#------------------------------------------------------------------------------ #$Date: 2024-04-02 01:39:53 +0300 (Tue, 02 Apr 2024) $ #$Revision: 290718 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/83/7248366.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_7248366 loop_ _publ_author_name 'Sahoo, Subham' 'Patra, Rajesh' 'Sarma, Debajit' _publ_section_title ; Coordinatively Unsaturated 5-Nitroisophthalate based Cobalt(II) Coordination Polymers: Efficient Catalytic CO2 Fixation and Hantzsch Condensation ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D4CE00102H _journal_year 2024 _chemical_formula_sum 'C20 H15 Co N7 O7' _chemical_formula_weight 524.32 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2024-01-16 deposited with the CCDC. 2024-04-01 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 95.5580(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.0760(3) _cell_length_b 14.6490(5) _cell_length_c 16.6993(6) _cell_measurement_reflns_used 4473 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 26.407 _cell_measurement_theta_min 2.649 _cell_volume 2209.81(13) _computing_cell_refinement 'SAINT V8.37A (Bruker, 2016)' _computing_data_collection 'Apex4 v2022 (Bruker, 2022)' _computing_data_reduction 'SAINT V8.37A (Bruker, 2016)' _computing_molecular_graphics 'Ortep-3 for windows (Farrugia, 1999)' _computing_publication_material 'PLATON (Spek, 2003)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 273(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_device_type 'Bruker D8 Quest PHOTON II diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0623 _diffrn_reflns_av_unetI/netI 0.0479 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 38040 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.407 _diffrn_reflns_theta_min 2.649 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.835 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1068 _exptl_crystal_size_max 0.285 _exptl_crystal_size_mid 0.182 _exptl_crystal_size_min 0.156 _exptl_transmission_factor_max 0.881 _exptl_transmission_factor_min 0.797 _refine_diff_density_max 0.356 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.078 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.186 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 322 _refine_ls_number_reflns 4473 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.186 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0624 _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^)+4.7137P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0908 _refine_ls_wR_factor_ref 0.1022 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3396 _reflns_number_total 4473 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00102h2.cif _cod_data_source_block SSICG-7 _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7248366 _shelx_shelxl_version_number 2018/3 _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 0.797 _shelx_estimated_absorpt_t_max 0.881 _shelx_res_file ; TITL CoNA1_2_0m_a.res in P2(1)/c shelx.res created by SHELXL-2018/3 at 16:32:51 on 15-Nov-2023 CELL 0.71073 9.0760 14.6490 16.6993 90.000 95.558 90.000 ZERR 4.00 0.0003 0.0005 0.0006 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H CO N O UNIT 80 60 4 28 28 MERG 2 OMIT 1 0 0 OMIT 0 0 2 OMIT 11 4 0 OMIT 5 10 13 OMIT -11 3 5 OMIT 4 16 4 OMIT -9 11 2 OMIT -10 6 4 OMIT -10 7 5 OMIT -4 16 7 OMIT -6 15 1 OMIT 7 14 2 OMIT 7 10 2 OMIT 5 15 5 OMIT 11 2 1 OMIT -8 12 7 OMIT 7 6 13 OMIT 8 11 1 OMIT -5 7 17 OMIT 8 11 4 OMIT -8 8 12 OMIT 10 6 5 OMIT -11 2 5 OMIT -11 4 1 OMIT -7 12 9 OMIT -7 11 7 OMIT 10 8 0 OMIT 9 11 0 OMIT 4 7 17 OMIT -11 1 3 OMIT -3 16 7 OMIT -6 9 15 OMIT -8 11 1 OMIT -10 8 5 OMIT -11 2 4 OMIT -6 6 15 OMIT -10 1 9 OMIT -3 6 19 OMIT 5 2 17 OMIT -9 10 5 OMIT -1 18 1 OMIT 1 11 16 OMIT 9 9 4 OMIT -11 2 6 OMIT -11 0 6 OMIT -4 16 6 OMIT 9 10 1 OMIT 6 10 12 OMIT -11 4 3 OMIT 0 2 0 MORE -1 FMAP 2 PLAN 20 SIZE 0.156 0.182 0.285 ACTA BOND BOND $H CONF LIST 6 L.S. 10 TEMP 0.00 WGHT 0.000000 4.713700 FVAR 0.40741 CO1 3 0.328207 0.839791 0.168569 11.00000 0.02252 0.03670 = 0.02041 -0.00029 0.00057 -0.00238 O2 5 0.016551 0.914970 0.234708 11.00000 0.04783 0.09514 = 0.02330 0.01433 0.00366 0.03356 O1 5 0.246578 0.868287 0.275565 11.00000 0.02896 0.06459 = 0.02241 0.00036 0.00440 0.01499 O3 5 0.334597 0.734867 0.551594 11.00000 0.03224 0.05378 = 0.03230 0.00819 -0.00011 0.00987 O4 5 0.192682 0.777761 0.643258 11.00000 0.05670 0.05784 = 0.02212 0.00555 0.00403 0.02105 O6 5 -0.328872 0.968732 0.432306 11.00000 0.04918 0.12228 = 0.05714 0.01509 0.00674 0.04544 O5 5 -0.284175 0.921737 0.552846 11.00000 0.07043 0.16933 = 0.06071 0.04378 0.04243 0.05365 O7 5 0.171054 0.926099 0.109515 11.00000 0.03535 0.05587 = 0.02297 0.00427 0.00181 0.00376 AFIX 7 H7A 2 0.092577 0.925081 0.133524 11.00000 -1.50000 H7B 2 0.144672 0.904754 0.062959 11.00000 -1.50000 AFIX 0 C17 1 1.296033 0.471976 0.427378 11.00000 0.03993 0.06540 = 0.02877 0.01312 0.00990 0.02395 AFIX 43 H17 2 1.242970 0.460876 0.471304 11.00000 -1.20000 AFIX 0 C18 1 1.419934 0.421499 0.416080 11.00000 0.05120 0.06383 = 0.02855 0.01363 0.00698 0.02750 AFIX 43 H18 2 1.449310 0.376879 0.453915 11.00000 -1.20000 AFIX 0 C15 1 1.112364 0.588634 0.381188 11.00000 0.02215 0.03251 = 0.02780 0.00033 -0.00079 -0.00130 C14 1 0.894919 0.650185 0.354235 11.00000 0.02615 0.03441 = 0.02504 -0.00068 0.00165 0.00131 C11 1 0.757492 0.685789 0.312177 11.00000 0.02356 