#------------------------------------------------------------------------------ #$Date: 2020-10-06 11:51:45 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257541 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705240.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_7705240 loop_ _publ_author_name 'Melle, Philipp' 'S\'egaud, Nathalie' 'Albrecht, Martin' _publ_section_title ; Ambidentate bonding and electrochemical implications of pincer-type pyridylidene amide ligands in complexes of nickel, cobalt and zinc. ; _journal_issue 36 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 12662 _journal_page_last 12673 _journal_paper_doi 10.1039/d0dt02482a _journal_volume 49 _journal_year 2020 _chemical_formula_moiety 'C19 H17 Cl2 Co N5 O2' _chemical_formula_sum 'C19 H17 Cl2 Co N5 O2' _chemical_formula_weight 477.20 _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 geom _atom_sites_solution_primary dual _audit_creation_date 2019-03-03 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-07-13 deposited with the CCDC. 2020-08-21 downloaded from the CCDC. ; _cell_angle_alpha 102.016(2) _cell_angle_beta 99.280(2) _cell_angle_gamma 104.188(2) _cell_formula_units_Z 2 _cell_length_a 7.9978(2) _cell_length_b 9.2730(2) _cell_length_c 14.4181(4) _cell_measurement_reflns_used 5682 _cell_measurement_temperature 173.00(10) _cell_measurement_theta_max 27.0170 _cell_measurement_theta_min 2.3290 _cell_volume 988.23(5) _computing_cell_refinement 'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 173.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0965 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.929 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -10.00 103.00 1.00 27.50 -- 27.42 57.00 0.00 113 2 \w -16.00 112.00 1.00 27.50 -- 27.42 77.00 -90.00 128 3 \w -16.00 112.00 1.00 27.50 -- 27.42 77.00 30.00 128 4 \w -10.00 103.00 1.00 27.50 -- 27.42 57.00-180.00 113 5 \w 35.00 122.00 1.00 27.50 -- 27.42 178.00 -90.00 87 6 \w 35.00 122.00 1.00 27.50 -- 27.42 178.00-180.00 87 7 \w -108.00 -55.00 1.00 27.50 -- -23.50-153.00-144.00 53 8 \w -54.00 83.00 1.00 27.50 -- 27.42 -38.00 30.00 137 9 \w 35.00 122.00 1.00 27.50 -- 27.42 178.00 -30.00 87 10 \w -16.00 63.00 1.00 27.50 -- 27.42 77.00 120.00 79 11 \w -49.00 65.00 1.00 27.50 -- 27.42 -57.00 -90.00 114 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0587525000 _diffrn_orient_matrix_UB_12 0.0269970000 _diffrn_orient_matrix_UB_13 -0.0287144000 _diffrn_orient_matrix_UB_21 -0.0685854000 _diffrn_orient_matrix_UB_22 -0.0347918000 _diffrn_orient_matrix_UB_23 -0.0425092000 _diffrn_orient_matrix_UB_31 -0.0255688000 _diffrn_orient_matrix_UB_32 0.0687950000 _diffrn_orient_matrix_UB_33 0.0056342000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_unetI/netI 0.0376 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.929 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 16903 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.929 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.103 _diffrn_reflns_theta_min 2.345 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.165 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.78321 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light