 0 28.15 0.99 -5 10 0 28.53 1.04 -4 10 0 6.05 0.38 -4 10 0 5.78 0.40 -3 10 0 2.80 0.28 -3 10 0 3.62 0.33 -2 10 0 36.67 1.17 -2 10 0 37.25 1.26 -1 10 0 28.85 0.93 -1 10 0 28.59 1.03 0 10 0 75.06 2.30 1 10 0 64.82 2.05 2 10 0 3.36 0.35 -3 -10 0 0.43 0.19 3 10 0 0.43 0.22 -4 -10 0 9.91 0.58 4 10 0 10.97 0.63 -5 -10 0 33.59 1.25 5 10 0 32.42 1.25 -6 -10 0 19.18 0.87 6 10 0 17.72 0.84 -7 -10 0 19.11 0.88 7 10 0 18.19 0.88 -8 -10 0 1.41 0.33 8 10 0 1.44 0.32 -9 -10 0 -0.22 0.24 9 10 0 0.24 0.25 -13 11 0 1.34 0.37 -12 11 0 12.33 0.79 -11 11 0 9.00 0.67 -10 11 0 14.21 0.81 -9 11 0 0.77 0.28 -8 11 0 0.21 0.23 -8 11 0 0.07 0.14 -7 11 0 2.54 0.36 -7 11 0 2.52 0.28 -6 11 0 4.58 0.41 -6 11 0 4.81 0.35 -5 11 0 47.63 1.53 -4 11 0 18.69 0.76 -4 11 0 18.34 0.76 -3 11 0 15.65 0.66 -3 11 0 16.01 0.69 -2 11 0 0.13 0.18 -2 11 0 0.03 0.15 -1 11 0 1.53 0.26 0 11 0 57.50 1.86 1 11 0 33.77 1.24 2 11 0 92.48 2.83 3 11 0 3.91 0.41 -4 -11 0 3.95 0.40 4 11 0 3.98 0.43 -5 -11 0 0.16 0.20 5 11 0 0.44 0.25 -6 -11 0 0.30 0.22 6 11 0 0.18 0.22 -7 -11 0 21.88 0.99 7 11 0 21.66 1.00 -8 -11 0 11.39 0.72 8 11 0 12.18 0.74 -13 12 0 2.41 0.46 -12 12 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9 -2 -17 3.89 0.49 -8 2 17 4.11 0.51 -7 2 17 0.31 0.25 -6 2 17 0.22 0.23 -5 2 17 14.03 0.81 -4 2 17 5.03 0.51 -3 2 17 25.23 1.10 -2 2 17 4.67 0.49 -1 2 17 5.30 0.48 0 2 17 0.93 0.26 -1 -2 -17 3.43 0.36 -2 -2 -17 19.67 0.86 -3 -2 -17 12.90 0.69 -9 3 17 2.56 0.44 -8 3 17 14.54 0.86 -7 3 17 2.06 0.40 -6 3 17 7.91 0.61 -5 3 17 0.11 0.25 -4 3 17 0.41 0.23 -3 3 17 11.85 0.72 -2 3 17 5.45 0.55 -1 3 17 24.47 1.10 0 3 17 5.31 0.49 -1 -3 -17 10.48 0.59 -2 -3 -17 -0.41 0.17 -9 4 17 3.69 0.50 -8 4 17 3.11 0.47 -7 4 17 0.42 0.27 -6 4 17 15.89 0.88 -5 4 17 14.20 0.85 -4 4 17 12.60 0.77 -3 4 17 0.08 0.20 -2 4 17 2.19 0.38 -1 4 17 1.05 0.28 0 4 17 4.75 0.52 -8 5 17 4.26 0.52 -7 5 17 3.32 0.48 -6 5 17 0.53 0.30 -5 5 17 1.52 0.37 -4 5 17 21.26 1.07 -3 5 17 7.44 0.63 -2 5 17 18.46 0.98 -1 5 17 11.54 0.76 0 5 17 5.08 0.54 -6 6 17 10.81 0.78 -5 6 17 13.90 0.87 -4 6 17 2.47 0.44 -3 6 17 0.07 0.25 -2 6 17 4.19 0.53 2 9 -18 6.32 0.55 1 9 -18 15.48 0.87 0 9 -18 2.45 0.41 4 8 -18 18.96 0.92 3 8 -18 4.30 0.48 2 8 -18 0.93 0.29 1 8 -18 7.63 0.63 0 8 -18 12.59 0.77 -1 8 -18 11.24 0.73 -2 8 -18 6.32 0.57 6 7 -18 0.03 0.27 5 7 -18 3.54 0.44 4 7 -18 20.14 0.96 3 7 -18 11.01 0.68 2 7 -18 27.37 1.13 0 7 -18 1.91 0.37 -1 7 -18 6.17 0.57 -2 7 -18 2.50 0.39 -3 7 -18 19.87 0.99 6 6 -18 11.59 0.72 5 6 -18 13.58 0.78 4 6 -18 0.07 0.23 3 6 -18 2.44 0.35 2 6 -18 6.95 0.52 0 6 -18 17.95 0.89 -1 6 -18 3.49 0.45 -2 6 -18 4.50 0.51 -3 6 -18 2.90 0.43 7 5 -18 4.38 0.52 6 5 -18 3.59 0.46 5 5 -18 29.98 1.25 4 5 -18 17.04 0.87 3 5 -18 18.74 0.90 2 5 -18 -0.43 0.16 0 5 -18 9.58 0.62 -1 5 -18 6.22 0.55 -2 5 -18 27.29 1.16 -3 5 -18 3.58 0.45 -4 5 -18 2.59 0.38 8 4 -18 25.61 1.19 7 4 -18 5.49 0.58 6 4 -18 1.49 0.33 5 4 -18 -0.01 0.19 4 4 -18 1.97 0.35 3 4 -18 14.27 0.77 2 4 -18 9.50 0.60 1 4 -18 17.60 0.92 0 4 -18 0.84 0.25 -1 4 -18 1.03 0.29 -2 4 -18 7.12 0.55 -3 4 -18 7.33 0.57 -4 4 -18 14.43 0.78 8 3 -18 10.93 0.76 7 3 -18 18.08 0.95 6 3 -18 23.49 1.08 5 3 -18 8.03 0.60 4 3 -18 14.92 0.80 3 3 -18 0.48 0.22 2 3 -18 -0.28 0.16 1 3 -18 15.83 0.77 0 3 -18 8.15 0.54 -1 3 -18 18.67 0.88 -2 3 -18 12.61 0.71 8 2 -18 11.89 0.75 7 2 -18 0.30 0.27 6 2 -18 5.00 0.54 5 2 -18 8.42 0.59 4 2 -18 21.33 0.98 3 2 -18 4.79 0.44 2 2 -18 19.75 0.91 1 2 -18 2.18 0.34 0 2 -18 1.02 0.26 -1 2 -18 7.02 0.52 -3 2 -18 13.65 0.71 9 1 -18 8.13 0.64 8 1 -18 11.63 0.77 7 1 -18 23.66 1.09 6 1 -18 6.93 0.59 5 1 -18 0.88 0.28 4 1 -18 2.58 0.39 3 1 -18 1.50 0.31 2 1 -18 21.12 0.95 1 1 -18 23.11 0.99 0 1 -18 16.33 0.72 -1 1 -18 2.06 0.29 -2 1 -18 2.74 0.33 -3 1 -18 0.89 0.26 9 0 -18 0.09 0.24 8 0 -18 0.06 0.24 7 0 -18 4.10 0.51 6 0 -18 7.03 0.56 5 0 -18 17.83 0.89 4 0 -18 8.74 0.61 3 0 -18 6.81 0.52 -3 0 18 7.97 0.58 -2 0 18 0.06 0.22 -1 0 18 1.91 0.33 -1 0 -18 4.83 0.41 -2 0 -18 15.73 0.75 8 -1 -18 11.15 0.73 7 -1 -18 2.48 0.40 6 -1 -18 3.52 0.45 -6 1 18 2.38 0.42 -5 1 18 1.93 0.38 -4 1 18 6.76 0.58 -3 1 18 26.33 1.15 -2 1 18 11.74 0.71 -1 1 18 10.58 0.65 -1 -1 -18 0.25 0.19 -2 -1 -18 2.41 0.33 8 -2 -18 8.88 0.68 -8 2 18 10.00 0.74 -7 2 18 3.86 0.51 -6 2 18 13.89 0.82 -5 2 18 4.87 0.54 -4 2 18 6.34 0.61 -3 2 18 0.44 0.24 -2 2 18 0.35 0.25 -1 2 18 10.46 0.68 -7 3 18 -0.01 0.23 -6 3 18 4.47 0.54 -5 3 18 5.00 0.54 -4 3 18 15.79 0.88 -3 3 18 2.72 0.43 -2 3 18 11.14 0.73 -1 3 18 3.18 0.45 -6 4 18 4.07 0.53 -5 4 18 1.72 0.38 -4 4 18 