#------------------------------------------------------------------------------ #$Date: 2017-09-14 05:44:36 +0300 (Thu, 14 Sep 2017) $ #$Revision: 200876 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/42/7044227.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_7044227 loop_ _publ_author_name 'Mandal, Shuvankar' 'Mondal, Suraj' 'Rajnak, Cyril' 'Titis, Jan' 'Boca, Roman' 'Mohanta, Sasankasekhar' _publ_section_title ; Syntheses, crystal structures and magnetic properties of two mixed-valence Co(III)Co(II) compounds derived from Schiff base ligands: Field supported single-ion-magnet behaviour with easy plane anisotropy ; _journal_name_full 'Dalton Trans.' _journal_paper_doi 10.1039/C7DT02455J _journal_year 2017 _chemical_formula_sum 'C22 H39 Co2 N16 O2' _chemical_formula_weight 677.55 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2017-07-03 deposited with the CCDC. 2017-09-13 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.424(6) _cell_length_b 13.764(9) _cell_length_c 25.759(16) _cell_measurement_reflns_used 1419 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 17.74 _cell_measurement_theta_min 2.17 _cell_volume 2987(3) _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-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.985 _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 0.1148 _diffrn_reflns_av_unetI/netI 0.1580 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 14078 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.597 _diffrn_reflns_theta_min 1.581 _exptl_absorpt_coefficient_mu 1.162 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_crystal_colour Brown _exptl_crystal_density_diffrn 1.507 _exptl_crystal_description Rectangular _exptl_crystal_F_000 1412 _exptl_crystal_size_max 0.160 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.120 _exptl_transmission_factor_max 0.873 _exptl_transmission_factor_min 0.836 _refine_diff_density_max 0.660 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.124 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.43(6) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 375 _refine_ls_number_reflns 5331 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.004 _refine_ls_R_factor_all 0.1673 _refine_ls_R_factor_gt 0.0797 _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^)+(0.0900P)^2^+0.6696P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1745 _refine_ls_wR_factor_ref 0.2173 _reflns_Friedel_coverage 0.762 _reflns_Friedel_fraction_full 0.997 _reflns_Friedel_fraction_max 0.989 _reflns_number_gt 2668 _reflns_number_total 5331 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt02455j2.cif _cod_data_source_block 1 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas ; _cod_database_code 7044227 _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_estimated_absorpt_t_min 0.836 _shelx_estimated_absorpt_t_max 0.873 _shelx_res_file ; 1.res created by SHELXL-2014/7 TITL 1 in P2(1)2(1)2(1) CELL 0.71073 8.4240 13.7640 25.7590 90.000 90.000 90.000 ZERR 4.00 0.0056 0.0090 0.0165 0.000 0.000 0.000 LATT -1 SYMM x+1/2, -y+1/2, -z SYMM -x, y+1/2, -z+1/2 SYMM -x+1/2, -y, z+1/2 SFAC C H N O Co UNIT 88 156 64 8 8 OMIT -3 51.2 L.S. 30 ACTA BOND $H FMAP 2 PLAN 5 EADP N14 N15 EADP N6 N7 TWIN SIZE 0.12 0.14 0.16 TEMP 23.000 WGHT 0.090000 0.669565 BASF 0.42731 FVAR 0.11392 C1 1 0.713852 -0.008340 0.249661 11.00000 0.05978 0.04456 = 0.05874 -0.00706 0.00137 0.01713 C2 1 0.605801 -0.078580 0.234178 11.00000 0.03914 0.05725 = 0.06622 0.00438 -0.01680 -0.00653 C3 1 0.579742 -0.094171 0.181779 11.00000 0.04443 0.05705 = 0.07345 0.01340 -0.00343 0.00042 AFIX 43 H3 2 0.509338 -0.142945 0.172075 11.00000 -1.20000 AFIX 0 C4 1 0.652560 -0.041286 0.143470 11.00000 0.05023 0.08414 = 0.06200 0.00352 -0.01320 0.00336 C5 1 0.761572 0.030786 0.159454 11.00000 0.04598 0.08189 = 0.05739 0.01110 0.00647 0.00181 AFIX 43 H5 2 0.813864 0.068311 0.134776 11.00000 -1.20000 AFIX 0 C6 1 0.790335 0.045483 0.210987 11.00000 0.03294 0.06259 = 0.05649 0.01305 0.00524 0.00638 C7 1 0.619784 -0.056037 0.087510 11.00000 0.08552 0.12758 = 0.07361 0.00275 -0.01534 -0.01039 AFIX 137 H7A 2 0.572031 -0.118651 0.082444 11.00000 -1.50000 H7B 2 0.717402 -0.052602 0.068368 11.00000 -1.50000 H7C 2 0.548683 -0.006413 0.075460 11.00000 -1.50000 AFIX 0 C8 1 0.902697 0.125193 0.224741 11.00000 0.03881 0.07045 = 0.08206 0.00987 -0.00303 0.00407 AFIX 43 H8 2 0.955979 0.155100 0.197456 11.00000 -1.20000 AFIX 0 C9 1 1.044159 0.232888 0.277352 11.00000 0.04412 0.06924 = 0.09406 -0.00233 -0.00773 -0.00564 AFIX 23 H9A 2 1.145127 0.206579 0.288758 11.00000 -1.20000 H9B 2 1.061291 0.269079 0.245529 11.00000 -1.20000 AFIX 0 C10 1 0.978471 0.295626 0.316874 11.00000 0.05269 0.06643 = 0.09227 0.00457 -0.00567 -0.00622 AFIX 23 H10A 2 0.883890 0.327498 0.303787 11.00000 -1.20000 H10B 2 1.055104 0.345267 0.326168 11.00000 -1.20000 AFIX 0 C11 1 1.090009 0.213630 0.394278 11.00000 0.05146 0.09068 = 0.11178 -0.02225 -0.03499 -0.00315 AFIX 23 H11A 2 1.158705 0.174805 0.372302 11.00000 -1.20000 H11B 2 1.143912 0.274704 0.400782 11.00000 -1.20000 AFIX 0 C12 1 1.070138 0.161766 0.445117 11.00000 0.11522 0.10362 = 0.08653 -0.00148 -0.04771 0.00674 AFIX 137 H12A 2 1.021017 0.204572 0.469769 11.00000 -1.50000 H12B 2 1.172243 0.142037 0.457876 11.00000 -1.50000 H12C 2 1.004442 0.105515 0.440223 11.00000 -1.50000 AFIX 0 C13 1 0.831143 0.291500 0.396766 11.00000 0.09359 0.05387 = 0.07800 -0.00797 -0.02625 0.00891 AFIX 23 H13A 2 0.802815 0.251897 0.426505 11.00000 -1.20000 H13B 2 0.734505 0.303041 0.377241 11.00000 -1.20000 AFIX 0 C14 1 0.890739 0.390095 0.417153 11.00000 0.09016 0.07219 = 0.13257 -0.00523 -0.01561 -0.00719 AFIX 137 H14A 2 0.971751 0.379582 0.442755 11.00000 -1.50000 H14B 2 0.803969 0.424981 0.432523 11.00000 -1.50000 H14C 2 0.933663 0.427212 0.388894 11.00000 -1.50000 AFIX 0 C15 1 0.505142 -0.135662 0.268466 11.00000 0.05968 0.08266 = 0.05245 -0.00648 -0.00235 -0.00791 AFIX 43 H15 2 0.431517 -0.176722 0.252896 11.00000 -1.20000 AFIX 0 C16 1 0.384446 -0.194360 0.342850 11.00000 0.08629 0.08436 = 0.06502 0.01206 -0.00548 -0.02668 AFIX 23 H16A 2 0.361983 -0.251833 0.322332 11.00000 -1.20000 H16B 2 0.287190 -0.157227 0.346420 11.00000 -1.20000 AFIX 0 C17 1 0.446037 -0.222994 0.395412 11.00000 0.11372 0.06359 = 0.07310 0.01553 0.01404 -0.02812 AFIX 23 H17A 2 0.360292 -0.250746 0.415705 11.00000 -1.20000 H17B 2 0.527503 -0.272232 0.391408 11.00000 -1.20000 AFIX 0 C18 1 0.596460 -0.175012 0.468736 11.00000 0.16465 0.10671 = 0.08664 0.03634 -0.03285 -0.01901 AFIX 23 H18A 2 0.519868 -0.205347 0.491713 11.00000 -1.20000 H18B 2 0.670227 -0.225006 0.457671 11.00000 -1.20000 AFIX 0 C19 1 0.683278 -0.102946 0.497865 11.00000 0.18473 0.12744 = 0.11689 0.03204 -0.08528 -0.03130 AFIX 137 H19A 2 0.773013 -0.081455 0.477968 11.00000 -1.50000 H19B 2 0.719330 -0.130797 0.529935 11.00000 -1.50000 H19C 2 0.615256 -0.048637 0.505073 11.00000 -1.50000 AFIX 0 C20 1 0.386264 -0.067847 0.434233 11.00000 0.13173 0.07446 = 0.09595 0.01213 -0.00420 -0.03174 AFIX 23 H20A 2 0.341938 -0.046488 0.401405 11.00000 -1.20000 H20B 2 0.434577 -0.011624 0.450539 11.00000 -1.20000 AFIX 0 C21 1 0.248526 -0.102401 0.469008 11.00000 0.14460 0.11631 = 0.16827 0.01221 0.08116 -0.01821 AFIX 137 H21A 2 0.193417 -0.154717 0.452194 11.00000 -1.50000 H21B 2 0.176408 -0.049510 0.474836 11.00000 -1.50000 H21C 2 0.289949 -0.124503 0.501657 11.00000 -1.50000 AFIX 0 C22 1 0.244013 0.023282 0.185992 11.00000 0.09423 0.24072 = 0.16739 -0.01934 -0.00667 0.04457 AFIX 137 H22A 2 0.245346 0.013558 0.222894 11.00000 -1.50000 H22B 2 0.294369 -0.030803 0.169182 11.00000 -1.50000 H22C 2 0.136185 0.028439 0.174251 11.00000 -1.50000 AFIX 0 CO1 5 0.836614 0.115557 0.330906 11.00000 0.04008 0.05717 = 0.06979 -0.00244 -0.00912 0.00133 CO2 5 0.669473 -0.076884 0.364127 11.00000 0.06259 0.05765 = 0.07240 0.00535 -0.01647 -0.00374 N1 3 0.931502 0.155040 0.268582 11.00000 0.03012 0.07561 = 0.05255 -0.00359 0.00959 -0.00377 N2 3 0.937272 0.235085 0.364306 11.00000 0.02892 0.07553 = 0.08733 -0.01498 -0.01617 0.00758 N3 3 0.508721 -0.134479 0.316969 11.00000 0.04645 0.08179 = 0.07014 -0.00295 -0.00084 -0.01548 N4 3 0.512578 -0.138899 0.423156 11.00000 0.07927 0.05779 = 0.07183 0.01499 -0.01201 -0.00692 N5 3 0.648841 0.192589 0.314183 11.00000 0.05388 0.06137 = 0.07016 -0.00066 -0.01301 0.00878 