#------------------------------------------------------------------------------ #$Date: 2021-10-14 02:13:13 +0300 (Thu, 14 Oct 2021) $ #$Revision: 269926 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708552.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7708552 loop_ _publ_author_name 'Jim\'enez, Juan-Ram\'on' 'Xu, Buqin' 'El Said, Hasnaa' 'Li, Yanling' 'von Bardeleben, Jurgen' 'Chamoreau, Lise-Marie' 'Lescouezec, Rodrigue' 'Shova, Sergiu' 'Visinescu, Diana' 'Alexandru, Maria-Gabriela' 'Cano, Joan' 'Julve, Miguel' _publ_section_title ; Field-induced Single Ion Magnet behaviour in discrete and one-dimensional complexes containing the bis(1-methylimidazol-2-yl)ketone]-containing cobalt(II) building units ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT02441H _journal_year 2021 _chemical_formula_moiety 'C22 H20 Co N14 O2' _chemical_formula_sum 'C22 H20 Co N14 O2' _chemical_formula_weight 571.45 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2021-08-31 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-08-31 deposited with the CCDC. 2021-10-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 98.148(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.4394(6) _cell_length_b 13.0372(9) _cell_length_c 23.9828(16) _cell_measurement_reflns_used 4931 _cell_measurement_temperature 200 _cell_measurement_theta_max 68 _cell_measurement_theta_min 6 _cell_volume 2612.1(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'DIAMOND (Brandenburg)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 200 _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.974 _diffrn_measured_fraction_theta_max 0.970 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker Quazar' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_unetI/netI 0.0264 _diffrn_reflns_Laue_measured_fraction_full 0.974 _diffrn_reflns_Laue_measured_fraction_max 0.970 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 8338 _diffrn_reflns_point_group_measured_fraction_full 0.974 _diffrn_reflns_point_group_measured_fraction_max 0.970 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.350 _diffrn_reflns_theta_min 3.724 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\ms' _exptl_absorpt_coefficient_mu 5.577 _exptl_absorpt_correction_T_max 0.8 _exptl_absorpt_correction_T_min 0.68 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.453 _exptl_crystal_description plate _exptl_crystal_F_000 1172 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.150 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.034 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 197 _refine_ls_number_reflns 2329 _refine_ls_number_restraints 15 _refine_ls_restrained_S_all 1.049 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0300 _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^)+(0.0465P)^2^+1.1306P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0825 _refine_ls_wR_factor_ref 0.0841 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2231 _reflns_number_total 2329 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt02441h2.cif _cod_data_source_block jr_cobik_cnnnc_0m _cod_database_code 7708552 _shelx_shelxl_version_number 2017/1 _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_max 0.768 _shelx_estimated_absorpt_t_min 0.402 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Rigid body (RIGU) restrains N6, C10, C11 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 N6B, C10, C11 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 3. Others Fixed Sof: N6B(0.5) N6(0.5) N7B(0.5) N7(0.5) 4.a Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C6(H6), C7(H7) 4.b Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C9(H9A,H9B,H9C) ; _shelx_res_file ; TITL jr_cobik_cnnnc_0m_a.res in C2/c jr_cobik_cnnnc_0m.res created by SHELXL-2017/1 at 16:02:39 on 31-Aug-2021 REM Old TITL jr_cobik_cnnnc_0m in C2/c REM SHELXT solution in C2/c REM R1 0.139, Rweak 0.020, Alpha 0.055, Orientation as input REM Formula found by SHELXT: C24 N10 O4 Co CELL 1.54178 8.4394 13.0372 23.9828 90 98.148 90 ZERR 4 0.0006 0.0009 0.0016 0 0.004 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Co N O UNIT 88 80 4 56 8 RIGU N6 C10 C11 RIGU N6b C10 C11 L.S. 8 PLAN 20 SIZE 0.2 0.11 0.05 TEMP -73.15 BOND $H list 4 fmap 2 acta OMIT 1 3 1 OMIT -3 3 9 OMIT -5 1 9 OMIT -4 2 10 REM REM REM WGHT 0.046500 1.130600 FVAR 0.43250 CO1 3 0.500000 0.449473 0.250000 10.50000 0.04403 0.04320 = 0.02965 0.00000 0.00232 0.00000 O1 5 0.605871 0.385988 0.444156 11.00000 0.09397 0.09417 = 0.02998 -0.00881 0.00178 0.01730 N1 4 0.638416 0.338624 0.299611 11.00000 0.05578 0.04641 = 0.03034 -0.00088 0.00486 0.00750 N2 4 0.356573 0.446568 0.315649 11.00000 0.04682 0.05541 = 0.03900 -0.00470 0.00741 0.00333 N3 4 0.648416 0.561920 0.294958 11.00000 0.05884 0.05099 = 0.04775 -0.00287 -0.00511 -0.00381 N4 4 0.783330 0.267120 0.373407 11.00000 0.05512 0.05767 = 0.03755 0.00655 0.00137 0.00639 N5 4 0.282638 0.439182 0.400326 11.00000 0.06803 0.05902 = 0.05079 -0.01130 0.02623 -0.00014 PART 2 N6B 4 0.810967 0.679192 0.357146 10.50000 0.16512 0.07007 = 0.08431 0.02663 -0.06291 -0.06333 PART 0 PART 1 N6 4 0.755053 0.675355 0.371304 10.50000 0.09344 0.05498 = 0.10066 -0.03872 -0.02751 0.02659 PART 0 PART 2 N7B 4 0.950541 0.652118 0.449587 10.50000 0.09898 0.13424 = 0.04399 -0.01664 0.00885 -0.03606 PART 0 PART 1 N7 4 0.972817 0.637858 0.446342 10.50000 0.05660 0.15548 = 0.05946 -0.04323 -0.00498 0.01316 PART 0 C1 1 0.752902 0.278387 0.282014 11.00000 0.07071 0.05886 = 0.03887 -0.00147 0.01399 0.01563 AFIX 43 H1 2 0.768655 0.269249 0.243885 11.00000 -1.20000 AFIX 0 C2 1 0.841325 0.233257 0.326940 11.00000 0.06353 0.06268 = 