3.35 0.46 -3 4 18 2.12 0.40 -2 4 18 13.36 0.82 1 7 -19 3.60 0.48 4 6 -19 3.54 0.44 3 6 -19 25.91 1.11 1 6 -19 2.46 0.38 0 6 -19 0.92 0.28 -1 6 -19 0.79 0.29 5 5 -19 1.16 0.32 4 5 -19 1.06 0.31 3 5 -19 2.75 0.41 2 5 -19 8.44 0.59 1 5 -19 14.41 0.79 0 5 -19 10.18 0.68 -1 5 -19 8.25 0.63 6 4 -19 23.19 1.08 5 4 -19 8.86 0.62 4 4 -19 9.35 0.65 3 4 -19 3.28 0.43 2 4 -19 3.05 0.40 0 4 -19 4.31 0.48 -1 4 -19 22.20 1.02 6 3 -19 0.77 0.28 5 3 -19 0.73 0.28 4 3 -19 4.83 0.51 3 3 -19 6.11 0.50 2 3 -19 16.10 0.81 0 3 -19 6.37 0.52 -1 3 -19 0.48 0.25 7 2 -19 11.09 0.73 6 2 -19 9.59 0.66 5 2 -19 14.36 0.81 4 2 -19 3.23 0.42 3 2 -19 2.26 0.38 2 2 -19 4.65 0.48 0 2 -19 26.78 1.13 7 1 -19 -0.06 0.25 6 1 -19 2.10 0.40 5 1 -19 11.55 0.71 4 1 -19 12.28 0.72 3 1 -19 20.83 0.97 2 1 -19 0.89 0.26 -1 1 -19 1.94 0.31 6 0 -19 7.73 0.62 5 0 -19 -0.09 0.23 4 0 -19 0.29 0.24 3 0 -19 22.33 1.03 2 0 -19 12.85 0.72 -2 0 19 12.07 0.73 6 -1 -19 12.07 0.76 5 -1 -19 4.23 0.50 -5 1 19 4.32 0.53 -4 1 19 13.11 0.78 -3 1 19 2.03 0.37 -2 1 19 -0.01 0.21 -5 2 19 0.67 0.28 -4 2 19 8.30 0.65 -3 2 19 5.73 0.53 -2 2 19 11.59 0.74 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 28706 _shelx_res_file ; TITL 1 in P1 New: P-1 1.res created by SHELXL-2018/1 at 15:47:03 on 16-Oct-2018 CELL 0.71073 11.8977 12.649 14.8487 98.518 99.901 102.715 ZERR 1 0.0006 0.0006 0.0008 0.001 0.001 0.001 LATT 1 SFAC C H Co N O Tb UNIT 72 80 1 12 42 2 ISOR 0.008 0.005 O21 O20 L.S. 10 PLAN -20 SIZE 0.2 0.22 0.24 TEMP 23 BOND $H CONF fmap 2 acta OMIT -3 50 OMIT -5 -1 1 OMIT -12 -1 1 OMIT 1 0 11 OMIT -5 8 2 OMIT 5 5 7 OMIT -8 -2 2 OMIT 1 1 8 OMIT 0 -1 3 REM REM REM WGHT 0.038800 2.506000 FVAR 0.11573 TB1 6 0.423335 0.194219 0.284851 11.00000 0.02200 0.02243 = 0.02108 0.00609 0.00463 0.00114 CO1 3 0.000000 0.000000 0.000000 10.50000 0.02187 0.02499 = 0.02038 0.00652 0.00200 -0.00148 O1 5 0.303152 -0.079923 0.437432 11.00000 0.07298 0.03271 = 0.05696 0.01910 0.01781 -0.00871 O2 5 0.339042 0.021030 0.328833 11.00000 0.04036 0.02537 = 0.03604 0.00786 0.00978 -0.00366 O3 5 0.542211 0.362405 0.383967 11.00000 0.04631 0.02600 = 0.02390 0.00786 0.00557 -0.00733 O4 5 0.635078 0.466710 0.522586 11.00000 0.05713 0.03542 = 0.02549 0.00242 0.00617 -0.01616 O5 5 0.530512 0.280065 0.177498 11.00000 0.03667 0.03538 = 0.03400 0.01519 0.01531 0.00939 O6 5 0.556270 0.395894 0.079016 11.00000 0.07696 0.05475 = 0.05931 0.03206 0.04283 0.01969 O7 5 0.254416 0.236979 0.336469 11.00000 0.03926 0.03861 = 0.03755 0.01297 0.01779 0.01135 O8 5 0.115334 0.330108 0.338105 11.00000 0.04233 0.05844 = 0.05491 0.00914 0.02124 0.02138 O9 5 0.610710 0.148982 0.318793 11.00000 0.02742 0.04746 = 0.02909 0.00591 -0.00272 0.00667 O10 5 0.740179 0.054322 0.284712 11.00000 0.02795 0.08974 = 0.06070 0.01703 -0.00015 0.02461 O11 5 0.259876 0.108099 0.151182 11.00000 0.02386 0.03447 = 0.03119 -0.00083 -0.00258 0.00615 O12 5 0.167410 -0.029335 0.031108 11.00000 0.02681 0.03639 = 0.02814 -0.00099 -0.00279 0.00115 O13 5 0.043631 0.145374 0.101682 11.00000 0.02704 0.03733 = 0.03037 0.00196 0.00419 0.00335 AFIX 3 H13A 2 0.112061 0.138884 0.129372 11.00000 -1.20000 H13B 2 -0.001399 0.136994 0.140152 11.00000 -1.20000 AFIX 0 N1 4 0.456607 0.196025 0.455957 11.00000 0.02675 0.02598 = 0.02588 0.01081 0.00909 0.00059 N2 4 0.348901 0.345185 0.220000 11.00000 0.03312 0.02499 = 0.02534 0.00509 0.00660 0.00672 N3 4 0.451547 0.038787 0.171232 11.00000 0.02161 0.02609 = 0.02411 0.00799 0.00458 0.00433 N4 4 -0.061576 -0.099716 0.095653 11.00000 0.03324 0.03186 = 0.02851 0.01079 0.00854 0.00304 N5 4 -0.280529 -0.407777 0.412246 11.00000 0.05740 0.03495 = 0.03532 0.01416 0.01949 0.00016 AFIX 43 H5 2 -0.308311 -0.446271 0.451917 11.00000 -1.20000 AFIX 0 C1 1 0.409187 0.106272 0.487419 11.00000 0.03153 0.03128 = 0.03300 0.01602 0.01005 0.00311 C2 1 0.421642 0.105747 0.581433 11.00000 0.05342 0.04894 = 0.04037 0.02748 0.01542 0.00308 AFIX 43 H2 2 0.387105 0.041194 0.602293 11.00000 -1.20000 AFIX 0 C3 1 0.485015 0.200323 0.644992 11.00000 0.06297 0.05930 = 0.02367 0.01805 0.00732 -0.00123 AFIX 43 H3 2 0.493955 0.201837 0.710026 11.00000 -1.20000 AFIX 0 C4 1 0.535465 0.293200 0.612227 11.00000 0.04786 0.04664 = 0.02800 0.00916 0.00603 -0.00551 AFIX 43 H4 2 0.580582 0.358932 0.654172 11.00000 -1.20000 AFIX 0 C5 1 0.518080 0.287136 0.516856 11.00000 0.02887 0.03119 = 0.02594 0.00903 0.00504 0.00061 C6 1 0.343889 0.006636 0.411785 11.00000 0.03792 0.02669 = 0.04296 0.01408 0.01330 0.00173 C7 1 0.568875 0.381047 0.471837 11.00000 0.03265 