#------------------------------------------------------------------------------ #$Date: 2023-11-28 01:41:14 +0200 (Tue, 28 Nov 2023) $ #$Revision: 287819 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/77/7247796.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_7247796 loop_ _publ_author_name 'Yang, Yuanyu' 'Xue, Jian-Hua' 'Yang, Dong-Dong' 'Zhang, Liyang' 'Ma, Qi' 'Zhao, Xuan' _publ_section_title ; Effects of solvents and metal ions on the synthesis, structural diversity and magnetic properties of 5'-nitro-[1,1':3',1''-terphenyl]-3,3'',5,5''-tetracarboxylic acid ligand and a highly sensitive sensor for Fe3+ ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D3CE01076G _journal_year 2023 _chemical_formula_sum 'C54 H36 Co4 N4 O25' _chemical_formula_weight 1376.59 _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 mixed _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2020-07-25 deposited with the CCDC. 2023-11-27 downloaded from the CCDC. ; _cell_angle_alpha 107.389(3) _cell_angle_beta 91.634(3) _cell_angle_gamma 107.736(3) _cell_formula_units_Z 1 _cell_length_a 9.3660(7) _cell_length_b 10.5136(8) _cell_length_c 15.0815(12) _cell_measurement_reflns_used 9930 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 31.45 _cell_measurement_theta_min 2.97 _cell_volume 1338.12(18) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014 (Sheldrick 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_unetI/netI 0.0530 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 30150 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.050 _diffrn_reflns_theta_min 2.968 _exptl_absorpt_coefficient_mu 1.313 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour pink _exptl_crystal_density_diffrn 1.708 _exptl_crystal_description block _exptl_crystal_F_000 696 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_transmission_factor_max 0.7463 _exptl_transmission_factor_min 0.6727 _refine_diff_density_max 2.050 _refine_diff_density_min -2.223 _refine_diff_density_rms 0.162 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 397 _refine_ls_number_reflns 9236 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.059 _refine_ls_R_factor_all 0.1134 _refine_ls_R_factor_gt 0.0662 _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^)+(0.1374P)^2^+1.6476P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2087 _refine_ls_wR_factor_ref 0.2401 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5890 _reflns_number_total 9236 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce01076g2.cif _cod_data_source_block complex1 _cod_database_code 7247796 _shelx_shelxl_version_number 2014/7 _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_res_file ; L78+CO-1.res created by SHELXL-2014/7 TITL L78+CO-1 in P-1 CELL 0.71073 9.36600 10.51360 15.08150 107.3893 91.6339 107.7359 ZERR 1.00 0.00070 0.00080 0.00120 0.0028 0.0030 0.0025 LATT 1 SFAC C H N O Co UNIT 54 36 4 25 4 L.S. 8 ACTA BOND FMAP 2 PLAN 5 DFIX 0.82 0.01 O11 H11A O11 H11B DFIX 1.32 0.01 H11A H11B TEMP 24.880 WGHT 0.137400 1.647600 FVAR 0.21952 MOLE 1 CO1 5 1.167752 1.418741 0.363853 11.00000 0.01710 0.01356 = 0.03711 -0.00036 -0.00288 0.00358 CO2 5 0.029026 1.127084 0.181085 11.00000 0.03556 0.02064 = 0.07307 -0.00126 -0.02156 0.01048 C1 1 0.040376 0.148647 -0.181999 11.00000 0.03686 0.01845 = 0.05732 -0.00331 -0.00156 0.00554 C2 1 0.079744 0.305537 -0.132581 11.00000 0.02949 0.01702 = 0.04158 0.00083 0.00081 0.00532 C3 1 0.015600 0.383309 -0.171344 11.00000 0.02926 0.02342 = 0.03446 -0.00075 -0.00205 0.00494 AFIX 43 H3 2 -0.053469 0.338810 -0.225670 11.00000 -1.20000 AFIX 0 C4 1 0.055829 0.527971 -0.128048 11.00000 0.02918 0.02072 = 0.03242 0.00301 0.00269 0.00916 C5 1 -0.008865 0.613784 -0.171244 11.00000 0.03251 0.02809 = 0.03215 0.00655 0.00301 0.01195 C6 1 0.159805 0.594352 -0.046805 11.00000 0.03164 0.01588 = 0.03007 0.00070 -0.00241 0.00586 AFIX 43 H6 2 0.185939 0.691436 -0.018634 11.00000 -1.20000 AFIX 0 C7 1 0.225606 0.518324 -0.006770 11.00000 0.02363 0.01677 = 0.03052 0.00154 -0.00033 0.00488 C8 1 0.182207 0.372033 -0.051287 11.00000 0.02885 0.01768 = 0.04075 0.00334 -0.00104 0.00643 AFIX 43 H8 2 0.223029 0.318433 -0.025737 11.00000 -1.20000 AFIX 0 C9 1 0.341070 0.588964 0.077738 11.00000 0.02383 0.01706 = 0.03318 0.00340 0.00019 0.00536 C10 1 0.417412 0.514159 0.111935 11.00000 0.03377 0.01603 = 0.03685 0.00584 0.00231 0.00757 AFIX 43 H10 2 0.394551 0.417573 0.082967 11.00000 -1.20000 AFIX 0 C11 1 0.526326 0.584508 0.188591 11.00000 0.02739 0.02341 = 0.03577 0.01227 0.00371 0.01107 C12 1 0.568118 0.727711 0.235229 11.00000 0.02571 0.02313 = 0.03451 0.00760 -0.00087 0.00660 AFIX 43 H12 2 0.643626 0.771499 0.286351 11.00000 -1.20000 AFIX 0 C13 1 0.492579 0.804400 0.202665 11.00000 0.02104 0.01623 = 0.03734 0.00440 0.00013 0.00583 C14 1 0.381093 0.733658 0.125518 11.00000 0.02530 0.01577 = 0.03951 0.00184 -0.00456 0.00699 AFIX 43 H14 2 0.330668 0.785222 0.104692 11.00000 -1.20000 AFIX 0 C15 1 0.534038 0.958949 0.247954 11.00000 0.01871 0.01650 = 0.03578 