0.05412 0.00435 0.01213 0.01831 AFIX 43 H2 2 0.927547 0.186737 0.325996 11.00000 -1.20000 AFIX 0 C3 1 0.658513 0.330808 0.355641 11.00000 0.05022 0.04274 = 0.02989 -0.00025 0.00093 0.00019 C4 1 0.560662 0.381158 0.393625 11.00000 0.06307 0.04847 = 0.03076 -0.00409 0.00654 -0.00167 C5 1 0.402892 0.422086 0.369344 11.00000 0.05622 0.04533 = 0.03665 -0.00862 0.01383 -0.00282 C6 1 0.156375 0.474640 0.364441 11.00000 0.05983 0.07807 = 0.07831 -0.01054 0.02722 0.00824 AFIX 43 H6 2 0.054275 0.492563 0.373814 11.00000 -1.20000 AFIX 0 C7 1 0.202402 0.479846 0.312762 11.00000 0.05141 0.08163 = 0.06569 -0.00180 0.01044 0.01264 AFIX 43 H7 2 0.137410 0.503089 0.279573 11.00000 -1.20000 AFIX 0 C8 1 0.843401 0.233076 0.431305 11.00000 0.07181 0.09094 = 0.04456 0.01677 -0.00548 0.01812 AFIX 137 H8A 2 0.883647 0.292404 0.454123 11.00000 -1.50000 H8B 2 0.930208 0.183477 0.430303 11.00000 -1.50000 H8C 2 0.756197 0.200764 0.447895 11.00000 -1.50000 AFIX 0 C9 1 0.279242 0.419135 0.460641 11.00000 0.10640 0.09027 = 0.05539 -0.00812 0.04563 0.00190 AFIX 137 H9A 2 0.314425 0.348653 0.469575 11.00000 -1.50000 H9B 2 0.169957 0.428281 0.469185 11.00000 -1.50000 H9C 2 0.351086 0.467145 0.483259 11.00000 -1.50000 AFIX 0 C10 1 0.716093 0.612009 0.329305 11.00000 0.06618 0.04330 = 0.05867 0.00220 -0.01173 0.00178 C11 1 0.876663 0.655559 0.408744 11.00000 0.05705 0.06894 = 0.05504 -0.02079 0.00771 -0.00964 HKLF 4 REM jr_cobik_cnnnc_0m_a.res in C2/c REM R1 = 0.0300 for 2231 Fo > 4sig(Fo) and 0.0318 for all 2329 data REM 197 parameters refined using 15 restraints END WGHT 0.0465 1.1306 REM Highest difference peak 0.150, deepest hole -0.245, 1-sigma level 0.034 Q1 1 0.6094 0.3686 0.3701 11.00000 0.05 0.15 Q2 1 0.3913 0.4512 0.3393 11.00000 0.05 0.13 Q3 1 0.5689 0.4563 0.2893 11.00000 0.05 0.13 Q4 1 0.6020 0.3859 0.2813 11.00000 0.05 0.13 Q5 1 0.8910 0.6142 0.3464 11.00000 0.05 0.12 Q6 1 0.8593 0.3033 0.4418 11.00000 0.05 0.12 Q7 1 0.5395 0.3432 0.4393 11.00000 0.05 0.12 Q8 1 0.8811 0.5936 0.4239 11.00000 0.05 0.11 Q9 1 0.7328 0.6153 0.3944 11.00000 0.05 0.11 Q10 1 0.1761 0.5166 0.2885 11.00000 0.05 0.11 Q11 1 0.6620 0.3525 0.3257 11.00000 0.05 0.11 Q12 1 0.7783 0.5812 0.3176 11.00000 0.05 0.10 Q13 1 0.5784 0.5966 0.2686 11.00000 0.05 0.10 Q14 1 0.3615 0.4393 0.3878 11.00000 0.05 0.10 Q15 1 0.7317 0.5528 0.2677 11.00000 0.05 0.10 Q16 1 0.5513 0.3368 0.2698 11.00000 0.05 0.10 Q17 1 0.2385 0.4944 0.3888 11.00000 0.05 0.10 Q18 1 0.4337 0.4358 0.3017 11.00000 0.05 0.09 Q19 1 0.5076 0.2648 0.2687 11.00000 0.05 0.09 Q20 1 0.8322 0.2805 0.3092 11.00000 0.05 0.09 ; _shelx_res_checksum 89678 _shelx_hkl_file ; -2 0 0 5434.46 157.18 -2 0 0 5350.66 155.98 -4 0 0 97.39 3.40 -6 0 0 453.95 14.40 -6 0 0 464.45 13.90 -8 0 0 201.78 6.90 -8 0 0 199.78 7.50 -8 0 0 197.08 8.40 -10 0 0 2.00 1.00 -10 0 0 2.90 2.10 1 -1 0 7187.38 