0.02776 = 0.02787 0.00748 0.00794 -0.00289 C8 1 0.255139 0.373816 0.244243 11.00000 0.03742 0.03451 = 0.03114 0.00344 0.00670 0.01194 C9 1 0.206896 0.450574 0.205580 11.00000 0.06522 0.05904 = 0.05826 0.02291 0.02129 0.03899 AFIX 43 H9 2 0.138753 0.468220 0.222421 11.00000 -1.20000 AFIX 0 C10 1 0.259632 0.501385 0.141803 11.00000 0.09443 0.07605 = 0.07331 0.04368 0.02963 0.05656 AFIX 43 H10 2 0.228604 0.555493 0.115153 11.00000 -1.20000 AFIX 0 C11 1 0.357434 0.473455 0.116851 11.00000 0.07904 0.04706 = 0.04932 0.02687 0.02358 0.02675 AFIX 43 H11 2 0.394792 0.507624 0.073177 11.00000 -1.20000 AFIX 0 C12 1 0.399536 0.393714 0.157673 11.00000 0.04454 0.03157 = 0.02548 0.00665 0.00912 0.00724 C13 1 0.203305 0.309447 0.311869 11.00000 0.03152 0.03369 = 0.03205 0.00074 0.00733 0.00483 C14 1 0.504479 0.354102 0.135719 11.00000 0.04386 0.02939 = 0.02937 0.00740 0.01322 0.00368 C15 1 0.553670 0.009988 0.184190 11.00000 0.02768 0.03701 = 0.03316 0.01383 0.01041 0.01185 C16 1 0.572904 -0.076153 0.125020 11.00000 0.04268 0.04987 = 0.05772 0.00321 0.01285 0.02504 AFIX 43 H16 2 0.646342 -0.095201 0.135324 11.00000 -1.20000 AFIX 0 C17 1 0.483134 -0.134130 0.050472 11.00000 0.05856 0.05165 = 0.06903 -0.01451 0.01670 0.02314 AFIX 43 H17 2 0.494243 -0.193741 0.008811 11.00000 -1.20000 AFIX 0 C18 1 0.377591 -0.104882 0.037047 11.00000 0.04338 0.04528 = 0.03970 -0.00840 0.00464 0.00871 AFIX 43 H18 2 0.314906 -0.143880 -0.013728 11.00000 -1.20000 AFIX 0 C19 1 0.364641 -0.017430 0.099078 11.00000 0.02735 0.02652 = 0.02457 0.00419 0.00500 0.00179 C20 1 0.643025 0.077162 0.269025 11.00000 0.02387 0.04535 = 0.03757 0.02205 0.00697 0.00918 C21 1 0.255321 0.023379 0.093117 11.00000 0.02416 0.02762 = 0.02240 0.00661 0.00317 -0.00086 C22 1 -0.161098 -0.181883 0.068550 11.00000 0.03449 0.03834 = 0.02741 0.01039 0.00388 -0.00009 AFIX 43 H22 2 -0.201163 -0.197433 0.005118 11.00000 -1.20000 AFIX 0 C23 1 -0.207597 -0.244225 0.127657 11.00000 0.03519 0.03486 = 0.03363 0.00970 0.01027 0.00195 C24 1 -0.150332 -0.222872 0.220885 11.00000 0.04138 0.02620 = 0.02800 0.00895 0.01412 0.00497 C25 1 -0.046916 -0.138819 0.248772 11.00000 0.05006 0.03168 = 0.02841 0.00955 0.00706 0.00151 AFIX 43 H25 2 -0.004681 -0.121671 0.311672 11.00000 -1.20000 AFIX 0 C26 1 -0.006353 -0.080856 0.184770 11.00000 0.03825 0.03461 = 0.03141 0.01175 0.00489 -0.00401 AFIX 43 H26 2 0.064873 -0.024267 0.205018 11.00000 -1.20000 AFIX 0 C27 1 -0.303115 -0.454300 0.322200 11.00000 0.06437 0.03492 = 0.03706 0.00618 0.01424 -0.01026 AFIX 43 H27 2 -0.348243 -0.528682 0.301809 11.00000 -1.20000 AFIX 0 C28 1 -0.261998 -0.396046 0.259039 11.00000 0.06347 0.03352 = 0.03305 0.00337 0.01477 -0.00869 AFIX 43 H28 2 -0.278249 -0.429995 0.195108 11.00000 -1.20000 AFIX 0 C29 1 -0.196285 -0.286924 0.288438 11.00000 0.04387 0.02783 = 0.03174 0.01015 0.01332 0.00366 C30 1 -0.174197 -0.241693 0.382133 11.00000 0.06997 0.02871 = 0.03449 0.00371 0.01902 -0.00659 AFIX 43 H30 2 -0.129651 -0.167428 0.404820 11.00000 -1.20000 AFIX 0 C31 1 -0.217327 -0.305180 0.442698 11.00000 0.07861 0.03706 = 0.03004 0.00379 0.02122 -0.00266 AFIX 43 H31 2 -0.201137 -0.274341 0.507321 11.00000 -1.20000 AFIX 0 O14 5 0.098017 -0.281575 0.044697 11.00000 0.12663 0.07043 = 0.07970 0.03253 0.05083 0.04398 AFIX 3 H14A 2 0.116437 -0.213805 0.040797 11.00000 -1.20000 H14B 2 0.135537 -0.315845 0.011857 11.00000 -1.20000 AFIX 0 O15 5 -0.026859 -0.428301 0.142120 11.00000 0.08846 0.07832 = 0.07294 0.00964 -0.00006 0.00141 AFIX 3 H15A 2 -0.001699 -0.391451 0.103010 11.00000 -1.20000 H15B 2 -0.074529 -0.485151 0.106580 11.00000 -1.20000 AFIX 0 O16 5 0.113730 0.063946 0.410204 11.00000 0.05232 0.06226 = 0.08413 0.01884 0.02518 0.00955 AFIX 3 H16A 2 0.147210 0.118596 0.388944 11.00000 -1.20000 H16B 2 0.047870 0.073066 0.419984 11.00000 -1.20000 AFIX 0 O17 5 0.782741 0.330671 0.224718 11.00000 0.08218 0.12318 = 0.12447 0.04167 0.01227 0.01090 AFIX 3 H17A 2 0.716051 0.287611 0.222498 11.00000 -1.20000 H17B 2 0.836442 0.299961 0.244288 11.00000 -1.20000 AFIX 0 O18 5 0.099668 -0.068821 0.549909 11.00000 0.05119 0.12038 = 0.07745 0.04737 0.01825 0.02588 AFIX 3 H18A 2 0.156228 -0.054501 0.597069 11.00000 -1.20000 H18B 2 0.116178 -0.023131 0.514639 11.00000 -1.20000 AFIX 0 O19 5 0.230700 -0.214679 0.241513 11.00000 0.09860 0.06034 = 0.06267 0.01965 0.00186 -0.00911 AFIX 3 H19A 2 0.258830 -0.145549 0.260723 11.00000 -1.20000 H19B 2 0.195050 -0.225979 0.184873 11.00000 -1.20000 AFIX 0 O20 5 -0.083159 0.189607 0.230372 11.00000 0.05996 