#------------------------------------------------------------------------------ #$Date: 2020-08-18 05:04:26 +0300 (Tue, 18 Aug 2020) $ #$Revision: 255417 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/51/7705196.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_7705196 loop_ _publ_author_name 'Ghosh, Subrata' 'Selvamani, S.' 'Kamilya, Sujit' 'Mehta, Sakshi' 'Mondal, Abhishake' _publ_section_title ; Tuning of Spin Crossover Properties in a Series of Mononuclear Cobalt(II) Complexes Based on Macrocyclic Tetradentate Ligand and Pseudohalide Coligands ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02546A _journal_year 2020 _chemical_formula_sum 'C30 H32 Co N10' _chemical_formula_weight 591.58 _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 difmap _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2020-05-15 deposited with the CCDC. 2020-08-17 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 110.0870(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.3379(2) _cell_length_b 12.6230(2) _cell_length_c 18.7965(4) _cell_measurement_reflns_used 6235 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 25.31 _cell_measurement_theta_min 2.29 _cell_volume 2972.16(9) _computing_cell_refinement 'Bruker APEX2' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'CrystalMaker 10.4.2' _computing_publication_material 'Encifer (Allen et al, 2004)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.999 _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 0.0594 _diffrn_reflns_av_unetI/netI 0.0474 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 48238 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.985 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.599 _diffrn_reflns_theta_min 2.291 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 0.615 _exptl_absorpt_correction_T_max 0.943 _exptl_absorpt_correction_T_min 0.875 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour Brown _exptl_crystal_density_diffrn 1.322 _exptl_crystal_description Block _exptl_crystal_F_000 1236 _exptl_crystal_size_max 0.700 _exptl_crystal_size_mid 0.420 _exptl_crystal_size_min 0.335 _refine_diff_density_max 0.320 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.048 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 498 _refine_ls_number_reflns 9010 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.999 _refine_ls_R_factor_all 0.0938 _refine_ls_R_factor_gt 0.0447 _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^)+(0.0559P)^2^+0.2484P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1035 _refine_ls_wR_factor_ref 0.1247 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5288 _reflns_number_total 9010 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02546a2.cif _cod_data_source_block Complex3 _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7705196 _shelx_shelxl_version_number 2016/6 _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 0.635 _shelx_estimated_absorpt_t_max 0.775 _shelx_res_file ; TITL SIR92 run in space group P 1 21/c 1 shelx.res created by SHELXL-2016/6 at 10:22:13 on 12-May-2020 CELL 0.71073 13.3379 12.6230 18.7965 90.000 110.087 90.000 ZERR 4.00 0.0002 0.0002 0.0004 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N CO UNIT 120 128 40 4 MERG 2 FMAP 2 PLAN 25 ACTA BOND $H CONF L.S. 10 TEMP 23.00 WGHT 0.055900 0.248400 FVAR 0.09572 CO1 4 0.248206 0.158328 0.755446 11.00000 0.03619 0.04971 = 0.03403 -0.00022 0.00965 -0.00283 N9 3 -0.126187 0.288865 0.481938 11.00000 0.08048 0.07501 = 0.08883 -0.01067 0.00450 0.00867 N1 3 0.214457 0.328021 0.789704 11.00000 0.04065 0.04861 = 0.04376 0.00151 0.01630 -0.00062 N4 3 0.189929 0.127777 0.833384 11.00000 0.03952 0.04760 = 0.04064 -0.00156 0.01263 -0.00817 N2 3 0.384097 0.186322 0.832645 11.00000 0.03725 0.04600 = 0.03566 -0.00200 0.01245 -0.00586 N3 3 0.316387 -0.012258 0.787677 11.00000 0.04559 0.04595 = 0.04029 -0.00541 0.00616 -0.00214 C11 1 0.502797 0.305504 0.917107 11.00000 0.05230 0.05269 = 0.04555 -0.00477 0.01507 -0.01610 N6 3 0.109961 0.136339 0.677865 11.00000 0.04990 0.06442 = 0.04801 -0.00086 0.00956 -0.00185 N5 3 0.310718 0.185602 0.679115 11.00000 0.05445 0.05935 = 0.04382 0.00268 0.01656 0.00344 C10 1 0.401415 0.279125 0.869676 11.00000 0.04364 0.04806 = 0.03589 -0.00020 0.01544 -0.00975 C21 1 0.127802 0.201745 0.849214 11.00000 0.04034 0.06033 = 0.04690 -0.00609 0.01802 -0.01043 C23 1 0.199356 0.422510 0.736897 11.00000 0.06238 0.04994 = 0.05300 0.00880 0.01958 0.00467 C27 1 0.276947 -0.102954 0.731621 11.00000 0.05876 0.04798 = 0.05634 -0.01303 0.00442 -0.00071 C9 1 0.305034 0.345162 0.861997 11.00000 0.04842 0.04951 = 0.04467 -0.00447 0.01719 -0.00701 C15 1 0.431025 0.010338 0.804065 11.00000 0.04370 0.05631 = 0.04948 -0.00515 0.00870 0.00479 C14 1 0.462048 0.113538 0.845886 11.00000 0.03783 0.05298 = 0.04094 0.00029 0.01126 -0.00168 C13 1 0.563167 0.135640 0.895510 11.00000 0.03774 0.06614 = 0.05214 0.00197 0.00842 -0.00018 C17 1 0.211078 0.035935 0.871156 11.00000 0.04947 0.05347 = 0.04190 -0.00180 0.01044 -0.01652 C5 1 0.033830 0.129960 0.626283 11.00000 0.04806 0.06357 = 0.04901 -0.00320 0.01588 -0.00023 C28 1 0.278770 -0.069328 0.654511 11.00000 0.07810 0.06869 = 0.05297 -0.02086 0.00812 0.00721 C19 1 0.095346 0.085213 0.937648 11.00000 0.06664 0.09164 = 0.05764 -0.00006 0.03271 -0.02353 C20 1 0.080083 0.181870 0.901929 11.00000 0.05384 0.07893 = 0.06249 -0.00743 0.03205 -0.01066 C26 1 0.307728 0.449084 0.729400 11.00000 0.07837 0.06290 = 0.06646 0.01025 0.03357 -0.01078 C6 1 -0.059409 0.122952 0.563577 11.00000 0.04955 0.07444 = 0.04902 -0.00293 0.00377 -0.00941 C22 1 0.116510 0.304109 0.806754 11.00000 0.04313 0.05727 = 0.05672 -0.00222 0.02290 0.00214 C16 1 0.297656 -0.031030 0.860078 11.00000 0.05961 0.04606 = 0.04677 0.00353 0.00875 -0.00744 C7 1 -0.096548 0.214304 0.518990 11.00000 0.04826 0.07170 = 0.06069 -0.01404 0.00535 0.00063 C12 1 0.583445 0.232931 0.930053 11.00000 0.04071 0.07372 = 0.05167 -0.00072 0.00560 -0.01621 C24 1 0.158063 0.520413 0.766001 11.00000 0.09456 0.05477 = 0.08755 0.01033 0.03680 0.01704 C18 1 0.161846 0.011768 0.922850 11.00000 0.06551 0.06817 = 0.05518 0.00887 0.01951 -0.02018 C25 1 0.122078 0.393183 0.658412 11.00000 0.07761 0.07179 = 0.05823 0.01803 0.01397 0.01081 N10 3 -0.149864 -0.056895 0.525963 11.00000 0.15582 0.10860 = 0.08478 0.01863 -0.00205 -0.06502 C29 1 0.344808 -0.202771 0.757813 11.00000 0.08946 0.04866 = 0.08603 -0.01280 0.00846 0.00828 C30 1 0.161093 -0.127185 0.724474 11.00000 0.06525 0.06259 = 0.08182 -0.02038 0.00690 -0.01719 C8 1 -0.109528 0.023776 0.542480 11.00000 0.07995 