blue' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary blue _exptl_crystal_density_diffrn 1.604 _exptl_crystal_description prism _exptl_crystal_F_000 486 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.324 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.061 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 264 _refine_ls_number_reflns 4480 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.033 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0333 _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^)+(0.0303P)^2^+0.3672P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.0776 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3596 _reflns_number_total 4480 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02482a2.cif _cod_data_source_block 19ma035_PM305 _cod_depositor_comments 'Adding full bibliography for 7705237--7705245.cif.' _cod_original_cell_volume 988.23(4) _cod_database_code 7705240 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula C19H17Cl2Co1N5O2 _chemical_oxdiff_usercomment PM305 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.944 _shelx_estimated_absorpt_t_min 0.845 _reflns_odcompleteness_completeness 99.98 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, {H22A,H22B,H22C} of C22 At 1.5 times of: {H29A,H29B,H29C} of C29 2.a Aromatic/amide H refined with riding coordinates: C6(H6), C8(H8), C17(H17), C24(H24), C7(H7), C27(H27), C18(H18), C25(H25), C20(H20), C19(H19), C26(H26) 2.b Idealised Me refined as rotating group: C29(H29A,H29B,H29C), C22(H22A,H22B,H22C) ; _shelx_res_file ; 19ma035_c2.res created by SHELXL-2014/7 TITL 19ma035_c2_a.res in P-1 REM Old TITL 19MA035_C2 in P-1 REM SHELXT solution in P-1 REM R1 0.092, Rweak 0.005, Alpha 0.025, Orientation as input REM Formula found by SHELXT: C19 N5 O2 Cl2 Co CELL 0.71073 7.9978 9.273 14.4181 102.016 99.28 104.188 ZERR 2 0.0002 0.0002 0.0004 0.002 0.002 0.002 LATT 1 SFAC C H Cl Co N O UNIT 38 34 4 2 10 4 L.S. 40 PLAN 5 SIZE 0.15 0.1 0.05 BOND $H LIST 6 fmap 2 acta REM REM REM WGHT 0.030300 0.367200 FVAR 0.42151 CO1 4 0.230934 0.261035 0.256120 11.00000 0.02628 0.02730 = 0.02579 0.00895 0.00273 0.00273 CL2 3 0.157282 0.031714 0.144442 11.00000 0.03483 0.02890 = 0.02771 0.00773 0.00014 -0.00067 CL3 3 0.016863 0.365168 0.294229 11.00000 0.03116 0.03986 = 0.03664 0.00902 0.00497 0.01050 O14 6 0.291003 0.178724 0.388568 11.00000 0.03076 0.03136 = 0.02380 0.01165 0.00026 0.00417 O11 6 0.306318 0.407470 0.157365 11.00000 0.03198 0.02861 = 0.02472 0.01049 0.00115 -0.00240 N4 5 0.480433 0.390925 0.322358 11.00000 0.02745 0.02387 = 0.02058 0.00767 0.00624 0.00771 N15 5 0.519521 0.235564 0.526742 11.00000 0.02988 0.02860 = 0.02232 0.01148 0.00415 0.00981 N21 5 0.545173 0.125457 0.653884 11.00000 0.03203 0.02513 = 0.02298 0.00884 0.00357 0.00894 N28 5 0.548157 0.746166 0.034026 11.00000 0.03169 0.02472 = 0.02402 0.00729 0.00664 0.00073 N12 5 0.533103 0.618864 0.153835 11.00000 0.02983 0.02688 = 0.02432 0.01031 0.00748 0.00319 C9 1 0.555803 0.375256 0.408186 11.00000 0.02886 0.02520 = 0.02203 0.00755 0.00605 0.01252 C23 1 0.442534 0.657856 0.079790 11.00000 0.03264 0.02166 = 0.02267 0.00639 0.00757 0.00203 C13 1 0.440853 0.251402 0.442233 11.00000 