0.12366 = 0.08825 -0.01472 0.03980 -0.01112 AFIX 3 H20A 2 -0.018969 0.228677 0.265742 11.00000 -1.20000 H20B 2 -0.115609 0.141927 0.258932 11.00000 -1.20000 AFIX 0 O21 5 0.219301 -0.384700 -0.067841 11.00000 0.08251 0.11943 = 0.13096 -0.02169 0.04548 0.00745 AFIX 3 H21A 2 0.203271 -0.365840 -0.120251 11.00000 -1.20000 H21B 2 0.289451 -0.392080 -0.059731 11.00000 -1.20000 AFIX 0 N6 4 0.163630 -0.285266 0.416846 11.00000 0.03814 0.03178 = 0.05749 0.02086 0.01582 0.00217 AFIX 43 H6 2 0.204206 -0.230605 0.396025 11.00000 -1.20000 AFIX 0 C32 1 0.081896 -0.364335 0.356977 11.00000 0.05361 0.04189 = 0.03960 0.01599 0.01447 0.00661 AFIX 43 H32 2 0.067971 -0.361643 0.292512 11.00000 -1.20000 AFIX 0 C33 1 0.016677 -0.450862 0.387884 11.00000 0.04766 0.02989 = 0.03267 0.00558 0.00513 -0.00106 AFIX 43 H33 2 -0.040926 -0.508214 0.344446 11.00000 -1.20000 AFIX 0 C34 1 0.034975 -0.454343 0.482168 11.00000 0.02912 0.02324 = 0.03276 0.00721 0.00643 0.00505 C35 1 0.122713 -0.369764 0.541627 11.00000 0.04489 0.03152 = 0.03852 0.00886 0.00085 -0.00597 AFIX 43 H35 2 0.138985 -0.369819 0.606536 11.00000 -1.20000 AFIX 0 C36 1 0.186349 -0.285895 0.507643 11.00000 0.04099 0.03079 = 0.06002 0.01007 0.00109 -0.00740 AFIX 43 H36 2 0.246423 -0.228507 0.548911 11.00000 -1.20000 AFIX 0 HKLF 4 REM 1 in P1 New: P-1 REM R1 = 0.0264 for 6962 Fo > 4sig(Fo) and 0.0285 for all 7395 data REM 583 parameters refined using 12 restraints END WGHT 0.0373 2.7029 REM Highest difference peak 1.097, deepest hole -0.762, 1-sigma level 0.089 Q1 1 0.9002 0.2452 0.2027 11.00000 0.05 0.86 Q2 1 -0.2781 -0.3033 0.1000 11.00000 0.05 0.76 Q3 1 0.9207 0.1602 0.2344 11.00000 0.05 0.54 Q4 1 0.2391 -0.0452 0.4332 11.00000 0.05 0.41 Q5 1 0.4466 0.1420 0.2142 11.00000 0.05 0.40 Q6 1 0.3819 0.2369 0.3378 11.00000 0.05 0.40 Q7 1 0.0601 -0.2688 -0.0150 11.00000 0.05 0.31 Q8 1 0.4969 0.2938 0.5554 11.00000 0.05 0.27 Q9 1 0.0143 -0.3364 0.0223 11.00000 0.05 0.27 Q10 1 0.4658 0.6521 0.0831 11.00000 0.05 0.27 Q11 1 -0.1202 -0.1271 0.0869 11.00000 0.05 0.27 Q12 1 0.0550 -0.3396 -0.0368 11.00000 0.05 0.27 Q13 1 -0.1259 -0.2821 0.5312 11.00000 0.05 0.27 Q14 1 0.7465 0.0788 0.2319 11.00000 0.05 0.27 Q15 1 -0.0476 0.0396 0.0526 11.00000 0.05 0.27 Q16 1 0.5393 0.1469 0.4065 11.00000 0.05 0.27 Q17 1 0.3379 0.1825 0.2784 11.00000 0.05 0.26 Q18 1 0.2802 0.2950 0.4382 11.00000 0.05 0.26 Q19 1 -0.1792 -0.2356 0.1001 11.00000 0.05 0.26 Q20 1 0.2797 0.3400 0.2189 11.00000 0.05 0.25 ; _shelx_res_checksum 42292 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 Tb Tb1 0.42334(2) 0.19422(2) 0.28485(2) 0.02235(6) Uani d 1 Co Co1 0.000000 0.000000 0.000000 0.02368(13) Uani d 1 O O1 0.3032(3) -0.0800(2) 0.4374(2) 0.0563(8) Uani d 1 O O2 0.3390(2) 0.02105(18) 0.32881(16) 0.0355(5) Uani d 1 O O3 0.5422(2) 0.36242(18) 0.38396(15) 0.0346(5) Uani d 1 O O4 0.6351(2) 0.4667(2) 0.52259(17) 0.0444(7) Uani d 1 O O5 0.5305(2) 0.28005(19) 0.17751(16) 0.0335(5) Uani d 1 O O6 0.5562(3) 0.3959(2) 0.0790(2) 0.0575(8) Uani d 1 O O7 0.2544(2) 0.2370(2) 0.33648(17) 0.0363(5) Uani d 1 O O8 0.1154(2) 0.3301(2) 0.3381(2) 0.0494(7) Uani d 1 O O9 0.6107(2) 0.1490(2) 0.31880(16) 0.0363(5) Uani d 1 O O10 0.7402(2) 0.0543(3) 0.2847(2) 0.0588(8) Uani d 1 O O11 0.25987(19) 0.10806(19) 0.15117(16) 0.0318(5) Uani d 1 O O12 0.16742(19) -0.02932(19) 0.03111(16) 0.0334(5) Uani d 1 O O13 0.0436(2) 0.14535(19) 0.10167(16) 0.0331(5) Uani d 1 H H13A 0.112049 0.138855 0.129362 0.040 Uiso d 1 H H13B -0.001411 0.136975 0.140142 0.040 Uiso d 1 N N1 0.4566(2) 0.1960(2) 0.45596(18) 0.0261(6) Uani d 1 N N2 0.3489(2) 0.3452(2) 0.22002(18) 0.0278(6) Uani d 1 N N3 0.4515(2) 0.0388(2) 0.17121(17) 0.0239(5) Uani d 1 N N4 -0.0616(2) -0.0997(2) 0.09566(19) 0.0313(6) Uani d 1 N N5 -0.2806(3) -0.4077(2) 0.4122(2) 0.0424(7) Uani d 1 H H5 -0.308337 -0.446231 0.451867 0.051 Uiso calc 1 C C1 0.4092(3) 0.1063(3) 0.4874(2) 0.0313(7) Uani d 1 C C2 0.4218(4) 0.1058(3) 0.5815(3) 0.0463(10) Uani d 1 H H2 0.387385 0.041218 0.602410 0.056 Uiso calc 1 C C3 0.4850(4) 0.2003(4) 0.6449(3) 0.0504(10) Uani d 1 H H3 0.493946 0.201863 0.709903 0.061 Uiso calc 1 C C4 0.5354(3) 0.2932(3) 0.6122(3) 0.0436(9) Uani d 1 H H4 0.580373 0.358912 0.654164 0.052 Uiso calc 1 C C5 0.5181(3) 0.2872(3) 0.5169(2) 0.0295(7) Uani d 1 C C6 0.3440(3) 0.0067(3) 0.4118(3) 0.0355(8) Uani d 1 C C7 0.5689(3) 0.3811(3) 0.4719(2) 0.0307(7) Uani d 1 C C8 0.2551(3) 0.3738(3) 0.2442(2) 0.0342(8) Uani d 1 C C9 0.2067(4) 0.4505(4) 0.2056(3) 0.0549(11) Uani d 1 H H9 0.138532 0.468075 0.222358 