0.08861 = 0.05040 0.01108 0.00155 -0.02410 C2 1 0.414315 0.214760 0.589995 11.00000 0.05481 0.05002 = 0.04309 0.00318 0.02029 0.00580 C1 1 0.355532 0.199177 0.637730 11.00000 0.04919 0.05226 = 0.03875 -0.00165 0.01050 0.00125 C4 1 0.403923 0.309156 0.548499 11.00000 0.05110 0.05733 = 0.04115 -0.00023 0.01598 0.00823 N8 3 0.397491 0.386436 0.516137 11.00000 0.09569 0.06207 = 0.06720 0.01716 0.03224 0.01868 C3 1 0.491521 0.139512 0.590505 11.00000 0.07899 0.05748 = 0.05042 0.01024 0.02937 0.01587 N7 3 0.557189 0.079314 0.592757 11.00000 0.12182 0.08556 = 0.09177 0.02357 0.05156 0.05154 H22A 2 0.099795 0.359980 0.837297 11.00000 0.04707 H16A 2 0.283676 -0.103335 0.867888 11.00000 0.06179 H15B 2 0.446152 0.015973 0.755647 11.00000 0.05103 H11 2 0.508299 0.370962 0.940046 11.00000 0.04905 H9A 2 0.283751 0.329133 0.901322 11.00000 0.04364 H16B 2 0.361988 -0.015008 0.901980 11.00000 0.06265 H30A 2 0.114215 -0.060486 0.712425 11.00000 0.08708 H20 2 0.038478 0.234281 0.911931 11.00000 0.05865 H12 2 0.647131 0.244607 0.964035 11.00000 0.06893 H22B 2 0.051967 0.294059 0.759519 11.00000 0.05798 H25B 2 0.149750 0.332373 0.637186 11.00000 0.07973 H28B 2 0.248689 -0.130291 0.617661 11.00000 0.08375 H28A 2 0.231647 -0.007417 0.635617 11.00000 0.07621 H15A 2 0.477497 -0.049411 0.837045 11.00000 0.06397 H19 2 0.065309 0.070666 0.977928 11.00000 0.09296 H18 2 0.179033 -0.053143 0.945185 11.00000 0.06027 H26B 2 0.341436 0.386752 0.718695 11.00000 0.06774 H25A 2 0.048063 0.371848 0.659499 11.00000 0.06971 H13 2 0.614647 0.081584 0.905158 11.00000 0.05721 H29A 2 0.348049 -0.226789 0.811006 11.00000 0.07144 H24A 2 0.202253 0.541315 0.814154 11.00000 0.07270 H28C 2 0.351354 -0.057558 0.655547 11.00000 0.09705 H26A 2 0.360774 0.478111 0.777368 11.00000 0.08617 H24B 2 0.087346 0.504743 0.766814 11.00000 0.10240 H9B 2 0.325309 0.417774 0.869532 11.00000 0.06577 H30B 2 0.134467 -0.171307 0.682445 11.00000 0.07891 H29B 2 0.311501 -0.260026 0.725296 11.00000 0.09863 H30C 2 0.152041 -0.158131 0.768749 11.00000 0.06943 H26C 2 0.296120 0.506158 0.689896 11.00000 0.08330 H25C 2 0.115192 0.450123 0.624512 11.00000 0.10253 H29C 2 0.416733 -0.189262 0.754650 11.00000 0.09217 H24C 2 0.144981 0.585022 0.725195 11.00000 0.10608 HKLF 4 REM SIR92 run in space group P 1 21/c 1 REM R1 = 0.0447 for 5288 Fo > 4sig(Fo) and 0.0938 for all 9010 data REM 498 parameters refined using 0 restraints END WGHT 0.0523 0.3655 REM Highest difference peak 0.320, deepest hole -0.474, 1-sigma level 0.048 Q1 1 -0.1667 0.2580 0.5301 11.00000 0.05 0.32 Q2 1 -0.2032 0.0043 0.5301 11.00000 0.05 0.26 Q3 1 -0.1562 0.0749 0.5440 11.00000 0.05 0.22 Q4 1 0.2504 0.0375 0.7512 11.00000 0.05 0.21 Q5 1 0.2307 0.1126 0.6872 11.00000 0.05 0.18 Q6 1 0.5920 0.1429 0.5908 11.00000 0.05 0.18 Q7 1 0.0449 0.1327 0.6726 11.00000 0.05 0.18 Q8 1 0.3246 0.1692 0.8200 11.00000 0.05 0.18 Q9 1 0.1735 0.1508 0.6908 11.00000 0.05 0.18 Q10 1 0.5114 0.3004 0.6404 11.00000 0.05 0.17 Q11 1 -0.1440 0.1739 0.5889 11.00000 0.05 0.17 Q12 1 0.2952 0.2221 0.7231 11.00000 0.05 0.17 Q13 1 -0.1267 -0.0479 0.4929 11.00000 0.05 0.17 Q14 1 0.1989 0.0771 0.8476 11.00000 0.05 0.16 Q15 1 0.3880 0.2267 0.8508 11.00000 0.05 0.16 Q16 1 -0.1233 0.1649 0.5514 11.00000 0.05 0.16 Q17 1 0.2380 0.1738 0.6839 11.00000 0.05 0.16 Q18 1 0.2033 0.5985 0.7556 