0.00135 -0.00308 0.00426 C16 1 0.425167 1.025819 0.253099 11.00000 0.01702 0.02018 = 0.04434 0.00217 -0.00242 0.00417 AFIX 43 H16 2 0.324877 0.971775 0.229887 11.00000 -1.20000 AFIX 0 C17 1 0.462980 1.170216 0.291829 11.00000 0.01708 0.02086 = 0.03366 0.00258 0.00067 0.00796 C18 1 0.611932 1.252856 0.326854 11.00000 0.01957 0.01700 = 0.03241 0.00384 0.00163 0.00707 AFIX 43 H18 2 0.637137 1.349908 0.354762 11.00000 -1.20000 AFIX 0 C19 1 0.723028 1.189241 0.319833 11.00000 0.01673 0.01815 = 0.03176 0.00271 -0.00103 0.00400 C20 1 0.684891 1.043177 0.282005 11.00000 0.01888 0.01812 = 0.03619 0.00305 -0.00117 0.00685 AFIX 43 H20 2 0.759724 1.001359 0.279318 11.00000 -1.20000 AFIX 0 C21 1 0.886272 1.277300 0.345706 11.00000 0.01740 0.02066 = 0.03370 0.00588 -0.00273 0.00439 C22 1 1.440633 1.680335 0.447046 11.00000 0.02606 0.01568 = 0.04464 0.00331 -0.00189 0.00358 AFIX 43 H22 2 1.488694 1.614568 0.446079 11.00000 -1.20000 AFIX 0 C23 1 1.226068 1.729960 0.419682 11.00000 0.02315 0.01854 = 0.06085 0.00385 -0.01060 0.00141 AFIX 43 H23 2 1.123032 1.699383 0.399161 11.00000 -1.20000 AFIX 0 C24 1 1.302546 1.873265 0.451259 11.00000 0.02714 0.01714 = 0.06550 0.00445 -0.01028 0.00346 AFIX 43 H24 2 1.251084 1.936422 0.451871 11.00000 -1.20000 AFIX 0 C25 1 1.456825 1.922963 0.482167 11.00000 0.02579 0.01434 = 0.02739 0.00137 -0.00145 -0.00005 C26 1 1.525900 1.822232 0.479380 11.00000 0.02189 0.01773 = 0.04472 0.00290 -0.00337 0.00153 AFIX 43 H26 2 1.628915 1.850039 0.499146 11.00000 -1.20000 AFIX 0 C27 1 0.341966 1.234732 0.286727 11.00000 0.01686 0.02445 = 0.04548 0.00369 0.00180 0.00676 N1 3 0.607719 0.503570 0.222237 11.00000 0.03969 0.02944 = 0.04507 0.01739 0.00364 0.01470 N2 3 1.291327 1.633171 0.416937 11.00000 0.02330 0.01398 = 0.03453 0.00285 -0.00284 0.00050 O1 4 0.072971 0.076891 -0.134738 11.00000 0.05173 0.01859 = 0.06712 -0.00163 -0.00754 0.00952 O2 4 -0.020745 0.098125 -0.264188 11.00000 0.10387 0.03434 = 0.06234 -0.01682 -0.02886 0.01763 O3 4 -0.110510 0.551364 -0.238627 11.00000 0.03290 0.03436 = 0.04410 0.01312 -0.00738 0.00482 O4 4 0.047580 0.746930 -0.135053 11.00000 0.06035 0.02726 = 0.04546 0.00128 -0.01536 0.01534 O5 4 0.584361 0.380869 0.174864 11.00000 0.07397 0.03453 = 0.05719 0.02014 0.00882 0.03102 O6 4 0.694793 0.564656 0.295033 11.00000 0.05692 0.04515 = 0.06715 0.02259 -0.02016 0.01438 O7 4 0.235956 1.163856 0.220230 11.00000 0.02792 0.04816 = 0.06886 -0.01392 -0.01338 0.01900 O8 4 0.351354 1.350965 0.344388 11.00000 0.02445 0.02574 = 0.05275 -0.00186 -0.00362 0.01346 O9 4 0.986460 1.218264 0.319361 11.00000 0.01780 0.02065 = 0.04930 0.00273 -0.00105 0.00506 O10 4 0.927929 1.406538 0.388216 11.00000 0.02200 0.01943 = 0.04713 -0.00162 -0.00267 0.00396 O11 4 1.188595 1.400044 0.500305 11.00000 0.04321 0.03591 = 0.03909 0.00661 -0.00160 0.01475 AFIX 3 H11B 2 1.150706 1.431992 0.546388 11.00000 -1.50000 H11A 2 1.275674 1.453646 0.506910 11.00000 -1.50000 AFIX 0 O13 4 0.914700 0.909735 0.548147 11.00000 0.09326 0.09549 = 0.10508 0.05050 -0.00049 0.03190 AFIX 3 H13A 2 0.906214 0.929302 0.604169 11.00000 -1.50000 H13B 2 0.850797 0.832468 0.521347 11.00000 -1.50000 AFIX 0 O12 4 0.142467 1.111814 0.049651 10.50000 0.07213 0.10125 = 0.04253 0.03311 0.02029 0.05397 AFIX 3 H12A 2 0.146195 1.110763 -0.004804 10.50000 -1.50000 H12B 2 0.227866 1.123381 0.072406 10.50000 -1.50000 AFIX 0 HKLF 4 REM L78+CO-1 in P-1 REM R1 = 0.0662 for 5890 Fo > 4sig(Fo) and 0.1134 for all 9236 data REM 397 parameters refined using 3 restraints END WGHT 0.1391 1.4863 REM Highest difference peak 2.050, deepest hole -2.223, 1-sigma level 0.162 Q1 1 0.3380 0.9615 0.0014 11.00000 0.05 2.05 Q2 1 0.5000 1.0000 0.0000 10.50000 0.05 1.96 Q3 1 0.3867 1.0110 0.0007 11.00000 0.05 1.82 Q4 1 0.0530 1.0350 0.0387 11.00000 0.05 1.15 Q5 1 0.9095 0.8504 0.4410 11.00000 0.05 1.05 ; _shelx_res_checksum 55046 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 1.16775(5) 1.41874(4) 0.36385(3) 0.02507(15) Uani 1 1 d . . . . . Co2 Co 0.02903(7) 1.12708(6) 0.18109(5) 0.0472(2) Uani 1 1 d . . . . . C1 C 0.0404(5) 0.1486(4) -0.1820(3) 0.0422(10) Uani 1 1 d . . . . . C2 C 0.0797(4) 0.3055(4) -0.1326(3) 0.0320(8) Uani 1 1 d . . . . . C3 C 0.0156(4) 0.3833(4) -0.1713(3) 0.0324(8) Uani 1 1 d . . . . . H3 H -0.0535 0.3388 -0.2257 0.039 Uiso 1 1 calc R U . . . C4 C 0.0558(4) 0.5280(4) -0.1280(3) 0.0285(7) Uani 1 1 d . . . . . C5 C -0.0089(4) 0.6138(4) -0.1712(3) 0.0312(7) Uani 1 1 d . . . . . C6 C 0.1598(4) 0.5944(4) -0.0468(3) 0.0280(7) Uani 1 1 d . . . . . H6 H 0.1859 0.6914 -0.0186 0.034 Uiso 1 1 calc R U . . . C7 C 0.2256(4) 0.5183(3) -0.0068(3) 0.0256(6) Uani 1 1 d . . . . . C8 C 0.1822(4) 0.3720(4) -0.0513(3) 0.0309(7) Uani 1 1 d . . . . . H8 H 0.2230 0.3184 -0.0257 0.037 Uiso 1 1 calc R U . . . C9 C 0.3411(4) 0.5890(3) 0.0777(3) 0.0262(7) Uani 1 1 d . . . . . C10 C 0.4174(4) 0.5142(4) 0.1119(3) 0.0297(7) Uani 1 1 d . . . . . H10 H 0.3946 0.4176 0.0830 0.036 Uiso 1 1 calc R U . . . C11 C 0.5263(4) 0.5845(4) 0.1886(3) 0.0276(7) Uani 1 1 d . . . . . C12 C 