0.066 Uiso calc 1 C C10 0.2596(5) 0.5015(4) 0.1418(4) 0.0712(15) Uani d 1 H H10 0.228694 0.555651 0.115191 0.085 Uiso calc 1 C C11 0.3575(4) 0.4734(4) 0.1168(3) 0.0536(11) Uani d 1 H H11 0.394858 0.507557 0.073086 0.064 Uiso calc 1 C C12 0.3996(3) 0.3937(3) 0.1576(2) 0.0339(7) Uani d 1 C C13 0.2033(3) 0.3095(3) 0.3119(2) 0.0335(7) Uani d 1 C C14 0.5044(3) 0.3541(3) 0.1357(2) 0.0343(8) Uani d 1 C C15 0.5537(3) 0.0100(3) 0.1842(2) 0.0308(7) Uani d 1 C C16 0.5729(4) -0.0762(3) 0.1250(3) 0.0485(10) Uani d 1 H H16 0.646370 -0.095222 0.135245 0.058 Uiso calc 1 C C17 0.4833(4) -0.1341(4) 0.0506(3) 0.0608(13) Uani d 1 H H17 0.494385 -0.193772 0.008960 0.073 Uiso calc 1 C C18 0.3775(4) -0.1049(3) 0.0370(3) 0.0455(9) Uani d 1 H H18 0.314833 -0.143884 -0.013747 0.055 Uiso calc 1 C C19 0.3647(3) -0.0174(3) 0.0991(2) 0.0270(7) Uani d 1 C C20 0.6430(3) 0.0771(3) 0.2690(2) 0.0340(8) Uani d 1 C C21 0.2553(3) 0.0234(3) 0.0931(2) 0.0259(7) Uani d 1 C C22 -0.1611(3) -0.1818(3) 0.0685(2) 0.0348(8) Uani d 1 H H22 -0.201329 -0.197538 0.005146 0.042 Uiso calc 1 C C23 -0.2069(3) -0.2436(3) 0.1279(2) 0.0349(8) Uani d 1 H H23 -0.277414 -0.300707 0.105490 0.042 Uiso calc 1 C C24 -0.1503(3) -0.2228(3) 0.2209(2) 0.0312(7) Uani d 1 C C25 -0.0469(3) -0.1388(3) 0.2488(2) 0.0379(8) Uani d 1 H H25 -0.004696 -0.121699 0.311693 0.046 Uiso calc 1 C C26 -0.0064(3) -0.0808(3) 0.1848(2) 0.0366(8) Uani d 1 H H26 0.064811 -0.024224 0.205018 0.044 Uiso calc 1 C C27 -0.3032(4) -0.4543(3) 0.3222(3) 0.0487(10) Uani d 1 H H27 -0.348442 -0.528643 0.301746 0.058 Uiso calc 1 C C28 -0.2620(4) -0.3960(3) 0.2591(3) 0.0464(10) Uani d 1 H H28 -0.278275 -0.429877 0.195166 0.056 Uiso calc 1 C C29 -0.1964(3) -0.2870(3) 0.2884(2) 0.0342(7) Uani d 1 C C30 -0.1742(4) -0.2417(3) 0.3821(3) 0.0467(10) Uani d 1 H H30 -0.129636 -0.167454 0.404756 0.056 Uiso calc 1 C C31 -0.2173(4) -0.3052(3) 0.4427(3) 0.0504(11) Uani d 1 H H31 -0.201131 -0.274365 0.507334 0.060 Uiso calc 1 O O14 0.0981(4) -0.2816(3) 0.0446(3) 0.0837(12) Uani d 1 H H14A 0.116521 -0.213833 0.040742 0.100 Uiso d 1 H H14B 0.135621 -0.315863 0.011802 0.100 Uiso d 1 O O15 -0.0270(4) -0.4283(3) 0.1420(3) 0.0858(11) Uani d 1 H H15A -0.001844 -0.391485 0.102894 0.103 Uiso d 1 H H15B -0.074674 -0.485175 0.106464 0.103 Uiso d 1 O O16 0.1138(3) 0.0639(3) 0.4102(2) 0.0653(9) Uani d 1 H H16A 0.147240 0.118555 0.388980 0.078 Uiso d 1 H H16B 0.047900 0.073015 0.420020 0.078 Uiso d 1 O O17 0.7826(4) 0.3307(4) 0.2248(3) 0.1116(16) Uani d 1 H H17A 0.715925 0.287608 0.222536 0.134 Uiso d 1 H H17B 0.836315 0.299958 0.244326 0.134 Uiso d 1 O O18 0.0997(3) -0.0688(3) 0.5499(3) 0.0787(11) Uani d 1 H H18A 0.156299 -0.054494 0.597051 0.094 Uiso d 1 H H18B 0.116249 -0.023124 0.514621 0.094 Uiso d 1 O O19 0.2308(3) -0.2146(3) 0.2416(2) 0.0797(11) Uani d 1 H H19A 0.258882 -0.145513 0.260807 0.096 Uiso d 1 H H19B 0.195102 -0.225943 0.184956 0.096 Uiso d 1 O O20 -0.0833(3) 0.1896(4) 0.2304(3) 0.0971(14) Uani d 1 H H20A -0.019061 0.228664 0.265782 0.116 Uiso d 1 H H20B -0.115701 0.141914 0.258972 0.116 Uiso d 1 O O21 0.2194(4) -0.3847(4) -0.0678(4) 0.1160(17) Uani d 1 H H21A 0.203411 -0.365805 -0.120177 0.139 Uiso d 1 H H21B 0.289591 -0.392045 -0.059657 0.139 Uiso d 1 N N6 0.1635(3) -0.2853(2) 0.4170(2) 0.0415(7) Uani d 1 H H6 0.204128 -0.230599 0.396207 0.050 Uiso calc 1 C C32 0.0819(4) -0.3642(3) 0.3571(3) 0.0446(9) Uani d 1 H H32 0.068083 -0.361485 0.292604 0.054 Uiso calc 1 C C33 0.0166(3) -0.4508(3) 0.3879(3) 0.0389(8) Uani d 1 H H33 -0.041095 -0.508091 0.344431 0.047 Uiso calc 1 C C34 0.0350(3) -0.4543(3) 0.4822(2) 0.0284(7) Uani d 1 C C35 0.1227(3) -0.3697(3) 0.5416(3) 0.0417(9) Uani d 1 H H35 0.139033 -0.369611 0.606528 0.050 Uiso calc 1 C C36 0.1861(4) -0.2860(3) 0.5073(3) 0.0474(10) Uani d 1 H H36 0.246178 -0.228517 0.548521 0.057 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 Tb1 0.02201(9) 0.02243(9) 0.02108(9) 0.00114(6) 0.00463(6) 0.00609(6) Co1 0.0219(3) 0.0250(3) 0.0204(3) -0.0015(2) 0.0020(2) 0.0065(2) O1 0.073(2) 0.0328(15) 0.0567(18) -0.0088(14) 0.0179(15) 0.0191(13) O2 0.0404(13) 0.0254(12) 0.0361(13) -0.0037(10) 0.0099(11) 0.0079(10) O3 0.0464(14) 0.0261(12) 0.0239(12) -0.0073(10) 0.0057(10) 0.0079(9) O4 0.0571(16) 0.0353(14) 0.0254(12) -0.0160(12) 0.0061(11) 0.0024(10) O5 0.0368(13) 0.0354(13) 0.0339(13) 0.0094(10) 0.0153(10) 0.0152(10) O6 0.077(2) 0.0547(18) 0.0595(19) 0.0198(16) 0.0431(17) 0.0322(15) O7 0.0393(13) 0.0385(13) 0.0374(13) 0.0114(11) 0.0177(11) 0.0130(11) O8 0.0424(15) 0.0585(18) 