208.18 -1 -1 0 6665.13 205.88 -1 1 0 7243.78 209.88 -1 1 0 7002.70 204.88 -3 -1 0 179.58 5.30 -3 -1 0 179.98 5.20 -3 1 0 176.68 5.50 -5 1 0 76.89 3.00 -7 -1 0 136.79 5.10 -7 -1 0 143.59 6.00 -7 1 0 139.29 5.80 -7 1 0 141.29 5.20 -9 -1 0 46.50 4.50 -9 -1 0 41.30 2.80 -9 -1 0 44.70 3.60 -9 1 0 39.90 2.90 -9 1 0 40.50 3.10 -9 1 0 37.30 3.40 0 2 0 557.34 16.20 -2 -2 0 1450.55 43.30 -2 2 0 1537.85 43.80 -4 2 0 58.79 2.30 -6 -2 0 208.48 6.70 -6 -2 0 201.88 7.50 -6 2 0 196.98 7.00 -6 2 0 209.18 6.80 -8 -2 0 24.20 2.00 -8 -2 0 25.80 3.10 -8 -2 0 26.80 3.20 -8 2 0 21.80 2.10 -8 2 0 22.80 2.50 -8 2 0 22.40 3.10 -1 3 0 24.10 1.10 -3 -3 0 1494.95 43.30 -3 3 0 1494.65 43.50 -5 3 0 97.19 3.60 -7 -3 0 31.50 2.60 -7 -3 0 35.20 4.20 -7 3 0 33.20 3.00 -7 3 0 30.00 3.10 -7 3 0 32.50 3.00 -9 -3 0 54.79 2.90 -9 -3 0 53.39 2.80 -9 -3 0 51.59 3.60 -9 -3 0 56.19 4.30 -9 3 0 52.19 4.10 -9 3 0 51.79 3.20 0 4 0 56.59 6.90 -2 -4 0 1185.48 34.30 -2 4 0 1174.58 34.40 -4 -4 0 266.87 8.00 -4 4 0 275.47 8.40 -6 -4 0 156.28 5.40 -6 -4 0 154.88 6.90 -6 4 0 160.28 5.70 -8 -4 0 4.40 3.10 -8 -4 0 1.70 1.50 -8 -4 0 2.30 1.50 -8 4 0 1.30 2.20 -8 4 0 0.20 1.80 -1 5 0 1070.69 45.50 -3 5 0 451.35 13.60 -3 5 0 457.95 13.80 -5 -5 0 17.60 1.50 -5 -5 0 16.50 1.80 -5 -5 0 17.90 1.50 -5 5 0 17.50 1.70 -7 -5 0 109.99 6.60 -7 -5 0 110.69 4.40 -7 -5 0 105.09 4.40 -7 5 0 110.59 5.30 -7 5 0 110.29 5.00 -9 -5 0 17.10 2.70 -9 -5 0 17.70 1.70 -9 -5 0 17.20 1.60 -9 5 0 21.80 2.00 -9 5 0 18.20 2.00 9 5 0 20.80 1.70 0 6 0 637.54 18.90 -2 6 0 68.99 2.90 -4 6 0 134.99 5.00 -6 -6 0 11.50 1.70 -6 -6 0 7.80 3.20 -6 -6 0 10.60 1.70 -6 -6 0 13.10 2.10 -6 6 0 8.90 2.20 -8 -6 0 7.10 1.70 -8 -6 0 4.70 1.50 -8 -6 0 5.80 3.00 -8 6 0 4.10 2.20 -8 6 0 4.70 1.90 8 6 0 -0.50 5.40 1 7 0 1069.59 32.50 1 7 0 1062.99 31.40 -1 7 0 1078.29 31.50 -3 7 0 33.30 2.50 -5 -7 0 67.79 3.50 -5 -7 0 61.79 4.10 -5 -7 0 63.99 3.60 -5 7 0 59.09 4.20 -7 -7 0 64.39 3.70 -7 -7 0 65.89 3.80 -7 -7 0 71.89 5.50 -7 7 0 61.99 4.70 -9 -7 0 9.90 1.30 0 8 0 476.95 14.40 -2 8 0 35.00 2.50 -4 -8 0 19.80 2.10 -4 -8 0 25.10 2.50 -4 8 0 17.90 2.30 -4 8 0 22.90 2.60 -6 -8 0 103.49 4.90 -6 -8 0 116.29 5.70 6 -8 0 93.59 5.60 -6 -8 0 95.69 4.90 -6 -8 0 118.89 6.20 -6 8 0 96.69 6.00 -8 -8 0 49.00 3.60 -8 -8 0 44.90 2.70 -8 8 0 46.00 3.50 8 8 0 47.40 2.50 1 9 0 314.17 9.90 -1 9 0 310.57 10.10 -1 9 0 323.47 10.10 -1 9 0 323.17 10.10 -3 -9 0 16.90 1.70 -3 -9 0 13.50 2.00 3 9 0 24.70 2.30 3 9 0 17.30 1.90 -3 9 0 12.60 1.90 -3 9 0 13.50 2.00 -3 9 0 13.70 2.00 -5 -9 0 169.88 7.00 -5 -9 0 152.58 6.20 5 9 0 158.58 6.20 -5 9 0 169.38 7.10 -7 -9 0 80.19 4.40 -7 -9 0 77.49 3.60 -7 9 0 82.09 4.60 7 9 0 80.69 3.60 0 10 0 806.62 24.20 0 10 0 813.32 24.10 0 10 0 801.22 24.20 -2 -10 0 97.19 4.30 -2 10 0 97.69 4.40 2 10 0 102.09 4.50 -2 10 0 102.59 4.60 -2 10 0 97.39 4.40 -4 -10 0 11.90 1.80 -4 -10 0 11.60 