0.03636 = 0.02762 0.00197 0.00021 0.00268 C10 1 0.665981 0.738728 0.353705 11.00000 0.03488 0.05320 = 0.02516 -0.00694 -0.00215 0.00934 AFIX 43 H10 2 0.688583 0.749089 0.408461 11.00000 -1.20000 AFIX 0 C9 1 0.540343 0.776485 0.313847 11.00000 0.02895 0.05628 = 0.03168 -0.00647 0.00419 0.00955 AFIX 43 H9 2 0.481355 0.813438 0.342874 11.00000 -1.20000 AFIX 0 C13 1 0.582632 0.706897 0.197094 11.00000 0.03677 0.06807 = 0.02609 -0.00608 -0.00348 0.01290 AFIX 43 H13 2 0.552690 0.693007 0.143646 11.00000 -1.20000 AFIX 0 C12 1 0.711787 0.668313 0.232027 11.00000 0.03677 0.06602 = 0.03312 -0.01143 -0.00171 0.02125 AFIX 43 H12 2 0.767974 0.630737 0.201952 11.00000 -1.20000 AFIX 0 C1 1 0.114809 0.888599 0.286708 11.00000 0.04112 0.04039 = 0.02238 0.00321 0.00031 0.00688 C2 1 0.072754 0.879259 0.371787 11.00000 0.03412 0.03277 = 0.02155 0.00061 0.00235 0.00718 C7 1 -0.065625 0.908624 0.389554 11.00000 0.03500 0.03990 = 0.02386 0.00600 0.00075 0.00664 AFIX 43 H7 2 -0.132252 0.933732 0.349751 11.00000 -1.20000 AFIX 0 C6 1 -0.102461 0.899919 0.467120 11.00000 0.02707 0.03512 = 0.03021 0.00409 0.00644 0.00569 C5 1 -0.009675 0.860785 0.527148 11.00000 0.03678 0.03900 = 0.02298 0.00399 0.00561 0.00130 AFIX 43 H5 2 -0.038266 0.854982 0.578900 11.00000 -1.20000 AFIX 0 C4 1 0.127816 0.830022 0.509022 11.00000 0.03009 0.03339 = 0.02198 0.00136 0.00013 0.00212 C3 1 0.168331 0.839905 0.431651 11.00000 0.02859 0.03586 = 0.02705 0.00154 0.00316 0.00648 AFIX 43 H3 2 0.260954 0.819842 0.419753 11.00000 -1.20000 AFIX 0 N7 4 -0.249991 0.932339 0.485369 11.00000 0.03809 0.06603 = 0.04281 0.00510 0.01137 0.01561 N1 4 0.498727 0.762870 0.235779 11.00000 0.02662 0.04234 = 0.02635 -0.00183 0.00104 0.00413 N2 4 0.920355 0.644987 0.432929 11.00000 0.02737 0.04646 = 0.02642 -0.00440 -0.00020 0.00573 N3 4 1.057292 0.604816 0.449645 11.00000 0.03028 0.04324 = 0.02531 -0.00378 -0.00458 0.00753 N4 4 1.013946 0.617251 0.319515 11.00000 0.02686 0.03403 = 0.02131 0.00233 0.00186 0.00185 N5 4 1.020244 0.607137 0.236332 11.00000 0.03731 0.06323 = 0.02483 0.00697 0.00846 0.00788 AFIX 7 H5A 2 1.040166 0.551063 0.226550 11.00000 -1.20000 AFIX 0 N6 4 1.500883 0.432625 0.353972 11.00000 0.02620 0.04528 = 0.03100 -0.00140 0.00119 0.00624 C8 1 0.226505 0.779751 0.571508 11.00000 0.03256 0.03371 = 0.02793 0.00316 0.00048 -0.00116 C19 1 1.458764 0.498863 0.302401 11.00000 0.03067 0.05091 = 0.04889 0.01126 0.01423 0.00549 AFIX 43 H19 2 1.514008 0.508573 0.259093 11.00000 -1.20000 AFIX 0 C20 1 1.337867 0.553871 0.309582 11.00000 0.02873 0.04042 = 0.05227 0.01774 0.01097 0.00523 AFIX 43 H20 2 1.314315 0.600301 0.272561 11.00000 -1.20000 AFIX 0 C16 1 1.251439 0.539488 0.372492 11.00000 0.02189 0.03881 = 0.02997 -0.00453 -0.00200 -0.00069 H5B 2 1.081005 0.646880 0.221477 11.00000 0.05027 HKLF 4 REM CoNA1_2_0m_a.res in P2(1)/c REM wR2 = 0.1022, GooF = S = 1.186, Restrained GooF = 1.186 for all data REM R1 = 0.0624 for 3396 Fo > 4sig(Fo) and 0.0927 for all 4473 data REM 322 parameters refined using 0 restraints END WGHT 0.0000 4.7135 REM Highest difference peak 0.356, deepest hole -0.374, 1-sigma level 0.078 Q1 1 0.0650 0.8458 0.3341 11.00000 0.05 0.36 Q2 1 0.0766 0.9633 0.2591 11.00000 0.05 0.34 Q3 1 -0.1815 0.9092 0.4720 11.00000 0.05 0.34 Q4 1 0.3253 0.8804 0.1156 11.00000 0.05 0.31 Q5 1 -0.3003 0.8621 0.5267 11.00000 0.05 0.31 Q6 1 0.4061 0.8386 0.1284 11.00000 0.05 0.31 Q7 1 -0.2850 0.8758 0.5145 11.00000 0.05 0.30 Q8 1 -0.0488 0.9158 0.5010 11.00000 0.05 0.30 Q9 1 1.3333 0.5577 0.3683 11.00000 0.05 0.29 Q10 1 -0.1365 0.6983 0.5969 11.00000 0.05 0.29 Q11 1 0.5558 0.7907 0.4881 11.00000 0.05 0.29 Q12 1 1.1656 0.5021 0.2933 11.00000 0.05 0.29 Q13 1 -0.2387 0.9392 0.5530 11.00000 0.05 0.28 Q14 1 0.4400 0.8381 0.1915 11.00000 0.05 0.28 Q15 1 0.0985 0.9172 0.3394 11.00000 0.05 0.28 Q16 1 1.1908 0.3127 0.3942 11.00000 0.05 0.28 Q17 1 -0.2049 0.9188 0.3282 11.00000 0.05 0.27 Q18 1 1.5933 0.4799 0.1668 11.00000 0.05 0.27 Q19 1 0.8350 0.6977 0.3259 11.00000 0.05 0.27 Q20 1 1.2229 0.2813 0.4250 11.00000 0.05 0.27 ; _shelx_res_checksum 70243 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_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 0.32821(5) 0.83979(4) 0.16857(3) 0.02664(14) Uani 1 1 d . . . . . O2 O 0.0166(3) 0.9150(2) 0.23471(15) 0.0554(9) Uani 1 1 d . . . . . O1 O 0.2466(3) 0.8683(2) 0.27556(14) 0.0385(7) Uani 1 1 d . . . . . O3 O 0.3346(3) 0.7349(2) 0.55159(15) 0.0397(7) Uani 1 1 d . . . . . O4 O 0.1927(3) 0.7778(2) 0.64326(15) 0.0455(8) Uani 1 1 d . . . . . O6 O -0.3289(4) 0.9687(3) 0.4323(2) 0.0761(12) Uani 1 1 d . . . . . O5 O -0.2842(4) 0.9217(3) 0.5528(2) 0.0978(16) Uani 1 1 d . . . . . O7 O 0.1711(3) 0.92610(19) 0.10952(15) 0.0381(7) Uani 1 1 d . . . . . H7A H 0.092577 0.925081 0.133524 0.057 Uiso 1 1 d R U . . . H7B H 0.144672 0.904754 0.062959 0.057 Uiso 1 1 d R U . . . C17 C 1.2960(4) 0.4720(3) 0.4274(2) 0.0443(11) Uani 1 1 d . . . . . H17 H 1.242970 0.460876 0.471304 0.053 Uiso 1 1 calc R U . . . C18 C 1.4199(5) 0.4215(3) 0.4161(2) 0.0477(12) Uani 1 1 d . . . . . H18 H 1.449310 0.376879 0.453915 0.057 Uiso 1 1 calc R U . . . C15 C 1.1124(4) 0.5886(3) 0.3812(2) 0.0277(8) Uani 1 1 d . . . . . C14 C 0.8949(4) 0.6502(3) 0.3542(2) 0.0286(8) Uani 1 1 d . . . . . C11 C 0.7575(4) 0.6858(3) 0.3122(2) 0.0293(9) Uani 1 1 d . . . . . C10 C 0.6660(4) 0.7387(3) 0.3537(2) 0.0381(10) Uani 1 1 d . . . . . H10 H 0.688583 0.749089 0.408461 0.046 Uiso 1 1 calc