11.00000 0.05 0.16 Q19 1 0.2709 0.1839 0.6300 11.00000 0.05 0.15 Q20 1 -0.0152 -0.0609 0.5694 11.00000 0.05 0.15 Q21 1 0.1437 -0.1856 0.9301 11.00000 0.05 0.15 Q22 1 0.2414 0.5003 0.6584 11.00000 0.05 0.15 Q23 1 -0.0821 0.1186 0.6094 11.00000 0.05 0.15 Q24 1 0.3717 -0.1252 0.6542 11.00000 0.05 0.15 Q25 1 -0.1136 0.2381 0.5770 11.00000 0.05 0.15 ; _shelx_res_checksum 72880 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 0.24821(2) 0.15833(2) 0.75545(2) 0.04060(9) Uani 1 1 d . . . . . N9 N -0.1262(2) 0.2889(2) 0.48194(15) 0.0878(7) Uani 1 1 d . . . . . N1 N 0.21446(13) 0.32802(13) 0.78970(9) 0.0439(4) Uani 1 1 d . . . . . N4 N 0.18993(13) 0.12778(14) 0.83338(9) 0.0429(4) Uani 1 1 d . . . . . N2 N 0.38410(13) 0.18632(13) 0.83264(9) 0.0397(4) Uani 1 1 d . . . . . N3 N 0.31639(13) -0.01226(14) 0.78768(9) 0.0462(4) Uani 1 1 d . . . . . C11 C 0.50280(18) 0.3055(2) 0.91711(12) 0.0506(5) Uani 1 1 d . . . . . N6 N 0.10996(16) 0.13634(16) 0.67786(11) 0.0560(5) Uani 1 1 d . . . . . N5 N 0.31072(15) 0.18560(15) 0.67912(10) 0.0526(4) Uani 1 1 d . . . . . C10 C 0.40141(16) 0.27913(16) 0.86968(11) 0.0421(4) Uani 1 1 d . . . . . C21 C 0.12780(16) 0.20175(18) 0.84921(12) 0.0484(5) Uani 1 1 d . . . . . C23 C 0.1994(2) 0.42251(18) 0.73690(13) 0.0552(6) Uani 1 1 d . . . . . C27 C 0.2769(2) -0.10295(19) 0.73162(14) 0.0583(6) Uani 1 1 d . . . . . C9 C 0.30503(18) 0.34516(19) 0.86200(13) 0.0472(5) Uani 1 1 d . . . . . C15 C 0.43102(17) 0.01034(19) 0.80407(14) 0.0517(5) Uani 1 1 d . . . . . C14 C 0.46205(16) 0.11354(17) 0.84589(11) 0.0445(5) Uani 1 1 d . . . . . C13 C 0.56317(18) 0.1356(2) 0.89551(13) 0.0538(6) Uani 1 1 d . . . . . C17 C 0.21108(17) 0.03593(18) 0.87116(12) 0.0496(5) Uani 1 1 d . . . . . C5 C 0.03383(19) 0.12996(19) 0.62628(13) 0.0537(5) Uani 1 1 d . . . . . C28 C 0.2788(3) -0.0693(3) 0.65451(15) 0.0703(8) Uani 1 1 d . . . . . C19 C 0.0953(2) 0.0852(2) 0.93765(15) 0.0690(7) Uani 1 1 d . . . . . C20 C 0.0801(2) 0.1819(2) 0.90193(15) 0.0620(6) Uani 1 1 d . . . . . C26 C 0.3077(3) 0.4491(3) 0.72940(18) 0.0670(7) Uani 1 1 d . . . . . C6 C -0.05941(19) 0.1230(2) 0.56358(13) 0.0611(6) Uani 1 1 d . . . . . C22 C 0.11651(18) 0.3041(2) 0.80675(14) 0.0509(5) Uani 1 1 d . . . . . C16 C 0.2977(2) -0.03103(19) 0.86008(13) 0.0533(5) Uani 1 1 d . . . . . C7 C -0.09655(19) 0.2143(2) 0.51899(15) 0.0637(6) Uani 1 1 d . . . . . C12 C 0.5834(2) 0.2329(2) 0.93005(14) 0.0580(6) Uani 1 1 d . . . . . C24 C 0.1581(3) 0.5204(2) 0.7660(2) 0.0775(8) Uani 1 1 d . . . . . C18 C 0.1618(2) 0.0118(2) 0.92285(14) 0.0633(7) Uani 1 1 d . . . . . C25 C 0.1221(3) 0.3932(3) 0.65841(16) 0.0716(8) Uani 1 1 d . . . . . N10 N -0.1499(3) -0.0569(3) 0.52596(16) 0.1277(13) Uani 1 1 d . . . . . C29 C 0.3448(3) -0.2028(2) 0.7578(2) 0.0803(9) Uani 1 1 d . . . . . C30 C 0.1611(2) -0.1272(3) 0.7245(2) 0.0746(8) Uani 1 1 d . . . . . C8 C -0.1095(2) 0.0238(3) 0.54248(15) 0.0784(8) Uani 1 1 d . . . . . C2 C 0.41431(18) 0.21476(17) 0.58999(12) 0.0484(5) Uani 1 1 d . . . . . C1 C 0.35553(17) 0.19918(18) 0.63773(12) 0.0479(5) Uani 1 1 d . . . . . C4 C 0.40392(17) 0.30916(19) 0.54850(12) 0.0498(5) Uani 1 1 d . . . . . N8 N 0.39749(19) 0.38644(19) 0.51614(13) 0.0739(6) Uani 1 1 d . . . . . C3 C 0.4915(2) 0.1395(2) 0.59050(13) 0.0604(6) Uani 1 1 d . . . . . N7 N 0.5572(2) 0.0793(2) 0.59276(15) 