0.0550(17) 0.0214(13) 0.0213(13) 0.0092(14) O9 0.0273(12) 0.0476(15) 0.0290(12) 0.0066(11) -0.0027(10) 0.0060(11) O10 0.0281(14) 0.090(2) 0.0607(19) 0.0247(15) -0.0002(13) 0.0171(17) O11 0.0238(11) 0.0344(13) 0.0311(12) 0.0061(9) -0.0025(9) -0.0008(10) O12 0.0267(12) 0.0365(13) 0.0281(12) 0.0010(10) -0.0029(9) -0.0009(10) O13 0.0271(12) 0.0374(13) 0.0303(12) 0.0033(10) 0.0042(9) 0.0020(10) N1 0.0268(13) 0.0259(13) 0.0258(13) 0.0006(11) 0.0091(11) 0.0108(11) N2 0.0331(14) 0.0250(13) 0.0253(13) 0.0068(11) 0.0065(11) 0.0051(11) N3 0.0217(13) 0.0260(13) 0.0242(13) 0.0045(10) 0.0047(10) 0.0081(10) N4 0.0333(15) 0.0319(15) 0.0285(14) 0.0031(12) 0.0086(12) 0.0108(12) N5 0.057(2) 0.0351(16) 0.0352(16) 0.0002(14) 0.0194(15) 0.0141(13) C1 0.0315(17) 0.0314(17) 0.0332(18) 0.0031(14) 0.0101(14) 0.0161(14) C2 0.053(2) 0.049(2) 0.040(2) 0.0030(19) 0.0153(18) 0.0273(18) C3 0.062(3) 0.059(3) 0.0237(18) -0.001(2) 0.0072(17) 0.0180(17) C4 0.048(2) 0.047(2) 0.0281(18) -0.0049(17) 0.0062(16) 0.0094(16) C5 0.0288(16) 0.0311(17) 0.0260(16) 0.0005(13) 0.0050(13) 0.0089(13) C6 0.0378(19) 0.0266(17) 0.043(2) 0.0017(14) 0.0133(16) 0.0141(15) C7 0.0325(17) 0.0278(17) 0.0280(17) -0.0029(14) 0.0079(14) 0.0075(13) C8 0.0376(19) 0.0344(18) 0.0310(18) 0.0119(15) 0.0068(14) 0.0037(14) C9 0.065(3) 0.059(3) 0.058(3) 0.039(2) 0.021(2) 0.023(2) C10 0.095(4) 0.076(3) 0.074(3) 0.057(3) 0.030(3) 0.044(3) C11 0.079(3) 0.047(2) 0.049(2) 0.027(2) 0.023(2) 0.027(2) C12 0.045(2) 0.0314(18) 0.0257(17) 0.0072(15) 0.0093(15) 0.0067(14) C13 0.0314(17) 0.0338(18) 0.0321(18) 0.0048(15) 0.0074(14) 0.0006(14) C14 0.044(2) 0.0294(17) 0.0293(17) 0.0038(15) 0.0133(15) 0.0074(14) C15 0.0276(16) 0.0371(18) 0.0332(17) 0.0118(14) 0.0105(14) 0.0139(14) C16 0.042(2) 0.050(2) 0.058(3) 0.0251(19) 0.0129(19) 0.0033(19) C17 0.059(3) 0.052(3) 0.069(3) 0.023(2) 0.017(2) -0.015(2) C18 0.044(2) 0.045(2) 0.040(2) 0.0089(18) 0.0049(17) -0.0085(17) C19 0.0272(16) 0.0265(16) 0.0245(16) 0.0017(13) 0.0050(13) 0.0041(13) C20 0.0238(16) 0.045(2) 0.0376(19) 0.0089(15) 0.0069(14) 0.0219(16) C21 0.0242(15) 0.0276(16) 0.0223(15) -0.0009(13) 0.0032(12) 0.0067(13) C22 0.0343(18) 0.0384(19) 0.0275(17) -0.0001(15) 0.0037(14) 0.0103(14) C23 0.0329(18) 0.0335(18) 0.0346(18) -0.0017(14) 0.0088(14) 0.0084(14) C24 0.0413(19) 0.0262(16) 0.0280(17) 0.0049(14) 0.0142(14) 0.0089(13) C25 0.050(2) 0.0317(18) 0.0284(17) 0.0016(16) 0.0071(16) 0.0095(14) C26 0.0385(19) 0.0345(18) 0.0314(18) -0.0040(15) 0.0049(15) 0.0118(15) C27 0.064(3) 0.035(2) 0.037(2) -0.0100(18) 0.0142(19) 0.0061(16) C28 0.063(3) 0.034(2) 0.0329(19) -0.0086(18) 0.0147(18) 0.0037(15) C29 0.044(2) 0.0280(17) 0.0315(18) 0.0038(15) 0.0132(15) 0.0102(14) C30 0.070(3) 0.0288(19) 0.035(2) -0.0065(18) 0.0191(19) 0.0037(15) C31 0.079(3) 0.037(2) 0.0300(19) -0.003(2) 0.0213(19) 0.0038(16) O14 0.127(3) 0.071(2) 0.080(3) 0.044(2) 0.051(2) 0.033(2) O15 0.089(3) 0.078(3) 0.073(2) 0.001(2) 0.000(2) 0.010(2) O16 0.0523(18) 0.062(2) 0.085(2) 0.0097(15) 0.0253(17) 0.0191(18) O17 0.082(3) 0.124(4) 0.124(4) 0.011(3) 0.013(3) 0.042(3) O18 0.0510(19) 0.120(3) 0.078(2) 0.026(2) 0.0181(17) 0.047(2) O19 0.099(3) 0.060(2) 0.063(2) -0.009(2) 0.001(2) 0.0199(17) O20 0.060(2) 0.124(3) 0.088(3) -0.011(2) 0.0397(19) -0.015(2) O21 0.082(3) 0.119(3) 0.131(3) 0.007(2) 0.045(2) -0.022(3) N6 0.0380(17) 0.0313(16) 0.058(2) 0.0022(13) 0.0153(15) 0.0205(15) C32 0.054(2) 0.042(2) 0.040(2) 0.0069(18) 0.0146(18) 0.0163(17) C33 0.048(2) 0.0300(18) 0.0324(18) -0.0012(16) 0.0051(16) 0.0056(14) C34 0.0292(16) 0.0233(15) 0.0326(17) 0.0051(13) 0.0065(13) 0.0071(13) C35 0.045(2) 0.0317(18) 0.039(2) -0.0060(16) 0.0009(16) 0.0087(15) C36 0.042(2) 0.0301(19) 0.060(3) -0.0070(16) 0.0020(19) 0.0101(18) 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' Tb Tb -0.1723 4.1537 '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 O2 Tb1 O5 . . 145.44(8) O2 Tb1 O11 . . 78.37(8) O2 Tb1 N1 . . 64.42(8) O2 Tb1 N2 . . 137.13(9) O2 Tb1 N3 . . 71.80(8) O3 Tb1 O2 . . 128.23(8) O3 Tb1 O5 . . 78.50(8) O3 Tb1 O7 . . 88.30(8) O3 Tb1 O9 . . 79.10(9) O3 Tb1 O11 . . 146.71(8) O3 Tb1 N1 . . 63.89(8) O3 Tb1 N2 . . 75.02(8) O3 Tb1 N3 . . 137.70(8) O5 Tb1 O11 . . 87.75(8) O5 Tb1 N1 . . 137.21(8) O5 Tb1 N2 . . 63.66(8) O5 Tb1 N3 . . 73.68(8) O7 Tb1 O2 . . 79.81(8) O7 Tb1 O5 . . 127.59(8) O7 Tb1 O9 . . 149.74(8) O7 Tb1 O11 . . 76.29(8) O7 Tb1 N1 . . 73.13(8) O7 Tb1 N2 . . 63.93(8) O7 Tb1 N3 . . 133.99(8) O9 Tb1 O2 . . 86.57(8) O9 Tb1 O5 . . 76.91(8) O9 Tb1 O11 . . 127.29(8) O9 Tb1 N1 . . 76.62(8) O9 Tb1 N2 . . 