R U . . . C9 C 0.5403(4) 0.7765(3) 0.3138(2) 0.0389(10) Uani 1 1 d . . . . . H9 H 0.481355 0.813438 0.342874 0.047 Uiso 1 1 calc R U . . . C13 C 0.5826(4) 0.7069(3) 0.1971(2) 0.0441(11) Uani 1 1 d . . . . . H13 H 0.552690 0.693007 0.143646 0.053 Uiso 1 1 calc R U . . . C12 C 0.7118(4) 0.6683(3) 0.2320(2) 0.0456(11) Uani 1 1 d . . . . . H12 H 0.767974 0.630737 0.201952 0.055 Uiso 1 1 calc R U . . . C1 C 0.1148(4) 0.8886(3) 0.2867(2) 0.0348(9) Uani 1 1 d . . . . . C2 C 0.0728(4) 0.8793(3) 0.3718(2) 0.0295(9) Uani 1 1 d . . . . . C7 C -0.0656(4) 0.9086(3) 0.3896(2) 0.0331(9) Uani 1 1 d . . . . . H7 H -0.132252 0.933732 0.349751 0.040 Uiso 1 1 calc R U . . . C6 C -0.1025(4) 0.8999(3) 0.4671(2) 0.0306(9) Uani 1 1 d . . . . . C5 C -0.0097(4) 0.8608(3) 0.5271(2) 0.0327(9) Uani 1 1 d . . . . . H5 H -0.038266 0.854982 0.578900 0.039 Uiso 1 1 calc R U . . . C4 C 0.1278(4) 0.8300(3) 0.5090(2) 0.0286(8) Uani 1 1 d . . . . . C3 C 0.1683(4) 0.8399(3) 0.4317(2) 0.0305(8) Uani 1 1 d . . . . . H3 H 0.260954 0.819842 0.419753 0.037 Uiso 1 1 calc R U . . . N7 N -0.2500(4) 0.9323(3) 0.4854(2) 0.0485(10) Uani 1 1 d . . . . . N1 N 0.4987(3) 0.7629(2) 0.23578(17) 0.0319(7) Uani 1 1 d . . . . . N2 N 0.9204(3) 0.6450(2) 0.43293(17) 0.0336(8) Uani 1 1 d . . . . . N3 N 1.0573(3) 0.6048(2) 0.44964(17) 0.0334(8) Uani 1 1 d . . . . . N4 N 1.0139(3) 0.6173(2) 0.31951(16) 0.0274(7) Uani 1 1 d . . . . . N5 N 1.0202(4) 0.6071(3) 0.23633(19) 0.0414(9) Uani 1 1 d . . . . . H5A H 1.040166 0.551063 0.226550 0.050 Uiso 1 1 d R U . . . N6 N 1.5009(3) 0.4326(2) 0.35397(18) 0.0343(8) Uani 1 1 d . . . . . C8 C 0.2265(4) 0.7798(3) 0.5715(2) 0.0316(9) Uani 1 1 d . . . . . C19 C 1.4588(4) 0.4989(3) 0.3024(3) 0.0428(11) Uani 1 1 d . . . . . H19 H 1.514008 0.508573 0.259093 0.051 Uiso 1 1 calc R U . . . C20 C 1.3379(4) 0.5539(3) 0.3096(3) 0.0400(10) Uani 1 1 d . . . . . H20 H 1.314315 0.600301 0.272561 0.048 Uiso 1 1 calc R U . . . C16 C 1.2514(4) 0.5395(3) 0.3725(2) 0.0305(9) Uani 1 1 d . . . . . H5B H 1.081(5) 0.647(3) 0.221(3) 0.050(15) Uiso 1 1 d . . . . . 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 0.0225(2) 0.0367(3) 0.0204(2) -0.0003(2) 0.00057(18) -0.0024(2) O2 0.0478(18) 0.095(3) 0.0233(15) 0.0143(16) 0.0037(13) 0.0336(18) O1 0.0290(15) 0.065(2) 0.0224(13) 0.0004(13) 0.0044(11) 0.0150(14) O3 0.0322(15) 0.0538(19) 0.0323(15) 0.0082(13) -0.0001(12) 0.0099(14) O4 0.0567(19) 0.058(2) 0.0221(14) 0.0055(13) 0.0040(13) 0.0211(16) O6 0.049(2) 0.122(3) 0.057(2) 0.015(2) 0.0067(17) 0.045(2) O5 0.070(3) 0.169(4) 0.061(2) 0.044(3) 0.042(2) 0.054(3) O7 0.0354(15) 0.0559(19) 0.0230(14) 0.0043(13) 0.0018(11) 0.0038(14) C17 0.040(2) 0.065(3) 0.029(2) 0.013(2) 0.0099(18) 0.024(2) C18 0.051(3) 