N6 3 0.526842 0.154345 0.313392 11.00000 0.03740 0.10749 = 0.16114 -0.00585 0.00064 0.01177 N7 3 0.403640 0.119293 0.312846 11.00000 0.03740 0.10749 = 0.16114 -0.00585 0.00064 0.01177 N8 3 1.021861 0.035292 0.346207 11.00000 0.04044 0.07167 = 0.08751 -0.01878 -0.02837 0.01910 N9 3 1.072025 -0.014414 0.312443 11.00000 0.02714 0.08436 = 0.10501 -0.01372 -0.01959 0.00980 N10 3 1.119243 -0.062745 0.280697 11.00000 0.07606 0.12305 = 0.12577 -0.03074 -0.02115 0.03221 N11 3 0.725842 0.058401 0.390540 11.00000 0.04477 0.09022 = 0.06942 -0.00045 -0.00363 0.00046 N12 3 0.655560 0.101106 0.423278 11.00000 0.12743 0.08741 = 0.10794 0.01039 0.02425 -0.03765 N13 3 0.597231 0.141940 0.456501 11.00000 0.27788 0.13478 = 0.18521 -0.07661 0.14936 -0.08797 N14 3 0.849816 -0.170874 0.367810 11.00000 0.09763 0.09883 = 0.12326 -0.00232 -0.01376 0.03115 N15 3 0.920458 -0.225037 0.384387 11.00000 0.09763 0.09883 = 0.12326 -0.00232 -0.01376 0.03115 N16 3 1.001812 -0.282712 0.398304 11.00000 0.18760 0.19165 = 0.13921 -0.00187 -0.01717 0.10498 O1 4 0.743359 0.003754 0.299306 11.00000 0.05339 0.05973 = 0.05180 0.00492 -0.01732 0.00050 O2 4 0.321660 0.104404 0.174442 11.00000 0.16650 0.16049 = 0.85213 0.15347 0.21138 -0.00193 AFIX 147 H2 2 0.258275 0.149284 0.171513 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM 1 in P2(1)2(1)2(1) REM R1 = 0.0797 for 2668 Fo > 4sig(Fo) and 0.1673 for all 5331 data REM 375 parameters refined using 0 restraints END WGHT 0.0889 0.0000 REM Highest difference peak 0.660, deepest hole -0.518, 1-sigma level 0.124 Q1 1 0.8479 0.1895 0.3248 11.00000 0.05 0.66 Q2 1 0.6805 -0.0009 0.3644 11.00000 0.05 0.65 Q3 1 0.6682 -0.0720 0.4070 11.00000 0.05 0.51 Q4 1 0.8371 0.0402 0.3407 11.00000 0.05 0.49 Q5 1 0.6689 -0.1425 0.3901 11.00000 0.05 0.43 ; _shelx_res_checksum 98774 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, 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 C1 C 0.7139(17) -0.0083(10) 0.2497(6) 0.054(4) Uani 1 1 d . . C2 C 0.6058(16) -0.0786(10) 0.2342(6) 0.054(4) Uani 1 1 d . . C3 C 0.5797(17) -0.0942(10) 0.1818(6) 0.058(4) Uani 1 1 d . . H3 H 0.5093 -0.1429 0.1721 0.070 Uiso 1 1 calc R U C4 C 0.653(2) -0.0413(11) 0.1435(6) 0.065(4) Uani 1 1 d . . C5 C 0.7616(17) 0.0308(11) 0.1595(6) 0.062(4) Uani 1 1 d . . H5 H 0.8139 0.0683 0.1348 0.074 Uiso 1 1 calc R U C6 C 0.7903(15) 0.0455(10) 0.2110(6) 0.051(4) Uani 1 1 d . . C7 C 0.620(2) -0.0560(15) 0.0875(7) 0.096(6) Uani 1 1 d . . H7A H 0.5720 -0.1187 0.0824 0.143 Uiso 1 1 calc R U H7B H 0.7174 -0.0526 0.0684 0.143 Uiso 1 1 calc R U H7C H 0.5487 -0.0064 0.0755 0.143 Uiso 1 1 calc R U C8 C 0.9027(16) 0.1252(12) 0.2247(7) 0.064(4) Uani 1 1 d . . H8 H 0.9560 0.1551 0.1975 0.077 Uiso 1 1 calc R U C9 C 1.0442(18) 0.2329(11) 0.2774(7) 0.069(5) Uani 1 1 d . . H9A H 1.1451 0.2066 0.2888 0.083 Uiso 1 1 calc R U H9B H 1.0613 0.2691 0.2455 0.083 Uiso 1 1 calc R U C10 C 0.978(2) 0.2956(11) 0.3169(7) 0.070(5) Uani 1 1 d . . H10A H 0.8839 0.3275 0.3038 0.085 Uiso 1 1 calc R U H10B H 1.0551 0.3453 0.3262 0.085 Uiso 1 1 calc R U C11 C 1.0900(19) 0.2136(13) 0.3943(8) 0.085(6) Uani 1 1 d . . H11A H 1.1587 0.1748 0.3723 0.102 Uiso 1 1 calc R U H11B H 1.1439 0.2747 0.4008 0.102 Uiso 1 1 calc R U C12 C 1.070(3) 0.1618(14) 0.4451(8) 0.102(7) Uani 1 1 d . . H12A H 1.0210 0.2046 0.4698 0.153 Uiso 1 1 calc R U H12B H 1.1722 0.1420 0.4579 0.153 Uiso 1 1 calc R U H12C H 1.0044 0.1055 0.4402 0.153 Uiso 1 1 calc R U C13 C 0.831(2) 0.2915(10) 0.3968(6) 0.075(5) Uani 1 1 d . . H13A H 0.8028 0.2519 0.4265 0.090 Uiso 1 1 calc R U H13B H 0.7345 0.3030 0.3772 0.090 Uiso 1 1 calc R U C14 C 0.891(2) 0.3901(12) 0.4172(8) 0.098(6) Uani 1 1 d . . H14A H 0.9718 0.3796 0.4428 0.147 Uiso 1 1 calc R U H14B H 0.8040 0.4250 0.4325 0.147 Uiso 1 1 calc R U H14C H 0.9337 0.4272 0.3889 0.147 Uiso 1 1 calc R U C15 C 0.505(2) -0.1357(11) 0.2685(6) 0.065(4) Uani 1 1 d . . H15 H 0.4315 -0.1767 0.2529 0.078 Uiso 1 1 calc R U C16 C 0.384(2) -0.1944(12) 0.3428(6) 0.079(5) Uani 1 1 d . . H16A H 0.3620 -0.2518 0.3223 0.094 Uiso 1 1 calc R U H16B H 0.2872 -0.1572 0.3464 0.094 Uiso 1 1 calc R U C17 C 0.446(2) -0.2230(12) 0.3954(7) 0.083(6) Uani 1 1 d . . H17A H 0.3603 -0.2507 0.4157 0.100 Uiso 1 1 calc R U H17B H 0.5275 -0.2722 0.3914 0.100 Uiso 1 1 calc R U C18 C 0.596(3) -0.1750(15) 0.4687(8) 0.119(8) Uani 1 1 d . . H18A H 0.5199 -0.2053 0.4917 0.143 Uiso 1 1 calc R U H18B H 0.6702 -0.2250 0.4577 0.143 Uiso 1 1 calc R U C19 C 0.683(4) -0.1029(15) 0.4979(9) 0.143(10) Uani 1 1 d . . H19A H 0.7730 -0.0815 0.4780 0.215 Uiso 1 1 calc R U H19B H 0.7193 -0.1308 0.5299 0.215 Uiso 1 1 calc R U H19C H 0.6153 -0.0486 0.5051 0.215 Uiso 1 1 calc R U C20 C 0.386(3) -0.0678(13) 0.4342(8) 0.101(7) Uani 1 1 d . . H20A H 0.3419 -0.0465 0.4014 0.121 Uiso 1 1 calc R U H20B H 0.4346 -0.0116 0.4505 0.121 Uiso 1 1 calc R U C21 C 0.249(3) -0.1024(16) 0.4690(10) 0.143(10) Uani 1 1 d . . H21A H 0.1934 -0.1547 0.4522 0.215 Uiso 1 1 calc R U H21B H 0.1764 -0.0495 0.4748 0.215 Uiso 1 1 calc R U H21C H 0.2899 -0.1245 0.5017 0.215 Uiso 1 1 calc R U C22 C 0.244(3) 0.023(2) 0.1860(11) 0.167(12) Uani 1 1 d . . H22A H 0.2453 0.0136 0.2229 0.251 Uiso 1 1 calc R U H22B H 0.2944 -0.0308 0.1692 0.251 Uiso 1 1 calc R U H22C H 0.1362 0.0284 0.1743 0.251 Uiso 1 1 calc R U Co1 Co 0.8366(2) 0.11556(13) 0.33091(8) 0.0557(6) Uani 1 1 d . . Co2 Co 0.6695(3) -0.07688(13) 0.36413(8) 0.0642(7) Uani 1 1 d . . N1 N 0.9315(13) 0.1550(9) 0.2686(5) 0.053(3) Uani 1 1 d . . N2 N 0.9373(13) 0.2351(9) 0.3643(6) 0.064(3) Uani 1 1 d . . N3 N 0.5087(14) -0.1345(9) 0.3170(6) 0.066(3) Uani 