136.11(9) O9 Tb1 N3 . . 64.08(8) O11 Tb1 N1 . . 135.00(8) O11 Tb1 N2 . . 71.71(8) O11 Tb1 N3 . . 63.22(8) N1 Tb1 N2 . . 120.30(8) N1 Tb1 N3 . . 121.84(8) N3 Tb1 N2 . . 117.78(8) O12 Co1 O12 2 . 180.0 O12 Co1 O13 2 . 85.89(9) O12 Co1 O13 . . 94.12(9) O12 Co1 O13 2 2 94.12(9) O12 Co1 O13 . 2 85.88(9) O12 Co1 N4 2 2 91.35(10) O12 Co1 N4 . 2 88.65(10) O12 Co1 N4 2 . 88.65(10) O12 Co1 N4 . . 91.35(10) O13 Co1 O13 . 2 180.0 O13 Co1 N4 2 . 88.03(10) O13 Co1 N4 . . 91.97(10) O13 Co1 N4 2 2 91.97(10) O13 Co1 N4 . 2 88.03(10) N4 Co1 N4 2 . 180.0 C6 O2 Tb1 . . 124.8(2) C7 O3 Tb1 . . 126.3(2) C14 O5 Tb1 . . 125.6(2) C13 O7 Tb1 . . 125.9(2) C20 O9 Tb1 . . 125.5(2) C21 O11 Tb1 . . 124.7(2) C21 O12 Co1 . . 129.3(2) Co1 O13 H13A . . 97.2 Co1 O13 H13B . . 108.8 H13A O13 H13B . . 106.6 C1 N1 Tb1 . . 120.1(2) C5 N1 Tb1 . . 120.6(2) C5 N1 C1 . . 119.3(3) C8 N2 Tb1 . . 120.2(2) C8 N2 C12 . . 119.4(3) C12 N2 Tb1 . . 120.3(2) C15 N3 Tb1 . . 119.6(2) C15 N3 C19 . . 119.4(3) C19 N3 Tb1 . . 121.0(2) C22 N4 Co1 . . 121.0(2) C26 N4 Co1 . . 122.0(2) C26 N4 C22 . . 116.9(3) C27 N5 H5 . . 119.4 C31 N5 H5 . . 119.4 C31 N5 C27 . . 121.1(3) N1 C1 C2 . . 121.7(3) N1 C1 C6 . . 114.6(3) C2 C1 C6 . . 123.7(3) C1 C2 H2 . . 120.4 C1 C2 C3 . . 119.2(3) C3 C2 H2 . . 120.4 C2 C3 H3 . . 120.4 C2 C3 C4 . . 119.1(3) C4 C3 H3 . . 120.4 C3 C4 H4 . . 120.9 C5 C4 C3 . . 118.2(3) C5 C4 H4 . . 120.9 N1 C5 C4 . . 122.6(3) N1 C5 C7 . . 113.6(3) C4 C5 C7 . . 123.8(3) O1 C6 O2 . . 127.0(3) O1 C6 C1 . . 117.1(3) O2 C6 C1 . . 115.9(3) O3 C7 C5 . . 115.5(3) O4 C7 O3 . . 125.9(3) O4 C7 C5 . . 118.6(3) N2 C8 C9 . . 122.0(4) N2 C8 C13 . . 114.1(3) C9 C8 C13 . . 123.8(3) C8 C9 H9 . . 120.7 C8 C9 C10 . . 118.6(4) C10 C9 H9 . . 120.7 C9 C10 H10 . . 120.0 C11 C10 C9 . . 120.0(4) C11 C10 H10 . . 120.0 C10 C11 H11 . . 121.1 C10 C11 C12 . . 117.9(4) C12 C11 H11 . . 121.1 N2 C12 C11 . . 122.1(3) N2 C12 C14 . . 114.5(3) C11 C12 C14 . . 123.5(3) O7 C13 C8 . . 115.8(3) O8 C13 O7 . . 125.5(3) O8 C13 C8 . . 118.7(3) O5 C14 C12 . . 115.9(3) O6 C14 O5 . . 126.1(3) O6 C14 C12 . . 118.1(3) N3 C15 C16 . . 122.0(3) N3 C15 C20 . . 114.4(3) C16 C15 C20 . . 123.7(3) C15 C16 H16 . . 120.7 C17 C16 C15 . . 118.7(4) C17 C16 H16 . . 120.7 C16 C17 H17 . . 120.2 C18 C17 C16 . . 119.6(4) C18 C17 H17 . . 120.2 C17 C18 H18 . . 120.7 C17 C18 C19 . . 118.5(4) C19 C18 H18 . . 120.7 N3 C19 C18 . . 121.9(3) N3 C19 C21 . . 113.7(3) C18 C19 C21 . . 124.4(3) O9 C20 C15 . . 116.4(3) O10 C20 O9 . . 126.2(3) O10 C20 C15 . . 117.3(3) O11 C21 C19 . . 116.8(3) O12 C21 O11 . . 125.6(3) O12 C21 C19 . . 117.5(3) N4 C22 H22 . . 118.5 N4 C22 C23 . . 123.1(3) C23 C22 H22 . . 118.5 C22 C23 H23 . . 120.0 C22 C23 C24 . . 119.9(3) C24 C23 H23 . . 120.0 C23 C24 C25 . . 117.0(3) C23 C24 C29 . . 122.2(3) C25 C24 C29 . . 120.8(3) C24 C25 H25 . . 120.3 C26 C25 C24 . . 119.5(3) C26 C25 H25 . . 120.3 N4 C26 C25 . . 123.5(3) N4 C26 H26 . . 118.2 C25 C26 H26 . . 118.2 N5 C27 H27 . . 119.7 N5 C27 C28 . . 120.6(3) C28 C27 H27 . . 119.7 C27 C28 H28 . . 120.0 C27 C28 C29 . . 120.0(3) C29 C28 H28 . . 120.0 C28 C29 C24 . . 120.6(3) C30 C29 C24 . . 121.5(3) C30 C29 C28 . . 117.8(3) C29 C30 H30 . . 120.2 C29 C30 C31 . . 119.5(3) C31 C30 H30 . . 120.2 N5 C31 C30 . . 121.0(3) N5 C31 H31 . . 119.5 C30 C31 H31 . . 119.5 H14A O14 H14B . . 108.4 H15A O15 H15B . . 101.8 H16A O16 H16B . . 108.6 H17A O17 H17B . . 108.7 H18A O18 H18B . . 108.8 H19A O19 H19B . . 108.6 H20A O20 H20B . . 108.7 H21A O21 H21B . . 107.9 C32 N6 H6 . . 119.0 C32 N6 C36 . . 122.0(3) C36 N6 H6 . . 119.0 N6 C32 H32 . . 119.9 N6 C32 C33 . . 120.2(4) C33 C32 H32 . . 119.9 C32 C33 H33 . . 119.9 C32 C33 C34 . . 120.2(3) C34 C33 H33 . . 119.9 C33 C34 C34 . 2_546 121.5(4) C35 C34 C33 . . 117.0(3) C35 C34 C34 . 2_546 121.5(4) C34 C35 H35 . . 119.7 C36 C35 C34 . . 120.6(4) C36 C35 H35 . . 119.7 N6 C36 C35 . . 120.1(4) N6 C36 H36 . . 120.0 C35 C36 H36 . . 120.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Tb1 O2 . 2.431(2) Tb1 O3 . 2.393(2) Tb1 O5 . 2.439(2) Tb1 O7 . 2.409(2) Tb1 O9 . 2.411(2) Tb1 O11 . 2.451(2) Tb1 N1 . 2.499(3) Tb1 N2 . 2.520(3) Tb1 N3 . 2.515(3) Co1 O12 2 2.092(2) Co1 O12 . 2.092(2) Co1 O13 . 2.102(2) Co1 O13 2 2.102(2) Co1 N4 2 2.151(3) Co1 N4 . 2.151(3) O1 C6 . 1.238(4) O2 C6 . 1.266(4) O3 C7 . 1.263(4) O4 C7 . 1.240(4) O5 C14 . 1.262(4) O6 C14 . 1.239(4) O7 C13 . 1.270(4) O8 C13 . 1.243(4) O9 C20 . 1.254(4) O10 C20 . 1.244(4) O11 C21 . 1.256(4) O12 C21 . 1.252(4) O13 H13A . 0.8735 O13 H13B . 0.8501 N1 C1 . 1.338(4) N1 C5 . 1.332(4) N2 C8 . 