0.0959(9) Uani 1 1 d . . . . . H22A H 0.0998(16) 0.3600(17) 0.8373(12) 0.047(6) Uiso 1 1 d . . . . . H16A H 0.2837(18) -0.103(2) 0.8679(13) 0.062(7) Uiso 1 1 d . . . . . H15B H 0.4462(16) 0.0160(17) 0.7556(13) 0.051(6) Uiso 1 1 d . . . . . H11 H 0.5083(17) 0.3710(18) 0.9400(12) 0.049(6) Uiso 1 1 d . . . . . H9A H 0.2838(16) 0.3291(16) 0.9013(12) 0.044(6) Uiso 1 1 d . . . . . H16B H 0.3620(19) -0.0150(19) 0.9020(14) 0.063(7) Uiso 1 1 d . . . . . H30A H 0.114(2) -0.060(2) 0.7124(16) 0.087(9) Uiso 1 1 d . . . . . H20 H 0.0385(19) 0.2343(19) 0.9119(13) 0.059(7) Uiso 1 1 d . . . . . H12 H 0.647(2) 0.245(2) 0.9640(14) 0.069(8) Uiso 1 1 d . . . . . H22B H 0.0520(19) 0.2941(18) 0.7595(13) 0.058(6) Uiso 1 1 d . . . . . H25B H 0.150(2) 0.332(2) 0.6372(16) 0.080(9) Uiso 1 1 d . . . . . H28B H 0.249(2) -0.130(2) 0.6177(16) 0.084(8) Uiso 1 1 d . . . . . H28A H 0.232(2) -0.007(2) 0.6356(15) 0.076(8) Uiso 1 1 d . . . . . H15A H 0.4775(19) -0.0494(19) 0.8370(13) 0.064(7) Uiso 1 1 d . . . . . H19 H 0.065(2) 0.071(2) 0.9779(16) 0.093(9) Uiso 1 1 d . . . . . H18 H 0.1790(18) -0.053(2) 0.9452(13) 0.060(7) Uiso 1 1 d . . . . . H26B H 0.341(2) 0.387(2) 0.7187(14) 0.068(8) Uiso 1 1 d . . . . . H25A H 0.048(2) 0.372(2) 0.6595(14) 0.070(8) Uiso 1 1 d . . . . . H13 H 0.6146(18) 0.0816(18) 0.9052(12) 0.057(7) Uiso 1 1 d . . . . . H29A H 0.348(2) -0.227(2) 0.8110(16) 0.071(8) Uiso 1 1 d . . . . . H24A H 0.202(2) 0.541(2) 0.8142(17) 0.073(9) Uiso 1 1 d . . . . . H28C H 0.351(3) -0.058(2) 0.6555(17) 0.097(11) Uiso 1 1 d . . . . . H26A H 0.361(2) 0.478(2) 0.7774(18) 0.086(9) Uiso 1 1 d . . . . . H24B H 0.087(3) 0.505(3) 0.7668(18) 0.102(11) Uiso 1 1 d . . . . . H9B H 0.3253(18) 0.418(2) 0.8695(13) 0.066(7) Uiso 1 1 d . . . . . H30B H 0.134(2) -0.171(2) 0.6824(17) 0.079(9) Uiso 1 1 d . . . . . H29B H 0.312(2) -0.260(3) 0.7253(18) 0.099(10) Uiso 1 1 d . . . . . H30C H 0.152(2) -0.158(2) 0.7687(16) 0.069(8) Uiso 1 1 d . . . . . H26C H 0.296(2) 0.506(2) 0.6899(16) 0.083(8) Uiso 1 1 d . . . . . H25C H 0.115(2) 0.450(3) 0.6245(18) 0.103(10) Uiso 1 1 d . . . . . H29C H 0.417(3) -0.189(2) 0.7546(17) 0.092(10) Uiso 1 1 d . . . . . H24C H 0.145(2) 0.585(3) 0.7252(18) 0.106(10) 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 0.03619(15) 0.04971(17) 0.03403(15) -0.00022(12) 0.00965(11) -0.00283(12) N9 0.0805(17) 0.0750(17) 0.0888(18) -0.0107(14) 0.0045(14) 0.0087(14) N1 0.0406(9) 0.0486(10) 0.0438(9) 0.0015(7) 0.0163(7) -0.0006(7) N4 0.0395(9) 0.0476(10) 0.0406(9) -0.0016(7) 0.0126(7) -0.0082(7) N2 0.0372(9) 0.0460(9) 0.0357(8) -0.0020(7) 0.0124(7) -0.0059(7) N3 0.0456(10) 0.0460(10) 0.0403(9) -0.0054(7) 0.0062(7) -0.0021(8) C11 0.0523(13) 0.0527(13) 0.0455(12) -0.0048(10) 0.0151(10) -0.0161(11) N6 0.0499(11) 0.0644(13) 0.0480(11) -0.0009(9) 0.0096(9) -0.0018(9) N5 0.0545(11) 0.0593(12) 0.0438(10) 0.0027(8) 0.0166(9) 0.0034(9) C10 0.0436(11) 0.0481(12) 0.0359(10) -0.0002(8) 0.0154(8) -0.0098(9) C21 0.0403(11) 0.0603(13) 0.0469(11) -0.0061(10) 0.0180(9) -0.0104(10) C23 0.0624(14) 0.0499(13) 0.0530(13) 0.0088(10) 0.0196(11) 0.0047(11) C27 0.0588(14) 0.0480(13) 0.0563(14) -0.0130(11) 0.0044(11) -0.0007(11) C9 0.0484(12) 0.0495(12) 0.0447(11) -0.0045(10) 0.0172(10) -0.0070(10) C15 0.0437(12) 0.0563(14) 0.0495(13) -0.0051(11) 0.0087(10) 0.0048(10) C14 0.0378(11) 0.0530(12) 