1 1 d . . N4 N 0.5126(18) -0.1389(9) 0.4232(5) 0.070(4) Uani 1 1 d . . N5 N 0.6488(17) 0.1926(8) 0.3142(5) 0.062(3) Uani 1 1 d . . N6 N 0.5268(19) 0.1543(11) 0.3134(7) 0.102(4) Uani 1 1 d . . N7 N 0.4036(16) 0.1193(12) 0.3128(7) 0.102(4) Uani 1 1 d . . N8 N 1.0219(15) 0.0353(9) 0.3462(5) 0.067(4) Uani 1 1 d . . N9 N 1.0720(15) -0.0144(11) 0.3124(7) 0.072(4) Uani 1 1 d . . N10 N 1.1192(19) -0.0627(13) 0.2807(8) 0.108(6) Uani 1 1 d . . N11 N 0.7258(15) 0.0584(11) 0.3905(6) 0.068(4) Uani 1 1 d . . N12 N 0.656(3) 0.1011(13) 0.4233(8) 0.108(6) Uani 1 1 d . . N13 N 0.597(4) 0.1419(16) 0.4565(10) 0.199(15) Uani 1 1 d . . N14 N 0.850(2) -0.1709(11) 0.3678(7) 0.107(4) Uani 1 1 d . . N15 N 0.920(2) -0.2250(15) 0.3844(8) 0.107(4) Uani 1 1 d . . N16 N 1.002(3) -0.2827(19) 0.3983(9) 0.173(10) Uani 1 1 d . . O1 O 0.7434(11) 0.0038(6) 0.2993(4) 0.055(2) Uani 1 1 d . . O2 O 0.322(3) 0.1044(17) 0.174(2) 0.39(3) Uani 1 1 d . . H2 H 0.2583 0.1493 0.1715 0.590 Uiso 1 1 calc R 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 C1 0.060(10) 0.045(8) 0.059(10) -0.007(7) 0.001(8) 0.017(7) C2 0.039(8) 0.057(9) 0.066(11) 0.004(8) -0.017(7) -0.007(7) C3 0.044(8) 0.057(9) 0.073(12) 0.013(8) -0.003(8) 0.000(7) C4 0.050(9) 0.084(10) 0.062(11) 0.004(9) -0.013(9) 0.003(9) C5 0.046(9) 0.082(11) 0.057(12) 0.011(8) 0.006(8) 0.002(8) C6 0.033(8) 0.063(8) 0.056(10) 0.013(8) 0.005(7) 0.006(6) C7 0.086(15) 0.128(15) 0.074(14) 0.003(11) -0.015(10) -0.010(12) C8 0.039(9) 0.070(10) 0.082(13) 0.010(10) -0.003(8) 0.004(8) C9 0.044(10) 0.069(10) 0.094(14) -0.002(10) -0.008(9) -0.006(8) C10 0.053(10) 0.066(10) 0.092(14) 0.005(10) -0.006(9) -0.006(8) C11 0.051(10) 0.091(12) 0.112(17) -0.022(12) -0.035(10) -0.003(9) C12 0.115(17) 0.104(14) 0.087(15) -0.001(12) -0.048(13) 0.007(12) C13 0.094(12) 0.054(9) 0.078(11) -0.008(8) -0.026(12) 0.009(11) C14 0.090(14) 0.072(11) 0.133(18) -0.005(12) -0.016(12) -0.007(10) C15 0.060(10) 0.083(11) 0.052(11) -0.006(9) -0.002(9) -0.008(9) C16 0.086(14) 0.084(11) 0.065(12) 0.012(9) -0.005(9) -0.027(10) C17 0.114(16) 0.064(10) 0.073(13) 0.016(10) 0.014(11) -0.028(11) C18 0.16(2) 0.107(15) 0.087(16) 0.036(13) -0.033(15) -0.019(15) C19 0.18(3) 0.127(17) 0.117(19) 0.032(15) -0.085(19) -0.03(2) C20 0.13(2) 0.074(11) 0.096(15) 0.012(11) -0.004(13) -0.032(13) C21 0.14(2) 0.116(17) 0.17(2) 0.012(17) 0.081(19) -0.018(15) C22 0.094(19) 0.24(3) 0.17(3) -0.02(3) -0.007(18) 0.04(2) Co1 0.0401(10) 0.0572(10) 0.0698(13) -0.0024(10) -0.0091(11) 0.0013(10) Co2 0.0626(14) 0.0577(11) 0.0724(15) 0.0053(10) -0.0165(13) -0.0037(12) N1 0.030(6) 0.076(8) 0.053(8) -0.004(7) 0.010(6) -0.004(6) N2 0.029(7) 0.076(8) 0.087(10) -0.015(8) -0.016(7) 0.008(6) N3 0.046(7) 0.082(9) 0.070(10) -0.003(7) -0.001(7) -0.015(7) N4 0.079(10) 0.058(8) 0.072(9) 