0.5681(4) 0.7277(4) 0.2352(3) 0.0286(7) Uani 1 1 d . . . . . H12 H 0.6436 0.7715 0.2864 0.034 Uiso 1 1 calc R U . . . C13 C 0.4926(4) 0.8044(3) 0.2027(3) 0.0260(7) Uani 1 1 d . . . . . C14 C 0.3811(4) 0.7337(3) 0.1255(3) 0.0286(7) Uani 1 1 d . . . . . H14 H 0.3307 0.7852 0.1047 0.034 Uiso 1 1 calc R U . . . C15 C 0.5340(4) 0.9589(3) 0.2480(3) 0.0258(7) Uani 1 1 d . . . . . C16 C 0.4252(4) 1.0258(4) 0.2531(3) 0.0297(7) Uani 1 1 d . . . . . H16 H 0.3249 0.9718 0.2299 0.036 Uiso 1 1 calc R U . . . C17 C 0.4630(4) 1.1702(3) 0.2918(3) 0.0250(6) Uani 1 1 d . . . . . C18 C 0.6119(4) 1.2529(3) 0.3269(2) 0.0237(6) Uani 1 1 d . . . . . H18 H 0.6371 1.3499 0.3548 0.028 Uiso 1 1 calc R U . . . C19 C 0.7230(3) 1.1892(3) 0.3198(2) 0.0240(6) Uani 1 1 d . . . . . C20 C 0.6849(4) 1.0432(3) 0.2820(3) 0.0257(7) Uani 1 1 d . . . . . H20 H 0.7597 1.0014 0.2793 0.031 Uiso 1 1 calc R U . . . C21 C 0.8863(4) 1.2773(4) 0.3457(3) 0.0252(6) Uani 1 1 d . . . . . C22 C 1.4406(4) 1.6803(4) 0.4470(3) 0.0312(7) Uani 1 1 d . . . . . H22 H 1.4887 1.6146 0.4461 0.037 Uiso 1 1 calc R U . . . C23 C 1.2261(4) 1.7300(4) 0.4197(3) 0.0379(9) Uani 1 1 d . . . . . H23 H 1.1230 1.6994 0.3992 0.045 Uiso 1 1 calc R U . . . C24 C 1.3025(4) 1.8733(4) 0.4513(3) 0.0399(10) Uani 1 1 d . . . . . H24 H 1.2511 1.9364 0.4519 0.048 Uiso 1 1 calc R U . . . C25 C 1.4568(4) 1.9230(3) 0.4822(2) 0.0255(6) Uani 1 1 d . . . . . C26 C 1.5259(4) 1.8222(4) 0.4794(3) 0.0311(8) Uani 1 1 d . . . . . H26 H 1.6289 1.8500 0.4991 0.037 Uiso 1 1 calc R U . . . C27 C 0.3420(4) 1.2347(4) 0.2867(3) 0.0308(8) Uani 1 1 d . . . . . N1 N 0.6077(4) 0.5036(4) 0.2222(3) 0.0361(7) Uani 1 1 d . . . . . N2 N 1.2913(3) 1.6332(3) 0.4169(2) 0.0266(6) Uani 1 1 d . . . . . O1 O 0.0730(4) 0.0769(3) -0.1347(3) 0.0502(8) Uani 1 1 d . . . . . O2 O -0.0207(6) 0.0981(4) -0.2642(3) 0.0765(14) Uani 1 1 d . . . . . O3 O -0.1105(3) 0.5514(3) -0.2386(2) 0.0388(6) Uani 1 1 d . . . . . O4 O 0.0476(4) 0.7469(3) -0.1351(2) 0.0470(8) Uani 1 1 d . . . . . O5 O 0.5844(5) 0.3809(3) 0.1749(3) 0.0508(8) Uani 1 1 d . . . . . O6 O 0.6948(4) 0.5647(4) 0.2950(3) 0.0565(10) Uani 1 1 d . . . . . O7 O 0.2360(3) 1.1639(4) 0.2202(3) 0.0548(10) Uani 1 1 d . . . . . O8 O 0.3514(3) 1.3510(3) 0.3444(2) 0.0366(6) Uani 1 1 d . . . . . O9 O 0.9865(3) 1.2183(3) 0.3194(2) 0.0317(6) Uani 1 1 d . . . . . O10 O 0.9279(3) 1.4065(3) 0.3882(2) 0.0332(6) Uani 1 1 d . . . . . O11 O 1.1886(4) 1.4000(3) 0.5003(2) 0.0404(7) Uani 1 1 d D . . . . H11B H 1.1507 1.4320 0.5464 0.061 Uiso 1 1 d DR U . . . H11A