2.30 -4 10 0 12.90 2.30 4 10 0 10.00 1.70 -4 10 0 15.50 2.40 -6 -10 0 177.88 6.00 6 -10 0 179.18 6.70 -6 -10 0 156.08 6.80 6 10 0 173.48 5.90 -6 10 0 179.38 6.80 1 11 0 135.19 5.50 -1 11 0 138.19 5.50 -1 11 0 143.89 5.40 -1 11 0 137.99 5.50 1 11 0 134.39 5.50 -3 -11 0 35.40 2.80 -3 11 0 31.90 3.30 -3 11 0 33.70 3.50 3 11 0 31.30 3.20 -5 -11 0 73.39 4.30 -5 -11 0 71.09 3.40 -5 11 0 74.59 4.10 5 11 0 71.59 3.40 7 11 0 34.10 2.10 -7 11 0 36.30 2.30 0 12 0 10.10 1.90 0 12 0 8.90 2.00 -2 -12 0 84.59 4.50 -2 12 0 92.19 4.60 2 12 0 94.49 4.50 -2 12 0 88.69 4.50 -4 -12 0 100.39 4.70 -4 12 0 104.59 4.60 6 -12 0 6.10 1.30 -6 12 0 8.20 1.40 -1 -13 0 12.70 1.80 -1 13 0 12.60 2.10 1 13 0 14.60 2.10 -1 13 0 14.50 2.20 -3 -13 0 60.69 3.60 -3 13 0 60.39 3.50 -3 13 0 60.39 3.60 5 -13 0 8.10 1.50 -5 13 0 9.60 1.40 0 14 0 9.00 1.80 -2 -14 0 1.40 1.30 2 14 0 0.70 1.40 -2 14 0 2.00 1.50 -2 14 0 0.80 1.50 -4 -14 0 2.30 1.20 4 -14 0 1.20 1.40 -4 14 0 1.60 1.20 -1 15 0 0.60 1.20 1 15 0 2.40 1.30 -10 0 1 -0.40 1.90 -10 0 1 -2.20 1.00 -10 0 1 -1.10 1.00 -8 0 1 -0.90 2.80 -8 0 1 -0.10 1.60 -8 0 1 -0.90 2.10 -6 0 1 -0.60 1.60 -6 0 1 0.30 1.10 -4 0 1 -0.40 0.60 -2 0 1 -0.50 0.40 -2 0 1 -0.10 0.20 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1.80 1 -5 -24 -2.50 1.70 1 -5 -24 1.20 1.60 1 5 -24 1.20 1.60 -1 -5 -24 7.40 1.70 -1 5 -24 6.00 1.60 -3 5 -24 -1.20 1.10 4 -6 -24 10.40 1.80 4 -6 -24 11.40 1.50 4 6 -24 8.70 1.50 2 -6 -24 4.90 1.60 2 -6 -24 6.00 1.80 2 -6 -24 6.90 1.80 2 6 -24 5.00 1.50 0 -6 -24 65.29 3.30 0 -6 -24 69.69 3.60 0 -6 -24 65.79 3.30 0 6 -24 68.19 3.60 -2 -6 -24 3.40 1.10 -2 6 -24 2.40 1.30 3 -7 -24 80.09 3.30 3 -7 -24 73.49 3.40 3 7 -24 73.69 3.20 1 -7 -24 53.59 3.20 1 -7 -24 52.09 2.80 1 -7 -24 51.79 3.00 1 7 -24 49.40 3.00 -1 -7 -24 32.00 1.90 -1 -7 -24 30.10 2.30 -1 -7 -24 28.20 2.10 -1 7 -24 30.60 2.40 2 -8 -24 174.58 5.50 2 -8 -24 174.68 5.80 2 -8 -24 173.58 5.70 2 8 -24 169.88 5.70 0 -8 -24 21.10 1.60 0 -8 -24 21.60 1.90 0 8 -24 18.80 1.50 6 0 -25 -1.00 1.20 4 0 -25 -1.50 1.40 2 0 -25 0.50 1.30 2 0 -25 0.30 1.40 0 0 -25 -1.70 1.40 -2 0 -25 2.30 1.50 5 -1 -25 24.30 2.50 5 1 -25 20.40 1.90 3 -1 -25 29.00 2.60 3 -1 -25 27.50 2.30 3 1 -25 27.00 2.50 1 -1 -25 5.30 1.50 1 1 -25 6.40 1.40 -1 -1 -25 32.60 2.90 -1 1 -25 28.40 2.70 -3 -1 -25 23.90 1.90 -3 1 -25 24.20 2.30 6 -2 -25 2.70 1.30 6 2 -25 4.70 1.30 4 -2 -25 6.00 1.30 4 -2 -25 1.10 1.60 4 2 -25 5.70 1.50 2 -2 -25 8.10 1.60 2 -2 -25 7.10 1.60 0 -2 -25 3.00 1.60 0 2 -25 4.50 1.40 -2 -2 -25 65.59 3.40 -2 2 -25 60.69 2.90 -2 2 -25 64.49 3.10 5 -3 -25 6.60 1.20 5 -3 -25 7.20 1.70 5 3 -25 6.80 1.40 3 -3 -25 12.00 1.70 3 -3 -25 16.00 1.90 3 3 -25 13.50 1.60 1 -3 -25 80.09 3.90 1 -3 -25 80.99 3.50 -1 -3 -25 43.70 3.20 -1 3 -25 48.20 2.70 -1 3 -25 46.80 2.60 -3 -3 -25 88.49 3.50 -3 3 -25 85.99 3.40 4 -4 -25 12.00 1.50 4 -4 -25 