0.015(7) -0.012(8) -0.007(7) N5 0.054(8) 0.061(7) 0.070(9) -0.001(6) -0.013(7) 0.009(7) N6 0.037(6) 0.107(8) 0.161(10) -0.006(8) 0.001(8) 0.012(7) N7 0.037(6) 0.107(8) 0.161(10) -0.006(8) 0.001(8) 0.012(7) N8 0.040(7) 0.072(8) 0.088(11) -0.019(8) -0.028(7) 0.019(7) N9 0.027(7) 0.084(11) 0.105(14) -0.014(9) -0.020(8) 0.010(7) N10 0.076(13) 0.123(13) 0.126(16) -0.031(12) -0.021(10) 0.032(10) N11 0.045(8) 0.090(10) 0.069(10) 0.000(8) -0.004(7) 0.000(7) N12 0.127(16) 0.087(13) 0.108(15) 0.010(10) 0.024(13) -0.038(13) N13 0.28(3) 0.135(18) 0.19(2) -0.077(18) 0.15(2) -0.09(2) N14 0.098(11) 0.099(11) 0.123(11) -0.002(9) -0.014(9) 0.031(8) N15 0.098(11) 0.099(11) 0.123(11) -0.002(9) -0.014(9) 0.031(8) N16 0.19(2) 0.19(2) 0.139(18) -0.002(16) -0.017(18) 0.10(2) O1 0.053(6) 0.060(6) 0.052(6) 0.005(5) -0.017(5) 0.001(4) O2 0.17(2) 0.160(18) 0.85(9) 0.15(3) 0.21(4) -0.002(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' 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 O1 C1 C2 119.5(14) O1 C1 C6 122.6(13) C2 C1 C6 117.8(14) C3 C2 C1 119.5(14) C3 C2 C15 114.6(13) C1 C2 C15 125.8(14) C4 C3 C2 123.3(14) C4 C3 H3 118.4 C2 C3 H3 118.4 C3 C4 C5 117.0(14) C3 C4 C7 123.0(15) C5 C4 C7 120.0(15) C6 C5 C4 120.2(14) C6 C5 H5 119.9 C4 C5 H5 119.9 C5 C6 C1 122.2(14) C5 C6 C8 116.9(13) C1 C6 C8 120.8(14) C4 C7 H7A 109.5 C4 C7 H7B 109.5 H7A C7 H7B 109.5 C4 C7 H7C 109.5 H7A C7 H7C 109.5 H7B C7 H7C 109.5 N1 C8 C6 126.2(15) N1 C8 H8 116.9 C6 C8 H8 116.9 C10 C9 N1 107.5(13) C10 C9 H9A 110.2 N1 C9 H9A 110.2 C10 C9 H9B 110.2 N1 C9 H9B 110.2 H9A C9 H9B 108.5 C9 C10 N2 109.0(12) C9 C10 H10A 109.9 N2 C10 H10A 109.9 C9 C10 H10B 109.9 N2 C10 H10B 109.9 H10A C10 H10B 108.3 C12 C11 N2 116.0(15) C12 C11 H11A 108.3 N2 C11 H11A 108.3 C12 C11 H11B 108.3 N2 C11 H11B 108.3 H11A C11 H11B 107.4 C11 C12 H12A 109.5 C11 C12 H12B 109.5 H12A C12 H12B 109.5 C11 C12 H12C 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 N2 C13 C14 117.9(16) N2 C13 H13A 107.8 C14 C13 H13A 107.8 N2 C13 H13B 107.8 C14 C13 H13B 107.8 H13A C13 H13B 107.2 C13 C14 H14A 109.5 C13 C14 H14B 109.5 H14A C14 H14B 109.5 C13 C14 H14C 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 N3 C15 C2 125.9(15) N3 C15 H15 117.1 C2 C15 H15 117.1 N3 C16 C17 107.8(14) N3 C16 H16A 110.1 C17 C16 H16A 110.1 N3 C16 H16B 110.1 C17 C16 H16B 110.1 H16A C16 H16B 108.5 N4 C17 C16 111.3(13) N4 C17 H17A 109.4 C16 C17 H17A 109.4 N4 C17 H17B 109.4 C16 C17 H17B 109.4 H17A C17 H17B 108.0 C19 C18 N4 115.5(16) C19 C18 H18A 108.4 N4 C18 H18A 108.4 C19 C18 H18B 108.4 N4 C18 H18B 108.4 H18A C18 H18B 107.5 C18 C19 H19A 109.5 C18 C19 H19B 109.5 H19A C19 H19B 109.5 C18 C19 H19C 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 N4 C20 C21 116.8(15) N4 C20 H20A 108.1 C21 C20 H20A 108.1 N4 C20 H20B 108.1 C21 C20 H20B 108.1 