0.0409(11) 0.0003(9) 0.0113(9) -0.0017(9) C13 0.0377(12) 0.0661(15) 0.0521(13) 0.0020(11) 0.0084(10) -0.0002(11) C17 0.0495(12) 0.0535(13) 0.0419(11) -0.0018(9) 0.0104(9) -0.0165(10) C5 0.0481(13) 0.0636(14) 0.0490(13) -0.0032(11) 0.0159(11) -0.0002(11) C28 0.078(2) 0.0687(18) 0.0530(15) -0.0209(13) 0.0081(14) 0.0072(16) C19 0.0666(17) 0.092(2) 0.0576(15) -0.0001(14) 0.0327(13) -0.0235(15) C20 0.0538(14) 0.0789(18) 0.0625(15) -0.0074(13) 0.0321(12) -0.0107(13) C26 0.0784(19) 0.0629(17) 0.0665(18) 0.0103(14) 0.0336(15) -0.0108(15) C6 0.0495(13) 0.0744(16) 0.0490(13) -0.0029(12) 0.0038(10) -0.0094(12) C22 0.0431(12) 0.0573(13) 0.0567(13) -0.0022(11) 0.0229(11) 0.0021(10) C16 0.0596(15) 0.0461(13) 0.0468(12) 0.0035(10) 0.0087(11) -0.0074(11) C7 0.0483(14) 0.0717(18) 0.0607(15) -0.0140(14) 0.0054(11) 0.0006(13) C12 0.0407(13) 0.0737(17) 0.0517(13) -0.0007(12) 0.0056(10) -0.0162(12) C24 0.095(3) 0.0548(16) 0.088(2) 0.0103(16) 0.037(2) 0.0170(16) C18 0.0655(16) 0.0682(17) 0.0552(14) 0.0089(13) 0.0195(12) -0.0202(14) C25 0.078(2) 0.0718(19) 0.0582(16) 0.0180(15) 0.0140(14) 0.0108(16) N10 0.156(3) 0.109(2) 0.085(2) 0.0186(17) -0.0021(19) -0.065(2) C29 0.089(2) 0.0487(16) 0.086(2) -0.0128(16) 0.0085(19) 0.0083(16) C30 0.0652(18) 0.0626(18) 0.082(2) -0.0204(17) 0.0069(16) -0.0172(15) C8 0.0800(19) 0.089(2) 0.0504(15) 0.0111(14) 0.0015(13) -0.0241(17) C2 0.0548(13) 0.0500(12) 0.0431(11) 0.0032(9) 0.0203(10) 0.0058(10) C1 0.0492(12) 0.0523(12) 0.0388(11) -0.0017(9) 0.0105(9) 0.0013(10) C4 0.0511(13) 0.0573(13) 0.0411(11) -0.0002(10) 0.0160(10) 0.0082(10) N8 0.0957(17) 0.0621(13) 0.0672(14) 0.0172(12) 0.0322(13) 0.0187(12) C3 0.0790(17) 0.0575(14) 0.0504(13) 0.0102(11) 0.0294(12) 0.0159(13) N7 0.122(2) 0.0856(18) 0.0918(18) 0.0236(15) 0.0516(17) 0.0515(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' N N 0.0061 0.0033 '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 N4 Co1 N5 177.97(7) . . ? N4 Co1 N2 89.13(7) . . ? N5 Co1 N2 89.56(7) . . ? N4 Co1 N6 90.89(8) . . ? N5 Co1 N6 90.49(8) . . ? N2 Co1 N6 177.61(8) . . ? N4 Co1 N1 78.81(7) . . ? N5 Co1 N1 102.51(7) . . ? N2 Co1 N1 81.02(6) . . ? N6 Co1 N1 96.64(7) . . ? N4 Co1 N3 80.81(7) . . ? N5 Co1 N3 97.40(7) . . ? N2 Co1 N3 77.98(6) . . ? N6 Co1 N3 104.37(7) . . ? N1 Co1 N3 150.81(6) . . ? C22 N1 C9 109.36(17) . . ? C22 N1 C23 111.88(17) . . ? C9 N1 C23 111.42(17) . . ? C22 N1 Co1 98.13(13) . . ? C9 N1 Co1 102.28(12) . . ? C23 N1 Co1 122.47(13) . . ? C17 N4 C21 121.11(18) . . ? C17 N4 Co1 120.83(15) . . ? C21 N4 Co1 118.06(14) . . ? C10 N2 C14 121.07(17) . . ? C10 N2 Co1 120.06(14) . . ? C14 N2 Co1 118.80(13) . . ? C15 N3 C16 109.09(17) . . ? C15 N3 C27 112.07(17) . . ? C16 N3 C27 112.80(18) . . ? C15 N3 Co1 99.13(13) . . ? C16 N3 Co1 102.23(13) . . ? C27 N3 Co1 120.19(12) . . ? C12 C11 C10 119.3(2) . . ? C12 C11 H11 125.7(14) . . ? C10 C11 H11 114.9(14) . . ? C5 N6 Co1 171.4(2) . . ? C1 N5 Co1 174.54(18) . . ? N2 C10 C11 120.1(2) . . ? N2 C10 C9 116.56(17) . . ? C11 C10 C9 123.1(2) . . ? N4 C21 C20 120.4(2) . . ? N4 C21 C22 115.89(18) . . ? C20 C21 C22 123.7(2) . . ? N1 C23 C25 109.6(2) . . ? N1 C23 C24 112.6(2) . . ? C25 C23 C24 109.6(3) . . ? N1 C23 C26 108.3(2) . . ? C25 C23 C26 108.0(2) . . ? C24 C23 C26 108.8(2) . . ? C28 C27 N3 109.6(2) . . ? C28 C27 C29 109.6(3) . . ? N3 