10.70 1.80 4 4 -25 13.00 1.60 2 -4 -25 105.39 4.50 2 -4 -25 108.09 4.40 0 -4 -25 57.59 3.40 0 4 -25 67.29 3.20 -2 -4 -25 83.79 3.60 -2 4 -25 78.29 3.20 -2 4 -25 78.69 3.40 5 -5 -25 33.50 2.40 5 5 -25 36.70 2.20 3 -5 -25 87.69 4.00 3 -5 -25 87.89 3.80 1 -5 -25 40.70 2.70 1 -5 -25 38.30 3.00 1 5 -25 43.80 2.80 -1 -5 -25 25.10 1.90 -1 5 -25 23.30 2.40 4 -6 -25 109.79 4.30 4 -6 -25 119.79 4.10 4 6 -25 114.49 5.00 2 -6 -25 72.89 3.40 2 -6 -25 72.59 3.40 2 6 -25 67.69 3.20 0 -6 -25 75.19 3.20 0 -6 -25 67.39 3.00 0 6 -25 64.69 3.30 -2 6 -25 20.60 2.00 3 -7 -25 78.19 3.10 3 -7 -25 79.29 3.30 1 -7 -25 74.09 3.30 1 -7 -25 74.99 3.00 1 -7 -25 75.79 3.20 1 7 -25 74.99 3.20 -1 7 -25 2.40 1.20 4 0 -26 14.00 1.60 2 0 -26 67.09 3.00 0 0 -26 369.56 11.40 -2 0 -26 24.10 2.30 5 -1 -26 7.30 1.40 5 1 -26 6.00 1.40 3 -1 -26 28.70 2.50 3 -1 -26 31.80 2.20 3 1 -26 25.90 2.30 1 -1 -26 220.18 7.10 1 1 -26 214.48 7.00 -1 -1 -26 30.80 2.70 -1 1 -26 28.90 2.50 -3 -1 -26 24.00 2.00 -3 1 -26 22.90 2.00 4 -2 -26 5.80 1.10 4 -2 -26 5.20 1.50 4 2 -26 5.50 1.40 2 -2 -26 96.69 3.90 2 -2 -26 93.89 3.80 0 -2 -26 23.90 2.00 0 2 -26 25.60 2.20 -2 -2 -26 40.20 2.60 -2 2 -26 40.70 2.40 5 -3 -26 20.80 1.70 5 3 -26 20.50 2.00 3 -3 -26 6.10 1.60 3 -3 -26 8.10 1.40 3 3 -26 4.80 1.30 1 -3 -26 41.40 3.00 -1 -3 -26 13.00 1.70 -1 3 -26 14.50 1.40 4 -4 -26 51.19 2.80 4 -4 -26 51.09 2.50 4 4 -26 45.00 2.50 2 -4 -26 2.40 1.40 2 -4 -26 3.30 1.50 0 -4 -26 -1.90 1.50 -2 -4 -26 5.70 1.20 3 -5 -26 19.90 1.60 3 -5 -26 22.10 1.80 1 -5 -26 11.90 1.60 1 -5 -26 14.10 1.50 -1 -5 -26 18.20 1.50 -1 5 -26 15.40 1.40 2 -6 -26 3.20 1.20 2 -6 -26 3.40 1.30 0 -6 -26 33.60 2.10 0 6 -26 31.80 2.30 4 0 -27 -0.70 1.20 2 0 -27 0.80 1.10 0 0 -27 -0.50 1.20 -2 0 -27 0.90 1.10 3 -1 -27 11.30 1.20 3 -1 -27 6.10 1.30 3 1 -27 6.80 1.30 1 -1 -27 2.30 1.30 1 1 -27 3.30 1.10 -1 -1 -27 3.60 1.30 -1 1 -27 3.80 1.20 4 -2 -27 13.00 1.50 4 2 -27 10.80 1.30 2 -2 -27 72.69 3.10 2 -2 -27 67.99 2.90 0 -2 -27 48.50 2.80 0 2 -27 48.50 2.40 -2 -2 -27 24.50 2.30 3 -3 -27 8.60 1.30 3 -3 -27 7.00 1.40 1 -3 -27 60.49 3.00 -1 -3 -27 53.69 2.80 2 -4 -27 19.10 2.00 2 -4 -27 21.30 1.70 0 -4 -27 77.59 3.30 3 -5 -27 19.10 1.90 1 -5 -27 49.60 2.50 0 0 -28 55.49 2.60 1 -1 -28 106.29 3.80 1 1 -28 102.09 3.90 -1 -1 -28 20.50 1.60 2 -2 -28 63.59 2.70 0 -2 -28 30.00 2.20 1 -3 -28 6.30 1.20 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 62892 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.500000 0.44947(3) 0.250000 0.03924(14) Uani 1 2 d S T P . . O1 O 0.6059(2) 0.38599(14) 0.44416(5) 0.0734(5) Uani 1 1 d . . . . . N1 N 0.63842(19) 0.33862(11) 0.29961(6) 0.0443(3) Uani 1 1 d . . . . . N2 N 0.35657(19) 0.44657(12) 0.31565(7) 0.0470(4) Uani 1 1 d . . . . . N3 N 0.6484(2) 0.56192(13) 0.29496(7) 0.0537(4) Uani 1 1 d . . . . . N4 N 0.78333(19) 0.26712(13) 0.37341(6) 0.0506(4) Uani 