H 1.2757 1.4536 0.5069 0.061 Uiso 1 1 d DR U . . . O13 O 0.9147(7) 0.9097(6) 0.5481(4) 0.0938(16) Uani 1 1 d . . . . . H13A H 0.9062 0.9293 0.6042 0.141 Uiso 1 1 d R U . . . H13B H 0.8508 0.8325 0.5213 0.141 Uiso 1 1 d R U . . . O12 O 0.1425(10) 1.1118(10) 0.0497(5) 0.063(2) Uani 0.5 1 d . . P . . H12A H 0.1462 1.1108 -0.0048 0.095 Uiso 0.5 1 d R U P . . H12B H 0.2279 1.1234 0.0724 0.095 Uiso 0.5 1 d R U P . . 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 0.0171(2) 0.0136(2) 0.0371(3) -0.00036(17) -0.00288(17) 0.00358(15) Co2 0.0356(3) 0.0206(3) 0.0731(5) -0.0013(3) -0.0216(3) 0.0105(2) C1 0.037(2) 0.0185(16) 0.057(3) -0.0033(17) -0.0016(19) 0.0055(15) C2 0.0295(17) 0.0170(14) 0.042(2) 0.0008(14) 0.0008(15) 0.0053(13) C3 0.0293(17) 0.0234(16) 0.0345(18) -0.0008(14) -0.0020(14) 0.0049(13) C4 0.0292(16) 0.0207(15) 0.0324(17) 0.0030(13) 0.0027(14) 0.0092(13) C5 0.0325(18) 0.0281(17) 0.0322(18) 0.0066(14) 0.0030(15) 0.0120(15) C6 0.0316(17) 0.0159(13) 0.0301(17) 0.0007(12) -0.0024(14) 0.0059(12) C7 0.0236(14) 0.0168(14) 0.0305(16) 0.0015(12) -0.0003(13) 0.0049(12) C8 0.0288(17) 0.0177(14) 0.041(2) 0.0033(14) -0.0010(15) 0.0064(13) C9 0.0238(14) 0.0171(14) 0.0332(17) 0.0034(12) 0.0002(13) 0.0054(12) C10 0.0338(17) 0.0160(14) 0.0368(19) 0.0058(13) 0.0023(15) 0.0076(13) C11 0.0274(16) 0.0234(15) 0.0358(18) 0.0123(14) 0.0037(14) 0.0111(13) C12 0.0257(15) 0.0231(15) 0.0345(18) 0.0076(14) -0.0009(14) 0.0066(13) C13 0.0210(14) 0.0162(13) 0.0373(18) 0.0044(13) 0.0001(13) 0.0058(11) C14 0.0253(15) 0.0158(14) 0.0395(19) 0.0018(13) -0.0046(14) 0.0070(12) C15 0.0187(13) 0.0165(13) 0.0358(18) 0.0013(12) -0.0031(12) 0.0043(11) C16 0.0170(13) 0.0202(15) 0.044(2) 0.0022(14) -0.0024(13) 0.0042(12) C17 0.0171(13) 0.0209(14) 0.0337(17) 0.0026(13) 0.0007(12) 0.0080(11) C18 0.0196(13) 0.0170(13) 0.0324(17) 0.0038(12) 0.0016(12) 0.0071(11) C19 0.0167(13) 0.0181(14) 0.0318(16) 0.0027(12) -0.0010(12) 0.0040(11) C20 0.0189(13) 0.0181(14) 0.0362(18) 0.0030(13) -0.0012(12) 0.0069(11) C21 0.0174(13) 0.0207(14) 0.0337(17) 0.0059(13) -0.0027(12) 0.0044(11) C22 0.0261(16) 0.0157(14) 0.045(2) 0.0033(14) -0.0019(15) 0.0036(12) C23 0.0231(16) 0.0185(15) 0.061(3) 0.0039(16) -0.0106(16) 0.0014(13) C24 0.0271(17) 0.0171(15) 0.066(3) 0.0044(17) -0.0103(18) 0.0035(13) C25 0.0258(15) 0.0143(13) 0.0274(16) 0.0014(12) -0.0015(13) 0.0000(12) C26 0.0219(15) 0.0177(14) 0.045(2) 0.0029(14) -0.0034(14) 0.0015(12) C27 0.0169(13) 0.0244(16) 0.045(2) 0.0037(15) 0.0018(14) 0.0068(12) N1 0.0397(18) 0.0294(16) 