C27 C29 111.8(2) . . ? C28 C27 C30 108.5(2) . . ? N3 C27 C30 108.0(2) . . ? C29 C27 C30 109.3(3) . . ? N1 C9 C10 114.02(17) . . ? N1 C9 H9A 109.3(13) . . ? C10 C9 H9A 107.3(13) . . ? N1 C9 H9B 112.0(14) . . ? C10 C9 H9B 109.3(14) . . ? H9A C9 H9B 104.3(19) . . ? N3 C15 C14 110.78(18) . . ? N3 C15 H15B 109.9(12) . . ? C14 C15 H15B 108.0(13) . . ? N3 C15 H15A 110.3(13) . . ? C14 C15 H15A 108.5(13) . . ? H15B C15 H15A 109.3(18) . . ? N2 C14 C13 120.1(2) . . ? N2 C14 C15 116.00(18) . . ? C13 C14 C15 123.9(2) . . ? C12 C13 C14 119.3(2) . . ? C12 C13 H13 123.1(14) . . ? C14 C13 H13 117.6(14) . . ? N4 C17 C18 120.0(2) . . ? N4 C17 C16 116.49(18) . . ? C18 C17 C16 123.2(2) . . ? N6 C5 C6 179.5(3) . . ? C27 C28 H28B 107.8(16) . . ? C27 C28 H28A 110.3(15) . . ? H28B C28 H28A 107(2) . . ? C27 C28 H28C 111.4(19) . . ? H28B C28 H28C 107(2) . . ? H28A C28 H28C 113(3) . . ? C20 C19 C18 119.8(2) . . ? C20 C19 H19 120.6(17) . . ? C18 C19 H19 119.3(17) . . ? C21 C20 C19 119.2(3) . . ? C21 C20 H20 118.4(15) . . ? C19 C20 H20 122.4(15) . . ? C23 C26 H26B 111.3(16) . . ? C23 C26 H26A 113.1(16) . . ? H26B C26 H26A 105(2) . . ? C23 C26 H26C 108.2(15) . . ? H26B C26 H26C 113(2) . . ? H26A C26 H26C 106(2) . . ? C5 C6 C8 119.6(2) . . ? C5 C6 C7 118.7(2) . . ? C8 C6 C7 121.5(2) . . ? N1 C22 C21 110.89(18) . . ? N1 C22 H22A 112.0(12) . . ? C21 C22 H22A 108.0(12) . . ? N1 C22 H22B 112.6(12) . . ? C21 C22 H22B 105.0(13) . . ? H22A C22 H22B 107.9(18) . . ? N3 C16 C17 114.62(18) . . ? N3 C16 H16A 113.4(14) . . ? C17 C16 H16A 108.5(14) . . ? N3 C16 H16B 109.4(14) . . ? C17 C16 H16B 106.2(14) . . ? H16A C16 H16B 104(2) . . ? N9 C7 C6 179.2(3) . . ? C11 C12 C13 120.0(2) . . ? C11 C12 H12 121.3(17) . . ? C13 C12 H12 118.5(17) . . ? C23 C24 H24A 113.0(17) . . ? C23 C24 H24B 108(2) . . ? H24A C24 H24B 110(3) . . ? C23 C24 H24C 110.0(17) . . ? H24A C24 H24C 111(2) . . ? H24B C24 H24C 104(2) . . ? C19 C18 C17 119.3(3) . . ? C19 C18 H18 126.1(15) . . ? C17 C18 H18 114.6(16) . . ? C23 C25 H25B 110.8(17) . . ? C23 C25 H25A 112.2(15) . . ? H25B C25 H25A 107(2) . . ? C23 C25 H25C 110(2) . . ? H25B C25 H25C 106(2) . . ? H25A C25 H25C 110(2) . . ? C27 C29 H29A 112.1(15) . . ? C27 C29 H29B 108.9(19) . . ? H29A C29 H29B 105(2) . . ? C27 C29 H29C 108.4(18) . . ? H29A C29 H29C 113(2) . . ? H29B C29 H29C 110(3) . . ? C27 C30 H30A 112.0(16) . . ? C27 C30 H30B 105.8(17) . . ? H30A C30 H30B 106(2) . . ? C27 C30 H30C 115.2(16) . . ? H30A C30 H30C 106(2) . . ? H30B C30 H30C 111(2) . . ? N10 C8 C6 179.5(3) . . ? C1 C2 C3 118.4(2) . . ? C1 C2 C4 120.48(19) . . ? C3 C2 C4 120.79(19) . . ? N5 C1 C2 177.4(2) . . ? N8 C4 C2 178.5(3) . . ? N7 C3 C2 177.9(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 N4 1.9186(16) . ? Co1 N5 1.9220(19) . ? Co1 N2 1.9259(16) . ? Co1 N6 1.938(2) . ? Co1 N1 2.3248(17) . ? Co1 N3 2.3350(18) . ? N9 C7 1.157(3) . ? N1 C22 1.479(3) . ? N1 C9 1.492(3) . ? N1 C23 1.520(3) . ? N4 C17 1.338(3) . ? N4 C21 1.348(3) . ? N2 C10 1.342(3) . ? N2 C14 1.345(3) . ? N3 C15 1.480(3) . ? N3 C16 1.485(3) . ? N3 C27 1.522(3) . ? C11 C12 1.370(3) . ? C11 C10 1.381(3) . ? C11 H11 0.92(2) . ? N6 C5 1.141(3) . ? N5 C1 1.145(3) . ? C10 C9 1.497(3) . ? C21 C20 1.372(3) . ? C21 C22 1.499(3) . ? C23 C25 1.527(4) . ? C23 C24 1.529(4) . ? C23 C26 1.537(4) . ? C27 C28 1.518(4) . ? C27 C29 