1 1 d . . . . . N5 N 0.2826(2) 0.43918(13) 0.40033(7) 0.0576(4) Uani 1 1 d . . . . . N6B N 0.8110(12) 0.6792(7) 0.3571(4) 0.114(4) Uani 0.5 1 d . U . A 2 N6 N 0.7551(10) 0.6754(5) 0.3713(4) 0.087(3) Uani 0.5 1 d . U . A 1 N7B N 0.951(2) 0.6521(15) 0.4496(8) 0.093(5) Uani 0.5 1 d . . . A 2 N7 N 0.973(2) 0.6379(17) 0.4463(8) 0.092(4) Uani 0.5 1 d . . . A 1 C1 C 0.7529(3) 0.27839(16) 0.28201(8) 0.0555(5) Uani 1 1 d . . . . . H1 H 0.768655 0.269249 0.243885 0.067 Uiso 1 1 calc R . . . . C2 C 0.8413(3) 0.23326(17) 0.32694(9) 0.0597(5) Uani 1 1 d . . . . . H2 H 0.927547 0.186737 0.325996 0.072 Uiso 1 1 calc R . . . . C3 C 0.6585(2) 0.33081(13) 0.35564(7) 0.0414(4) Uani 1 1 d . . . . . C4 C 0.5607(2) 0.38116(14) 0.39362(7) 0.0474(4) Uani 1 1 d . . . . . C5 C 0.4029(2) 0.42209(14) 0.36934(7) 0.0454(4) Uani 1 1 d . . . . . C6 C 0.1564(3) 0.4746(2) 0.36444(11) 0.0704(6) Uani 1 1 d . . . . . H6 H 0.054275 0.492563 0.373814 0.084 Uiso 1 1 calc R . . . . C7 C 0.2024(3) 0.4798(2) 0.31276(10) 0.0660(6) Uani 1 1 d . . . . . H7 H 0.137410 0.503089 0.279573 0.079 Uiso 1 1 calc R . . . . C8 C 0.8434(3) 0.2331(2) 0.43130(9) 0.0704(6) Uani 1 1 d . . . . . H8A H 0.883647 0.292404 0.454123 0.106 Uiso 1 1 calc GR . . . . H8B H 0.930208 0.183477 0.430303 0.106 Uiso 1 1 calc GR . . . . H8C H 0.756197 0.200764 0.447895 0.106 Uiso 1 1 calc GR . . . . C9 C 0.2792(4) 0.4191(2) 0.46064(10) 0.0807(7) Uani 1 1 d . . . . . H9A H 0.314425 0.348653 0.469575 0.121 Uiso 1 1 calc GR . . . . H9B H 0.169957 0.428281 0.469185 0.121 Uiso 1 1 calc GR . . . . H9C H 0.351086 0.467145 0.483259 0.121 Uiso 1 1 calc GR . . . . C10 C 0.7161(3) 0.61201(15) 0.32930(9) 0.0580(5) Uani 1 1 d . U . . . C11 C 0.8767(3) 0.65556(18) 0.40874(10) 0.0604(5) Uani 1 1 d . U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0440(2) 0.0432(2) 0.0296(2) 0.000 0.00232(15) 0.000 O1 0.0940(11) 0.0942(12) 0.0300(7) -0.0088(7) 0.0018(7) 0.0173(9) N1 0.0558(8) 0.0464(8) 0.0303(7) -0.0009(5) 0.0049(6) 0.0075(6) N2 0.0468(8) 0.0554(9) 0.0390(8) -0.0047(6) 0.0074(6) 0.0033(6) N3 0.0588(10) 0.0510(9) 0.0478(9) -0.0029(7) -0.0051(8) -0.0038(7) N4 0.0551(9) 0.0577(9) 0.0376(8) 0.0065(6) 0.0014(7) 0.0064(7) N5 0.0680(11) 0.0590(10) 0.0508(10) -0.0113(7) 0.0262(9) -0.0001(8) N6B 0.165(9) 0.070(4) 0.084(5) 0.027(4) -0.063(5) -0.063(5) N6 0.093(5) 0.055(4) 0.101(5) -0.039(4) -0.028(3) 0.027(4) N7B 0.099(10) 0.134(9) 0.044(5) -0.017(5) 0.009(5) -0.036(8) N7 0.057(3) 0.155(9) 0.059(6) -0.043(4) -0.005(4) 0.013(4) C1 0.0707(12) 0.0589(11) 0.0389(9) -0.0015(8) 0.0140(9) 0.0156(10) C2 0.0635(12) 0.0627(12) 0.0541(11) 0.0043(9) 0.0121(9) 0.0183(10) C3 0.0502(9) 0.0427(9) 0.0299(7) -0.0003(6) 0.0009(7) 0.0002(7) C4 0.0631(11) 0.0485(9) 0.0308(8) -0.0041(7) 0.0065(8) -0.0017(8) C5 0.0562(10) 0.0453(9) 0.0366(9) -0.0086(7) 0.0138(8) -0.0028(8) C6 0.0598(13) 