0.0451(19) 0.0174(14) 0.0036(15) 0.0147(14) N2 0.0233(13) 0.0140(11) 0.0345(15) 0.0028(11) -0.0028(11) 0.0005(10) O1 0.0517(19) 0.0186(13) 0.067(2) -0.0016(13) -0.0075(16) 0.0095(13) O2 0.104(4) 0.0343(18) 0.062(2) -0.0168(17) -0.029(2) 0.018(2) O3 0.0329(14) 0.0344(15) 0.0441(16) 0.0131(13) -0.0074(12) 0.0048(12) O4 0.060(2) 0.0273(14) 0.0455(17) 0.0013(12) -0.0154(15) 0.0153(14) O5 0.074(2) 0.0345(16) 0.057(2) 0.0201(15) 0.0088(18) 0.0310(17) O6 0.057(2) 0.0451(19) 0.067(2) 0.0226(17) -0.0202(18) 0.0144(17) O7 0.0279(14) 0.0482(19) 0.069(2) -0.0139(16) -0.0134(14) 0.0190(14) O8 0.0244(12) 0.0257(12) 0.0527(17) -0.0019(12) -0.0036(11) 0.0135(10) O9 0.0178(10) 0.0207(11) 0.0493(16) 0.0027(11) -0.0010(10) 0.0051(9) O10 0.0220(11) 0.0194(11) 0.0471(16) -0.0016(11) -0.0027(11) 0.0040(9) O11 0.0432(16) 0.0359(15) 0.0391(15) 0.0066(12) -0.0016(13) 0.0148(13) O13 0.093(4) 0.095(4) 0.105(4) 0.050(3) 0.000(3) 0.032(3) O12 0.072(5) 0.101(7) 0.043(4) 0.033(4) 0.020(4) 0.054(5) 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' 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' Co Co 0.3494 0.9721 '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 O8 Co1 N2 95.94(12) 1_655 . ? O8 Co1 O3 105.73(13) 1_655 2_675 ? N2 Co1 O3 88.61(12) . 2_675 ? O8 Co1 O11 85.56(13) 1_655 . ? N2 Co1 O11 90.60(12) . . ? O3 Co1 O11 168.71(13) 2_675 . ? O8 Co1 O9 100.32(10) 1_655 . ? N2 Co1 O9 163.65(11) . . ? O3 Co1 O9 88.67(11) 2_675 . ? O11 Co1 O9 88.93(12) . . ? O8 Co1 O10 157.31(11) 1_655 . ? N2 Co1 O10 104.59(11) . . ? O3 Co1 O10 84.62(12) 2_675 . ? O11 Co1 O10 84.69(12) . . ? O9 Co1 O10 59.10(9) . . ? O7 Co2 O1 108.91(15) . 2_565 ? O7 Co2 O4 124.15(17) . 2_575 ? O1 Co2 O4 120.64(15) 2_565 2_575 ? O7 Co2 O9 92.97(13) . 1_455 ? O1 Co2 O9 111.61(14) 2_565 1_455 ? O4 Co2 O9 91.56(13) 2_575 1_455 ? O7 Co2 O12 74.5(2) . . ? O1 Co2 O12 89.7(3) 2_565 . ? O4 Co2 O12 81.3(2) 2_575 . ? O9 Co2 O12 158.1(3) 1_455 . ? O2 C1 O1 124.2(4) . . ? O2 C1 C2 119.1(4) . . ? O1 C1 C2 116.7(4) . . ? C3 C2 C8 120.3(3) . . ? C3 C2 C1 119.2(4) . . ? C8 C2 C1 120.5(4) . . ? C2 C3 C4 119.3(4) . . ? C3 C4 C6 120.2(3) . . ? C3 C4 C5 119.7(3) . . ? C6 C4 C5 120.1(3) . . ? O3 C5 O4 125.0(4) . . ? O3 C5 C4 118.8(3) . . ? O4 C5 C4 116.2(3) . . ? C4 C6 C7 121.5(3) . . ? C6 C7 C8 117.3(3) . . ? C6 C7 C9 121.8(3) . . ? C8 C7 C9 120.8(3) . . ? C2 C8 C7 121.5(3) . . ? C10 C9 C14 116.8(3) . . ? C10 C9 C7 121.5(3) . . ? C14 C9 C7 121.7(3) . . ? C11 C10 C9 119.5(3) . . ? C10 C11 C12 124.0(3) . . ? C10 C11 N1 118.5(3) . . ? C12 