1.531(4) . ? C27 C30 1.535(4) . ? C9 H9A 0.90(2) . ? C9 H9B 0.95(3) . ? C15 C14 1.504(3) . ? C15 H15B 1.00(2) . ? C15 H15A 1.04(2) . ? C14 C13 1.379(3) . ? C13 C12 1.372(4) . ? C13 H13 0.94(2) . ? C17 C18 1.381(3) . ? C17 C16 1.502(3) . ? C5 C6 1.392(3) . ? C28 H28B 1.02(3) . ? C28 H28A 0.99(3) . ? C28 H28C 0.97(3) . ? C19 C20 1.374(4) . ? C19 C18 1.376(4) . ? C19 H19 0.99(3) . ? C20 H20 0.92(2) . ? C26 H26B 0.96(3) . ? C26 H26A 1.00(3) . ? C26 H26C 1.01(3) . ? C6 C8 1.410(4) . ? C6 C7 1.411(4) . ? C22 H22A 0.98(2) . ? C22 H22B 1.01(2) . ? C16 H16A 0.95(3) . ? C16 H16B 0.97(2) . ? C12 H12 0.88(2) . ? C24 H24A 0.93(3) . ? C24 H24B 0.97(3) . ? C24 H24C 1.09(3) . ? C18 H18 0.91(2) . ? C25 H25B 0.99(3) . ? C25 H25A 1.03(3) . ? C25 H25C 0.94(3) . ? N10 C8 1.144(4) . ? C29 H29A 1.03(3) . ? C29 H29B 0.95(3) . ? C29 H29C 1.00(3) . ? C30 H30A 1.03(3) . ? C30 H30B 0.93(3) . ? C30 H30C 0.96(3) . ? C2 C1 1.393(3) . ? C2 C3 1.399(3) . ? C2 C4 1.405(3) . ? C4 N8 1.137(3) . ? C3 N7 1.149(3) . ? 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 C14 N2 C10 C11 6.0(3) . . . . ? Co1 N2 C10 C11 -170.81(15) . . . . ? C14 N2 C10 C9 -168.61(18) . . . . ? Co1 N2 C10 C9 14.6(2) . . . . ? C12 C11 C10 N2 -4.7(3) . . . . ? C12 C11 C10 C9 169.6(2) . . . . ? C17 N4 C21 C20 -3.5(3) . . . . ? Co1 N4 C21 C20 176.92(17) . . . . ? C17 N4 C21 C22 175.85(19) . . . . ? Co1 N4 C21 C22 -3.7(2) . . . . ? C22 N1 C23 C25 -68.7(3) . . . . ? C9 N1 C23 C25 168.6(2) . . . . ? Co1 N1 C23 C25 47.2(2) . . . . ? C22 N1 C23 C24 53.5(3) . . . . ? C9 N1 C23 C24 -69.2(3) . . . . ? Co1 N1 C23 C24 169.4(2) . . . . ? C22 N1 C23 C26 173.8(2) . . . . ? C9 N1 C23 C26 51.1(2) . . . . ? Co1 N1 C23 C26 -70.3(2) . . . . ? C15 N3 C27 C28 -67.4(3) . . . . ? C16 N3 C27 C28 169.0(2) . . . . ? Co1 N3 C27 C28 48.3(3) . . . . ? C15 N3 C27 C29 54.3(3) . . . . ? C16 N3 C27 C29 -69.3(3) . . . . ? Co1 N3 C27 C29 170.0(2) . . . . ? C15 N3 C27 C30 174.5(2) . . . . ? C16 N3 C27 C30 51.0(3) . . . . ? Co1 N3 C27 C30 -69.7(2) . . . . ? C22 N1 C9 C10 127.42(19) . . . . ? C23 N1 C9 C10 -108.4(2) . . . . ? Co1 N1 C9 C10 24.13(19) . . . . ? N2 C10 C9 N1 -27.8(3) . . . . ? C11 C10 C9 N1 157.73(19) . . . . ? C16 N3 C15 C14 -66.4(2) . . . . ? C27 N3 C15 C14 167.98(18) . . . . ? Co1 N3 C15 C14 40.05(19) . . . . ? C10 N2 C14 C13 -3.1(3) . . . . ? Co1 N2 C14 C13 173.72(16) . . . . ? C10 N2 C14 C15 176.68(18) . . . . ? Co1 N2 C14 C15 -6.5(2) . . . . ? N3 C15 C14 N2 -28.3(3) . . . . ? N3 C15 C14 C13 151.5(2) . . . . ? N2 C14 C13 C12 -1.0(3) . . . . ? C15 C14 C13 C12 179.2(2) . . . . ? C21 N4 C17 C18 5.5(3) . . . . ? Co1 N4 C17 C18 -174.92(16) . . . . ? C21 N4 C17 C16 -168.24(19) . . . . ? Co1 N4 C17 C16 11.3(2) . . . . ? N4 C21 C20 C19 -0.8(4) . . . . ? C22 C21 C20 C19 179.9(2) . . . . ? C18 C19 C20 C21 3.0(4) . . . . ? C9 N1 C22 C21 -64.5(2) . . . . ? C23 N1 C22 C21 171.60(18) . . . . ? Co1 N1 C22 C21 41.67(19) . . . . ? N4 C21 C22 N1 -31.3(3) . . . . ? C20 C21 C22 N1 148.0(2) . . . . ? C15 N3 C16 C17 126.8(2) . . . . ? C27 N3 C16 C17 -108.0(2) . . . . ? Co1 N3 C16 C17 22.5(2) . . . . ? N4 C17 C16 N3 -24.7(3) . . . . ? C18 C17 C16 N3 161.8(2) . . . . ? C10 C11 C12 C13 0.6(3) . . . . ? C14 C13 C12 C11 2.2(4) . . . . ? C20 C19 C18 C17 -1.0(4) . . . . ? N4 C17 C18 C19 -3.2(3) . . . . ? C16 C17 C18 C19 170.1(2) . . . . ?