0.064(3) 0.029(2) 0.014(2) 0.0070(19) 0.028(2) C15 0.0221(18) 0.033(2) 0.028(2) 0.0003(16) -0.0008(15) -0.0013(16) C14 0.0262(19) 0.034(2) 0.0250(19) -0.0007(17) 0.0016(15) 0.0013(17) C11 0.0236(19) 0.036(2) 0.0276(19) 0.0020(17) 0.0002(15) 0.0027(16) C10 0.035(2) 0.053(3) 0.025(2) -0.0069(19) -0.0021(17) 0.009(2) C9 0.029(2) 0.056(3) 0.032(2) -0.006(2) 0.0042(17) 0.010(2) C13 0.037(2) 0.068(3) 0.026(2) -0.006(2) -0.0035(18) 0.013(2) C12 0.037(2) 0.066(3) 0.033(2) -0.011(2) -0.0017(18) 0.021(2) C1 0.041(2) 0.040(2) 0.0224(19) 0.0032(17) 0.0003(17) 0.0069(19) C2 0.034(2) 0.033(2) 0.0216(18) 0.0006(16) 0.0023(15) 0.0072(17) C7 0.035(2) 0.040(2) 0.0239(19) 0.0060(17) 0.0008(16) 0.0066(18) C6 0.027(2) 0.035(2) 0.030(2) 0.0041(17) 0.0064(16) 0.0057(17) C5 0.037(2) 0.039(2) 0.0230(19) 0.0040(17) 0.0056(16) 0.0013(18) C4 0.030(2) 0.033(2) 0.0220(18) 0.0014(17) 0.0001(15) 0.0021(17) C3 0.0286(19) 0.036(2) 0.0270(19) 0.0015(18) 0.0032(15) 0.0065(18) N7 0.038(2) 0.066(3) 0.043(2) 0.005(2) 0.0114(18) 0.0156(19) N1 0.0266(16) 0.042(2) 0.0263(17) -0.0018(15) 0.0010(13) 0.0041(15) N2 0.0274(17) 0.046(2) 0.0264(16) -0.0044(15) -0.0002(13) 0.0057(15) N3 0.0303(17) 0.043(2) 0.0253(16) -0.0038(15) -0.0046(13) 0.0075(15) N4 0.0269(16) 0.0340(18) 0.0213(15) 0.0023(14) 0.0019(12) 0.0019(14) N5 0.037(2) 0.063(3) 0.0248(18) 0.0070(18) 0.0085(15) 0.008(2) N6 0.0262(17) 0.045(2) 0.0310(18) -0.0014(16) 0.0012(14) 0.0062(15) C8 0.033(2) 0.034(2) 0.028(2) 0.0032(17) 0.0005(16) -0.0012(18) C19 0.031(2) 0.051(3) 0.049(3) 0.011(2) 0.0142(19) 0.005(2) C20 0.029(2) 0.040(3) 0.052(3) 0.018(2) 0.0110(19) 0.0052(18) C16 0.0219(19) 0.039(2) 0.030(2) -0.0045(18) -0.0020(15) -0.0007(17) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O7 90.02(10) . . ? O1 Co1 N6 110.93(12) . 2_755 ? O7 Co1 N6 90.33(11) . 2_755 ? O1 Co1 O4 95.00(11) . 4_575 ? O7 Co1 O4 92.35(11) . 4_575 ? N6 Co1 O4 153.93(11) 2_755 4_575 ? O1 Co1 N1 87.36(11) . . ? O7 Co1 N1 174.22(12) . . ? N6 Co1 N1 85.79(12) 2_755 . ? O4 Co1 N1 93.02(12) 4_575 . ? O1 Co1 O3 154.57(11) . 4_575 ? O7 Co1 O3 87.59(10) . 4_575 ? N6 Co1 O3 94.41(11) 2_755 4_575 ? O4 Co1 O3 59.84(10) 4_575 4_575 ? N1 Co1 O3 96.98(11) . 4_575 ? O1 Co1 C8 124.58(12) . 4_575 ? O7 Co1 C8 85.72(11) . 4_575 ? N6 Co1 C8 124.30(13) 2_755 4_575 ? O4 Co1 C8 30.39(11) 4_575 4_575 ? N1 Co1 C8 100.01(12) . 4_575 ? O3 Co1 C8 29.99(10) 4_575 4_575 ? C1 O1 Co1 127.3(2) . . ? C8 O3 Co1 86.4(2) . 4_576 ? C8 O4 Co1 91.0(2) . 