0.0781(15) 0.0783(16) -0.0105(12) 0.0272(12) 0.0082(11) C7 0.0514(11) 0.0816(15) 0.0657(13) -0.0018(11) 0.0104(10) 0.0126(11) C8 0.0718(14) 0.0909(17) 0.0446(11) 0.0168(11) -0.0055(10) 0.0181(12) C9 0.106(2) 0.0903(17) 0.0554(13) -0.0081(12) 0.0456(13) 0.0019(15) C10 0.0662(12) 0.0433(10) 0.0587(12) 0.0022(9) -0.0117(10) 0.0018(9) C11 0.0571(13) 0.0689(13) 0.0550(13) -0.0208(10) 0.0077(10) -0.0096(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 93.82(8) 2_655 . ? N1 Co1 N2 94.46(6) . 2_655 ? N1 Co1 N2 84.14(6) 2_655 2_655 ? N1 Co1 N2 84.14(6) . . ? N1 Co1 N2 94.45(6) 2_655 . ? N1 Co1 N3 86.96(6) 2_655 2_655 ? N1 Co1 N3 175.93(6) . 2_655 ? N1 Co1 N3 86.96(6) . . ? N1 Co1 N3 175.93(6) 2_655 . ? N2 Co1 N2 177.95(8) . 2_655 ? N2 Co1 N3 89.60(7) 2_655 2_655 ? N2 Co1 N3 89.60(7) . . ? N2 Co1 N3 91.82(7) 2_655 . ? N2 Co1 N3 91.82(7) . 2_655 ? N3 Co1 N3 92.54(9) 2_655 . ? C1 N1 Co1 125.51(12) . . ? C3 N1 Co1 126.86(12) . . ? C3 N1 C1 105.92(15) . . ? C5 N2 Co1 127.11(13) . . ? C5 N2 C7 105.83(17) . . ? C7 N2 Co1 126.74(15) . . ? C10 N3 Co1 164.43(18) . . ? C2 N4 C3 107.18(15) . . ? C2 N4 C8 124.06(18) . . ? C3 N4 C8 128.65(17) . . ? C5 N5 C9 128.9(2) . . ? C6 N5 C5 106.87(18) . . ? C6 N5 C9 124.2(2) . . ? C10 N6B C11 118.0(6) . . ? C11 N6 C10 119.9(5) . . ? N1 C1 H1 125.1 . . ? C2 C1 N1 109.87(16) . . ? C2 C1 H1 125.1 . . ? N4 C2 C1 106.89(18) . . ? N4 C2 H2 126.6 . . ? C1 C2 H2 126.6 . . ? N1 C3 N4 110.12(15) . . ? N1 C3 C4 126.04(16) . . ? N4 C3 C4 123.83(15) . . ? O1 C4 C3 121.02(18) . . ? O1 C4 C5 120.75(17) . . ? C3 C4 C5 118.18(14) . . ? N2 C5 N5 110.50(18) . . ? N2 C5 C4 126.42(16) . . ? N5 C5 C4 123.08(17) . . ? N5 C6 H6 126.3 . . ? C7 C6 N5 107.3(2) . . ? C7 C6 H6 126.3 . . ? N2 C7 H7 125.3 . . ? C6 C7 N2 109.5(2) . . ? C6 C7 H7 125.3 . . ? N4 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? N4 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N5 C9 H9A 109.5 . . ? N5 C9 H9B 109.5 . . ? N5 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N3 C10 N6B 164.4(5) . . ? N3 C10 N6 164.6(4) . . ? N7B C11 N6B 165.5(10) . . ? N7 C11 N6 172.3(10) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 2.1153(14) 2_655 ? Co1 N1 2.1154(14) . ? Co1 N2 2.1179(15) . ? Co1 N2 2.1180(15) 2_655 ? Co1 N3 2.1208(16) 2_655 ? Co1 N3 2.1208(17) . ? O1 C4 1.219(2) . ? N1 C1 1.358(2) . ? N1 C3 1.334(2) . ? N2 C5 1.331(2) . ? N2 C7 1.364(3) . ? N3 C10 1.139(3) . ? N4 C2 1.353(3) . ? N4 C3 1.361(2) . ? N4 C8 1.477(2) . ? N5 C5 1.358(3) . ? N5 C6 1.353(3) . ? N5 C9 1.474(3) . ? N6B C10 1.305(9) . ? N6B C11 1.319(9) . ? N6 C10 1.308(8) . ? N6 C11 1.290(9) . ? N7B C11 1.085(18) . ? N7 C11 1.148(19) . ? C1 H1 0.9500 . ? C1 C2 1.355(3) . ? C2 H2 0.9500 . ? C3 C4 1.468(3) . ? C4 C5 1.475(3) . ? C6 H6 0.9500 . ? C6 C7 1.352(3) . ? 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 . ?