1.335(4) N2 C12 . 1.340(4) N3 C15 . 1.335(4) N3 C19 . 1.338(4) N4 C22 . 1.347(4) N4 C26 . 1.333(4) N5 H5 . 0.8800 N5 C27 . 1.334(5) N5 C31 . 1.316(5) C1 C2 . 1.380(5) C1 C6 . 1.517(5) C2 H2 . 0.9500 C2 C3 . 1.382(6) C3 H3 . 0.9500 C3 C4 . 1.390(5) C4 H4 . 0.9500 C4 C5 . 1.382(5) C5 C7 . 1.511(4) C8 C9 . 1.378(5) C8 C13 . 1.512(5) C9 H9 . 0.9500 C9 C10 . 1.384(7) C10 H10 . 0.9500 C10 C11 . 1.382(7) C11 H11 . 0.9500 C11 C12 . 1.391(5) C12 C14 . 1.510(5) C15 C16 . 1.382(5) C15 C20 . 1.505(5) C16 H16 . 0.9500 C16 C17 . 1.380(6) C17 H17 . 0.9500 C17 C18 . 1.378(6) C18 H18 . 0.9500 C18 C19 . 1.385(5) C19 C21 . 1.495(5) C22 H22 . 0.9500 C22 C23 . 1.366(5) C23 H23 . 0.9500 C23 C24 . 1.388(5) C24 C25 . 1.390(5) C24 C29 . 1.483(4) C25 H25 . 0.9500 C25 C26 . 1.372(5) C26 H26 . 0.9500 C27 H27 . 0.9500 C27 C28 . 1.366(5) C28 H28 . 0.9500 C28 C29 . 1.390(5) C29 C30 . 1.380(5) C30 H30 . 0.9500 C30 C31 . 1.382(5) C31 H31 . 0.9500 O14 H14A . 0.8500 O14 H14B . 0.8499 O15 H15A . 0.8501 O15 H15B . 0.8499 O16 H16A . 0.8504 O16 H16B . 0.8500 O17 H17A . 0.8503 O17 H17B . 0.8498 O18 H18A . 0.8501 O18 H18B . 0.8497 O19 H19A . 0.8500 O19 H19B . 0.8501 O20 H20A . 0.8499 O20 H20B . 0.8498 O21 H21A . 0.8502 O21 H21B . 0.8502 N6 H6 . 0.8800 N6 C32 . 1.321(5) N6 C36 . 1.324(5) C32 H32 . 0.9500 C32 C33 . 1.382(5) C33 H33 . 0.9500 C33 C34 . 1.389(5) C34 C34 2_546 1.489(6) C34 C35 . 1.387(5) C35 H35 . 0.9500 C35 C36 . 1.375(5) C36 H36 . 0.9500 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_4 _geom_torsion Tb1 O2 C6 O1 . . -179.4(3) Tb1 O2 C6 C1 . . -0.8(4) Tb1 O3 C7 O4 . . 176.4(3) Tb1 O3 C7 C5 . . -0.9(4) Tb1 O5 C14 O6 . . -177.7(3) Tb1 O5 C14 C12 . . 1.9(4) Tb1 O7 C13 O8 . . 179.2(3) Tb1 O7 C13 C8 . . -0.2(4) Tb1 O9 C20 O10 . . 178.5(3) Tb1 O9 C20 C15 . . -3.6(4) Tb1 O11 C21 O12 . . 171.1(2) Tb1 O11 C21 C19 . . -8.9(4) Tb1 N1 C1 C2 . . -177.3(3) Tb1 N1 C1 C6 . . 3.8(4) Tb1 N1 C5 C4 . . 177.8(3) Tb1 N1 C5 C7 . . -3.6(4) Tb1 N2 C8 C9 . . -175.5(3) Tb1 N2 C8 C13 . . 0.6(4) Tb1 N2 C12 C11 . . 176.8(3) Tb1 N2 C12 C14 . . -2.9(4) Tb1 N3 C15 C16 . . 178.6(3) Tb1 N3 C15 C20 . . 0.1(4) Tb1 N3 C19 C18 . . -178.4(3) Tb1 N3 C19 C21 . . 1.4(3) Co1 O12 C21 O11 . . -0.1(5) Co1 O12 C21 C19 . . 179.9(2) Co1 N4 C22 C23 . . -176.6(3) Co1 N4 C26 C25 . . 176.2(3) N1 C1 C2 C3 . . -0.1(6) N1 C1 C6 O1 . . 176.8(3) N1 C1 C6 O2 . . -2.0(5) N1 C5 C7 O3 . . 3.0(4) N1 C5 C7 O4 . . -174.6(3) N2 C8 C9 C10 . . -2.0(7) N2 C8 C13 O7 . . -0.3(4) N2 C8 C13 O8 . . -179.7(3) N2 C12 C14 O5 . . 0.8(4) N2 C12 C14 O6 . . -179.6(3) N3 C15 C16 C17 . . -0.2(6) N3 C15 C20 O9 . . 2.1(4) N3 C15 C20 O10 . . -179.8(3) N3 C19 C21 O11 . . 4.5(4) N3 C19 C21 O12 . . -175.5(3) N4 C22 C23 C24 . . 0.0(6) N5 C27 C28 C29 . . -0.3(7) C1 N1 C5 C4 . . 0.0(5) C1 N1 C5 C7 . . 178.6(3) C1 C2 C3 C4 . . -0.7(7) C2 C1 C6 O1 . . -2.1(6) C2 C1 C6 O2 . . 179.1(4) C2 C3 C4 C5 . . 1.0(6) C3 C4 C5 N1 . . -0.7(6) C3 C4 C5 C7 . . -179.2(4) C4 C5 C7 O3 . . -178.5(4) C4 C5 C7 O4 . . 4.0(5) C5 N1 C1 C2 . . 0.4(5) C5 N1 C1 C6 . . -178.5(3) C6 C1 C2 C3 . . 178.7(4) C8 N2 C12 C11 . . -0.1(5) C8 N2 C12 C14 . . -179.8(3) C8 C9 C10 C11 . . 1.2(8) C9 C8 C13 O7 . . 175.7(4) C9 C8 C13 O8 . . -3.7(5) C9 C10 C11 C12 . . 0.0(8) C10 C11 C12 N2 . . -0.6(6) C10 C11 C12 C14 . . 179.1(4) C11 C12 C14 O5 . . -178.9(4) C11 C12 C14 O6 . . 0.7(6) C12 N2 C8 C9 . . 1.4(5) C12 N2 C8 C13 . . 177.5(3) C13 C8 C9 C10 . . -177.7(4) C15 N3 C19 C18 . . -0.1(5) C15 N3 C19 C21 . . 179.8(3) C15 C16 C17 C18 . . 0.1(7) C16 C15 C20 O9 . . -176.4(4) C16 C15 C20 O10 . . 1.6(5) C16 C17 C18 C19 . . 0.1(7) C17 C18 C19 N3 . . -0.1(6) C17 C18 C19 C21 . . -180.0(4) C18 C19 C21 O11 . . -175.6(3) C18 C19 C21 O12 . . 4.4(5) C19 N3 C15 C16 . . 0.2(5) C19 N3 C15 C20 . . -178.3(3) C20 C15 C16 C17 . . 178.2(4) C22 N4 C26 C25 . . -1.2(6) C22 C23 C24 C25 . . -0.6(5) C22 C23 C24 C29 . . 179.7(3) C23 C24 C25 C26 . . 0.3(5) C23 C24 C29 C28 . . 29.0(6) C23 C24 C29 C30 . . -152.1(4) C24 C25 C26 N4 . . 0.6(6) C24 C29 C30 C31 . . -178.9(4) C25 C24 C29 C28 . . -150.7(4) C25 C24 C29 C30 . . 28.2(6) C26 N4 C22 C23 . . 0.9(5) C27 N5 C31 C30 . . 1.2(7) C27 C28 C29 C24 . . 179.5(4) C27 C28 C29 C30 . . 0.6(6) C28 C29 C30 C31 . . 0.0(6) C29 C24 C25 C26 . . -180.0(3) C29 C30 C31 N5 . . -0.9(7) C31 N5 C27 C28 . . -0.6(7) N6 C32 C33 C34 . . 1.1(6) C32 N6 C36 C35 . . -0.9(6) C32 C33 C34 C34 . 2_546 179.2(4) C32 C33 C34 C35 . . -1.7(5) C33 C34 C35 C36 . . 1.0(6) C34 C34 C35 C36 2_546 . -179.9(4) C34 C35 C36 N6 . . 0.2(6) C36 N6 C32 C33 . . 0.3(6) _cod_database_fobs_code 2021637