4_576 ? Co1 O7 H7A 109.4 . . ? Co1 O7 H7B 109.2 . . ? H7A O7 H7B 104.5 . . ? C18 C17 C16 119.0(4) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? N6 C18 C17 124.0(4) . . ? N6 C18 H18 118.0 . . ? C17 C18 H18 118.0 . . ? N3 C15 N4 109.0(3) . . ? N3 C15 C16 125.2(3) . . ? N4 C15 C16 125.6(3) . . ? N2 C14 N4 109.6(3) . . ? N2 C14 C11 123.9(3) . . ? N4 C14 C11 126.5(3) . . ? C10 C11 C12 116.9(3) . . ? C10 C11 C14 119.2(3) . . ? C12 C11 C14 123.9(3) . . ? C11 C10 C9 119.7(3) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? N1 C9 C10 123.6(4) . . ? N1 C9 H9 118.2 . . ? C10 C9 H9 118.2 . . ? N1 C13 C12 123.4(4) . . ? N1 C13 H13 118.3 . . ? C12 C13 H13 118.3 . . ? C13 C12 C11 119.7(4) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? O2 C1 O1 126.5(3) . . ? O2 C1 C2 117.0(3) . . ? O1 C1 C2 116.5(3) . . ? C3 C2 C7 119.5(3) . . ? C3 C2 C1 121.2(3) . . ? C7 C2 C1 119.3(3) . . ? C6 C7 C2 118.7(3) . . ? C6 C7 H7 120.6 . . ? C2 C7 H7 120.6 . . ? C5 C6 C7 122.7(3) . . ? C5 C6 N7 119.2(3) . . ? C7 C6 N7 118.1(3) . . ? C6 C5 C4 118.6(3) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? C3 C4 C5 119.7(3) . . ? C3 C4 C8 120.4(3) . . ? C5 C4 C8 119.8(3) . . ? C2 C3 C4 120.9(3) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? O5 N7 O6 123.6(4) . . ? O5 N7 C6 118.1(4) . . ? O6 N7 C6 118.3(3) . . ? C13 N1 C9 116.4(3) . . ? C13 N1 Co1 119.3(2) . . ? C9 N1 Co1 123.7(3) . . ? C14 N2 N3 107.1(3) . . ? C15 N3 N2 108.2(3) . . ? C15 N4 C14 106.0(3) . . ? C15 N4 N5 129.0(3) . . ? C14 N4 N5 124.6(3) . . ? N4 N5 H5A 108.6 . . ? N4 N5 H5B 108(3) . . ? H5A N5 H5B 116.2 . . ? C19 N6 C18 116.5(3) . . ? C19 N6 Co1 121.5(3) . 2_745 ? C18 N6 Co1 121.7(3) . 2_745 ? O3 C8 O4 120.5(3) . . ? O3 C8 C4 120.2(3) . . ? O4 C8 C4 119.1(3) . . ? O3 C8 Co1 63.58(19) . 4_576 ? O4 C8 Co1 58.57(19) . 4_576 ? C4 C8 Co1 162.2(3) . 4_576 ? N6 C19 C20 123.6(4) . . ? N6 C19 H19 118.2 . . ? C20 C19 H19 118.2 . . ? C19 C20 C16 119.4(4) . . ? C19 C20 H20 120.3 . . ? C16 C20 H20 120.3 . . ? C17 C16 C20 117.4(3) . . ? C17 C16 C15 118.9(3) . . ? C20 C16 C15 123.6(3) . . ? 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 O1 2.043(2) . ? Co1 O7 2.082(2) . ? Co1 N6 2.124(3) 2_755 ? Co1 O4 2.135(3) 4_575 ? Co1 N1 2.142(3) . ? Co1 O3 2.244(3) 4_575 ? Co1 C8 2.501(4) 4_575 ? O2 C1 1.244(4) . ? O1 C1 1.264(4) . ? O3 C8 1.252(4) . ? O4 C8 1.266(4) . ? O6 N7 1.208(4) . ? O5 N7 1.207(4) . ? O7 H7A 0.8507 . ? O7 H7B 0.8506 . ? C17 C18 1.374(5) . ? C17 C16 1.382(5) . ? C17 H17 0.9300 . ? C18 N6 1.338(5) . ? C18 H18 0.9300 . ? C15 N3 1.313(4) . ? C15 N4 1.362(4) . ? C15 C16 1.472(5) . ? C14 N2 1.314(4) . ? C14 N4 1.363(4) . ? C14 C11 1.467(5) . ? C11 C10 1.372(5) . ? C11 C12 1.386(5) . ? C10 C9 1.379(5) . ? C10 H10 0.9300 . ? C9 N1 1.337(5) . ? C9 H9 0.9300 . ? C13 N1 1.328(5) . ? C13 C12 1.379(5) . ? C13 H13 0.9300 . ? C12 H12 0.9300 . ? C1 C2 1.513(5) . ? C2 C3 1.384(5) . ? C2 C7 1.387(5) . ? C7 C6 1.375(5) . ? C7 H7 0.9300 . ? C6 C5 1.371(5) . ? C6 N7 1.480(5) . ? C5 C4 1.387(5) . ? C5 H5 0.9300 . ? C4 C3 1.385(5) . ? C4 C8 1.501(5) . ? C3 H3 0.9300 . ? N2 N3 1.379(4) . ? N4 N5 1.404(4) . ? N5 H5A 0.8601 . ? N5 H5B 0.86(4) . ? N6 C19 1.329(5) . ? C19 C20 1.376(5) . ? C19 H19 0.9300 . ? C20 C16 1.387(5) . ? C20 H20 0.9300 . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 C17 C18 N6 -0.9(7) . . . . ? N2 C14 C11 C10 18.2(6) . . . . ? N4 C14 C11 C10 -162.3(4) . . . . ? N2 C14 C11 C12 -160.9(4) . . . . ? N4 C14 C11 C12 18.6(6) . . . . ? C12 C11 C10 C9 -4.2(6) . . . . ? C14 C11 C10 C9 176.7(4) . . . . ? C11 C10 C9 N1 1.7(7) . . . . ? N1 C13 C12 C11 1.6(7) . . . . ? C10 C11 C12 C13 2.6(6) . . . . ? C14 C11 C12 C13 -178.2(4) . . . . ? Co1 O1 C1 O2 -17.2(6) . . . . ? Co1 O1 C1 C2 162.4(3) . . . . ? O2 C1 C2 C3 172.0(4) . . . . ? O1 C1 C2 C3 -7.7(6) . . . . ? O2 C1 C2 C7 -6.4(6) . . . . ? O1 C1 C2 C7 173.9(4) . . . . ? C3 C2 C7 C6 1.7(6) . . . . ? C1 C2 C7 C6 -179.9(4) . . . . ? C2 C7 C6 C5 -2.1(6) . . . . ? C2 C7 C6 N7 179.4(4) . . . . ? C7 C6 C5 C4 1.0(6) . . . . ? N7 C6 C5 C4 179.5(3) . . . . ? C6 C5 C4 C3 0.4(6) . . . . ? C6 C5 C4 C8 -174.8(3) . . . . ? C7 C2 C3 C4 -0.4(6) . . . . ? C1 C2 C3 C4 -178.7(4) . . . . ? C5 C4 C3 C2 -0.7(6) . . . . ? C8 C4 C3 C2 174.5(4) . . . . ? C5 C6 N7 O5 -1.1(6) . . . . ? C7 C6 N7 O5 177.5(4) . . . . ? C5 C6 N7 O6 178.2(4) . . . . ? C7 C6 N7 O6 -3.3(6) . . . . ? C12 C13 N1 C9 -4.2(6) . . . . ? C12 C13 N1 Co1 167.0(4) . . . . ? C10 C9 N1 C13 2.5(6) . . . . ? C10 C9 N1 Co1 -168.3(3) . . . . ? N4 C14 N2 N3 -2.0(4) . . . . ? C11 C14 N2 N3 177.5(3) . . . . ? N4 C15 N3 N2 -0.1(4) . . . . ? C16 C15 N3 N2 -174.7(3) . . . . ? C14 N2 N3 C15 1.3(4) . . . . ? N3 C15 N4 C14 -1.1(4) . . . . ? C16 C15 N4 C14 173.5(3) . . . . ? N3 C15 N4 N5 -174.3(4) . . . . ? C16 C15 N4 N5 0.2(6) . . . . ? N2 C14 N4 C15 1.9(4) . . . . ? C11 C14 N4 C15 -177.6(4) . . . . ? N2 C14 N4 N5 175.6(4) . . . . ? C11 C14 N4 N5 -4.0(6) . . . . ? C17 C18 N6 C19 2.1(7) . . . . ? C17 C18 N6 Co1 -171.0(4) . . . 2_745 ? Co1 O3 C8 O4 14.5(4) 4_576 . . . ? Co1 O3 C8 C4 -160.2(3) 4_576 . . . ? Co1 O4 C8 O3 -15.2(4) 4_576 . . . ? Co1 O4 C8 C4 159.5(3) 4_576 . . . ? C3 C4 C8 O3 -10.7(6) . . . . ? C5 C4 C8 O3 164.5(4) . . . . ? C3 C4 C8 O4 174.6(4) . . . . ? C5 C4 C8 O4 -10.3(6) . . . . ? C3 C4 C8 Co1 -108.1(9) . . . 4_576 ? C5 C4 C8 Co1 67.1(10) . . . 4_576 ? C18 N6 C19 C20 -0.9(6) . . . . ? Co1 N6 C19 C20 172.2(3) 2_745 . . . ? N6 C19 C20 C16 -1.5(7) . . . . ? C18 C17 C16 C20 -1.6(6) . . . . ? C18 C17 C16 C15 175.3(4) . . . . ? C19 C20 C16 C17 2.7(6) . . . . ? C19 C20 C16 C15 -174.0(4) . . . . ? N3 C15 C16 C17 30.7(6) . . . . ? N4 C15 C16 C17 -143.0(4) . . . . ? N3 C15 C16 C20 -152.6(4) . . . . ? N4 C15 C16 C20 33.7(6) . . . . ?