H20A C20 H20B 107.3 C20 C21 H21A 109.5 C20 C21 H21B 109.5 H21A C21 H21B 109.5 C20 C21 H21C 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 O2 C22 H22A 109.5 O2 C22 H22B 109.5 H22A C22 H22B 109.5 O2 C22 H22C 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 N1 Co1 O1 92.5(5) N1 Co1 N8 89.8(6) O1 Co1 N8 87.6(4) N1 Co1 N5 89.9(5) O1 Co1 N5 90.6(5) N8 Co1 N5 178.2(5) N1 Co1 N11 171.9(6) O1 Co1 N11 79.3(5) N8 Co1 N11 89.7(6) N5 Co1 N11 90.3(6) N1 Co1 N2 87.1(6) O1 Co1 N2 179.6(5) N8 Co1 N2 92.2(5) N5 Co1 N2 89.5(5) N11 Co1 N2 101.0(6) N3 Co2 N14 106.8(6) N3 Co2 N11 136.7(5) N14 Co2 N11 113.5(6) N3 Co2 O1 85.8(5) N14 Co2 O1 98.9(6) N11 Co2 O1 73.3(5) N3 Co2 N4 81.8(5) N14 Co2 N4 100.0(7) N11 Co2 N4 105.4(6) O1 Co2 N4 159.7(5) C8 N1 C9 121.4(14) C8 N1 Co1 127.4(11) C9 N1 Co1 111.1(11) C13 N2 C10 108.1(11) C13 N2 C11 109.3(13) C10 N2 C11 108.6(13) C13 N2 Co1 114.8(9) C10 N2 Co1 101.4(9) C11 N2 Co1 114.0(9) C15 N3 C16 115.0(13) C15 N3 Co2 129.3(11) C16 N3 Co2 115.3(10) C18 N4 C17 107.9(13) C18 N4 C20 114.9(16) C17 N4 C20 109.9(14) C18 N4 Co2 113.6(13) C17 N4 Co2 101.5(10) C20 N4 Co2 108.2(9) N6 N5 Co1 118.5(11) N7 N6 N5 177.8(19) N9 N8 Co1 117.6(10) N10 N9 N8 179(2) N12 N11 Co1 126.5(13) N12 N11 Co2 125.0(12) Co1 N11 Co2 102.5(7) N13 N12 N11 175(3) N15 N14 Co2 156(2) N14 N15 N16 174(3) C1 O1 Co1 126.5(9) C1 O1 Co2 130.6(9) Co1 O1 Co2 102.1(5) C22 O2 H2 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 O1 1.313(16) C1 C2 1.386(19) C1 C6 1.399(19) C2 C3 1.384(19) C2 C15 1.45(2) C3 C4 1.37(2) C3 H3 0.9300 C4 C5 1.41(2) C4 C7 1.48(2) C5 C6 1.364(19) C5 H5 0.9300 C6 C8 1.49(2) C7 H7A 0.9600 C7 H7B 0.9600 C7 H7C 0.9600 C8 N1 1.226(18) C8 H8 0.9300 C9 C10 1.45(2) C9 N1 1.449(18) C9 H9A 0.9700 C9 H9B 0.9700 C10 N2 1.519(19) C10 H10A 0.9700 C10 H10B 0.9700 C11 C12 1.50(2) C11 N2 1.529(19) C11 H11A 0.9700 C11 H11B 0.9700 C12 H12A 0.9600 C12 H12B 0.9600 C12 H12C 0.9600 C13 N2 1.450(19) C13 C14 1.54(2) C13 H13A 0.9700 C13 H13B 0.9700 C14 H14A 0.9600 C14 H14B 0.9600 C14 H14C 0.9600 C15 N3 1.250(16) C15 H15 0.9300 C16 N3 1.490(19) C16 C17 1.50(2) C16 H16A 0.9700 C16 H16B 0.9700 C17 N4 1.47(2) C17 H17A 0.9700 C17 H17B 0.9700 C18 C19 1.44(2) C18 N4 1.46(2) C18 H18A 0.9700 C18 H18B 0.9700 C19 H19A 0.9600 C19 H19B 0.9600 C19 H19C 0.9600 C20 N4 1.47(2) C20 C21 1.54(3) C20 H20A 0.9700 C20 H20B 0.9700 C21 H21A 0.9600 C21 H21B 0.9600 C21 H21C 0.9600 C22 O2 1.33(3) C22 H22A 0.9600 C22 H22B 0.9600 C22 H22C 0.9600 Co1 N1 1.874(12) Co1 O1 1.910(9) Co1 N8 1.952(12) Co1 N5 1.952(13) Co1 N11 1.962(15) Co1 N2 2.041(12) Co2 N3 1.984(13) Co2 N14 1.998(17) Co2 N11 2.039(15) Co2 O1 2.099(10) Co2 N4 2.188(14) N5 N6 1.155(18) N6 N7 1.145(19) N8 N9 1.185(18) N9 N10 1.127(19) N11 N12 1.19(2) N12 N13 1.14(2) N14 N15 1.05(2) N15 N16 1.11(2) O2 H2 0.8200