C11 N1 117.5(3) . . ? C11 C12 C13 117.5(3) . . ? C14 C13 C12 118.9(3) . . ? C14 C13 C15 120.7(3) . . ? C12 C13 C15 120.4(3) . . ? C13 C14 C9 123.3(3) . . ? C16 C15 C20 118.1(3) . . ? C16 C15 C13 120.8(3) . . ? C20 C15 C13 121.0(3) . . ? C17 C16 C15 121.5(3) . . ? C16 C17 C18 120.2(3) . . ? C16 C17 C27 118.0(3) . . ? C18 C17 C27 121.5(3) . . ? C17 C18 C19 119.4(3) . . ? C18 C19 C20 120.5(3) . . ? C18 C19 C21 120.3(3) . . ? C20 C19 C21 119.0(3) . . ? C19 C20 C15 120.3(3) . . ? O10 C21 O9 119.1(3) . . ? O10 C21 C19 122.3(3) . . ? O9 C21 C19 118.6(3) . . ? N2 C22 C26 123.0(3) . . ? N2 C23 C24 123.7(4) . . ? C23 C24 C25 119.8(4) . . ? C26 C25 C24 116.8(3) . . ? C26 C25 C25 121.8(4) . 2_896 ? C24 C25 C25 121.4(4) . 2_896 ? C22 C26 C25 119.7(3) . . ? O8 C27 O7 124.6(3) . . ? O8 C27 C17 120.5(3) . . ? O7 C27 C17 114.9(3) . . ? O5 N1 O6 124.5(4) . . ? O5 N1 C11 117.8(4) . . ? O6 N1 C11 117.7(3) . . ? C23 N2 C22 116.9(3) . . ? C23 N2 Co1 120.9(2) . . ? C22 N2 Co1 122.1(2) . . ? C1 O1 Co2 117.1(3) . 2_565 ? C5 O3 Co1 136.2(3) . 2_675 ? C5 O4 Co2 121.0(3) . 2_575 ? C27 O7 Co2 143.7(3) . . ? C27 O8 Co1 121.8(2) . 1_455 ? C21 O9 Co2 128.7(2) . 1_655 ? C21 O9 Co1 92.3(2) . . ? Co2 O9 Co1 101.34(11) 1_655 . ? C21 O10 Co1 89.1(2) . . ? 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 O8 2.050(3) 1_655 ? Co1 N2 2.084(3) . ? Co1 O3 2.086(3) 2_675 ? Co1 O11 2.134(3) . ? Co1 O9 2.165(3) . ? Co1 O10 2.258(3) . ? Co2 O7 1.896(3) . ? Co2 O1 1.954(3) 2_565 ? Co2 O4 1.963(3) 2_575 ? Co2 O9 2.124(3) 1_455 ? Co2 O12 2.262(7) . ? C1 O2 1.236(6) . ? C1 O1 1.273(6) . ? C1 C2 1.514(5) . ? C2 C3 1.391(6) . ? C2 C8 1.387(5) . ? C3 C4 1.387(5) . ? C4 C6 1.394(5) . ? C4 C5 1.506(5) . ? C5 O3 1.239(5) . ? C5 O4 1.270(5) . ? C6 C7 1.397(5) . ? C7 C8 1.403(5) . ? C7 C9 1.487(5) . ? C9 C10 1.400(5) . ? C9 C14 1.399(5) . ? C10 C11 1.373(5) . ? C11 C12 1.381(5) . ? C11 N1 1.481(5) . ? C12 C13 1.399(5) . ? C13 C14 1.392(5) . ? C13 C15 1.481(4) . ? C15 C16 1.396(5) . ? C15 C20 1.403(4) . ? C16 C17 1.379(5) . ? C17 C18 1.388(4) . ? C17 C27 1.498(5) . ? C18 C19 1.389(4) . ? C19 C20 1.393(4) . ? C19 C21 1.495(4) . ? C21 O10 1.246(4) . ? C21 O9 1.285(4) . ? C22 N2 1.347(5) . ? C22 C26 1.385(5) . ? C23 N2 1.329(5) . ? C23 C24 1.380(5) . ? C24 C25 1.391(5) . ? C25 C26 1.391(5) . ? C25 C25 1.491(6) 2_896 ? C27 O8 1.246(4) . ? C27 O7 1.262(5) . ? N1 O5 1.221(5) . ? N1 O6 1.221(5) . ? O1 Co2 1.954(3) 2_565 ? O3 Co1 2.086(3) 2_675 ? O4 Co2 1.963(3) 2_575 ? O8 Co1 2.050(3) 1_455 ? O9 Co2 2.124(3) 1_655 ?