0.03194 0.02476 = 0.02320 0.00791 0.00764 0.01255 C5 1 0.564855 0.498769 0.283083 11.00000 0.02760 0.02297 = 0.02309 0.00645 0.00919 0.00788 C16 1 0.436490 0.136438 0.572836 11.00000 0.03369 0.02484 = 0.02181 0.00665 0.00503 0.01295 C10 1 0.454729 0.505619 0.189707 11.00000 0.03122 0.02419 = 0.02199 0.00668 0.00874 0.00769 C6 1 0.733191 0.592958 0.328324 11.00000 0.02723 0.02745 = 0.03025 0.00852 0.00969 0.00628 AFIX 43 H6 2 0.792633 0.665073 0.299753 11.00000 -1.20000 AFIX 0 C8 1 0.722726 0.468865 0.458309 11.00000 0.02788 0.03116 = 0.02425 0.00717 0.00307 0.01108 AFIX 43 H8 2 0.773852 0.458647 0.518365 11.00000 -1.20000 AFIX 0 C17 1 0.258161 0.048774 0.552346 11.00000 0.03442 0.03302 = 0.02782 0.01125 0.00339 0.01231 AFIX 43 H17 2 0.180286 0.052483 0.498125 11.00000 -1.20000 AFIX 0 C24 1 0.258923 0.629756 0.049498 11.00000 0.03275 0.03290 = 0.03497 0.01665 0.00787 0.00263 AFIX 43 H24 2 0.183261 0.570593 0.078965 11.00000 -1.20000 AFIX 0 C7 1 0.811634 0.577602 0.417329 11.00000 0.02438 0.03190 = 0.03260 0.00450 0.00352 0.00650 AFIX 43 H7 2 0.924444 0.640729 0.449498 11.00000 -1.20000 AFIX 0 C27 1 0.478744 0.801643 -0.038460 11.00000 0.04578 0.02910 = 0.02858 0.01416 0.00919 0.00128 AFIX 43 H27 2 0.554390 0.859612 -0.068515 11.00000 -1.20000 AFIX 0 C18 1 0.196665 -0.041922 0.610473 11.00000 0.03411 0.03269 = 0.03514 0.01115 0.00796 0.00818 AFIX 43 H18 2 0.077989 -0.098209 0.596081 11.00000 -1.20000 AFIX 0 C29 1 0.741364 0.785233 0.065395 11.00000 0.03060 0.04148 = 0.03160 0.01397 0.00945 -0.00090 AFIX 137 H29A 2 0.778469 0.846314 0.131619 11.00000 -1.50000 H29B 2 0.795950 0.842569 0.024460 11.00000 -1.50000 H29C 2 0.776007 0.692362 0.060619 11.00000 -1.50000 AFIX 0 C25 1 0.189395 0.687753 -0.022485 11.00000 0.03374 0.03916 = 0.04282 0.01571 0.00135 0.00384 AFIX 43 H25 2 0.067616 0.669425 -0.041013 11.00000 -1.20000 AFIX 0 C20 1 0.484341 0.034897 0.711018 11.00000 0.04637 0.03078 = 0.02406 0.01331 0.00429 0.01298 AFIX 43 H20 2 0.562287 0.030623 0.765023 11.00000 -1.20000 AFIX 0 C22 1 0.733908 0.214388 0.679904 11.00000 0.03411 0.03674 = 0.03096 0.01402 -0.00059 0.00769 AFIX 137 H22A 2 0.786210 0.191247 0.625262 11.00000 -1.20000 H22B 2 0.793871 0.187309 0.734013 11.00000 -1.20000 H22C 2 0.744425 0.322463 0.697364 11.00000 -1.20000 AFIX 0 C19 1 0.312678 -0.049458 0.691226 11.00000 0.04453 0.03347 = 0.02844 0.01533 0.00901 0.00941 AFIX 43 H19 2 0.272888 -0.111425 0.730914 11.00000 -1.20000 AFIX 0 C26 1 0.301957 0.774504 -0.067975 11.00000 0.04390 0.04107 = 0.03064 0.01830 0.00021 0.00506 AFIX 43 H26 2 0.256264 0.813117 -0.117823 11.00000 -1.20000 AFIX 0 HKLF 4 REM 19ma035_c2_a.res in P-1 REM R1 = 0.0333 for 3596 Fo > 4sig(Fo) and 0.0486 for all 4480 data REM 264 parameters refined using 0 restraints END WGHT 0.0301 0.3746 REM Highest difference peak 0.324, deepest hole -0.294, 1-sigma level 0.061 Q1 1 0.5059 0.4965 0.2395 11.00000 0.05 0.32 Q2 1 0.3492 0.6755 0.0778 11.00000 0.05 0.30 Q3 1 0.3893 0.3363 0.2961 11.00000 0.05 0.30 Q4 1 0.1078 0.3172 0.2599 11.00000 0.05 0.29 Q5 1 0.1623 0.2688 0.3137 11.00000 0.05 0.28 ; _shelx_res_checksum 74595 _olex2_date_sample_data_collection 2019-03-01 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.647 _oxdiff_exptl_absorpt_empirical_full_min 0.750 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 0.23093(4) 0.26103(3) 0.25612(2) 0.02743(9) Uani 1 1 d . . . . . Cl2 Cl 0.15728(7) 0.03171(6) 0.14444(4) 0.03306(13) Uani 1 1 d . . . . . Cl3 Cl 0.01686(7) 0.36517(6) 0.29423(4) 0.03629(14) Uani 1 1 d . . . . . O14 O 0.29100(19) 0.17872(16) 0.38857(10) 0.0295(3) Uani 1 1 d . . . . . O11 O 0.30632(19) 0.40747(16) 0.15737(10) 0.0306(3) Uani 1 1 d . . . . . N4 N 0.4804(2) 0.39093(18) 0.32236(12) 0.0235(4) Uani 1 1 d . . . . . N15 N 0.5195(2) 0.23556(19) 0.52674(12) 0.0261(4) Uani 1 1 d . . . . . N21 N 0.5452(2) 0.12546(18) 0.65388(12) 0.0265(4) Uani 1 1 d . . . . . N28 N 0.5482(2) 0.74617(19) 0.03403(12) 0.0280(4) Uani 1 1 d . . . . . N12 N 0.5331(2) 0.61886(19) 0.15383(12) 0.0272(4) Uani 1 1 d . . . . . C9 C 0.5558(3) 0.3753(2) 0.40819(14) 0.0242(4) Uani 1 1 d . . . . . C23 C 0.4425(3) 0.6579(2) 0.07979(15) 0.0265(4) Uani 1 1 d . . . . . C13 C 0.4409(3) 0.2514(2) 0.44223(15) 0.0254(4) Uani 1 1 d . . . . . C5 C 0.5649(3) 0.4988(2) 0.28308(14) 0.0240(4) Uani 1 1 d . . . . . C16 C 0.4365(3) 0.1364(2) 0.57284(14) 0.0260(4) Uani 1 1 d . . . . . C10 C 0.4547(3) 0.5056(2) 0.18971(15) 0.0254(4) Uani 1 1 d . . . . . C6 C 0.7332(3) 0.5930(2) 0.32832(15) 0.0281(4) Uani 1 1 d . . . . . H6 H 0.7926 0.6651 0.2998 0.034 Uiso 1 1 calc R . . . . C8 C 0.7227(3) 0.4689(2) 0.45831(15) 0.0276(4) Uani 1 1 d . . . . . H8 H 0.7739 0.4586 0.5184 0.033 Uiso 1 1 calc R . . . . C17 C 0.2582(3) 0.0488(2) 0.55235(16) 0.0312(5) Uani 1 1 d . . . . . H17 H 0.1803 0.0525 0.4981 0.037 Uiso 1 1 calc R . . . . C24 C 0.2589(3) 0.6298(2) 0.04950(16) 0.0335(5) Uani 1 1 d . . . . . H24 H 0.1833 0.5706 0.0790 0.040 Uiso 1 1 calc R . . . . C7 C 0.8116(3) 0.5776(2) 0.41733(16) 0.0309(5) Uani 1 1 d . . . . . H7 H 0.9244 0.6407 0.4495 0.037 Uiso 1 1 calc R . . . . C27 C 0.4787(3) 0.8016(2) -0.03846(16) 0.0351(5) Uani 1 1 d . . . . . H27 H 0.5544 0.8596 -0.0685 0.042 Uiso 1 1 calc R . . . . C18 C 0.1967(3) -0.0419(2) 0.61047(16) 0.0339(5) Uani 1 1 d . . . . . H18 H 0.0780 -0.0982 0.5961 0.041 Uiso 1 1 calc R . . . . C29 C 0.7414(3) 0.7852(3) 0.06540(17) 0.0356(5) Uani 1 1 d . . . . . H29A H 0.7785 0.8463 0.1316 0.053 Uiso 1 1 calc GR . . . . H29B H 0.7960 0.8426 0.0245 0.053 Uiso 1 1 calc GR . . . . H29C H 0.7760 0.6924 0.0606 0.053 Uiso 1 1 calc GR . . . . C25 C 0.1894(3) 0.6878(3) -0.02249(18) 0.0399(6) Uani 1 1 d . . . . . H25 H 0.0676 0.6694 -0.0410 0.048 Uiso 1 1 calc R . . . . C20 C 0.4843(3) 0.0349(2) 0.71102(16) 0.0329(5) Uani 1 1 d . . . . . H20 H 0.5623 0.0306 0.7650 0.039 Uiso 1 1 calc R . . . . C22 C 0.7339(3) 0.2144(3) 0.67990(16) 0.0345(5) Uani 1 1 d . . . . . H22A H 0.7862 0.1912 0.6253 0.041 Uiso 1 1 calc GR . . . . H22B H 0.7939 0.1873 0.7340 0.041 Uiso 1 1 calc GR . . . . H22C H 0.7444 0.3225 0.6974 0.041 Uiso 1 1 calc GR . . . . C19 C 0.3127(3) -0.0495(2) 0.69123(16) 0.0346(5) Uani 1 1 d . . . . . H19 H 0.2729 -0.1114 0.7309 0.041 Uiso 1 1 calc R . . . . C26 C 0.3020(3) 0.7745(3) -0.06797(17) 0.0394(6) Uani 1 1 d . . . . . H26 H 0.2563 0.8131 -0.1178 0.047 Uiso 1 1 calc R . . . . 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 0.02628(16) 0.02730(16) 0.02579(16) 0.00895(12) 0.00273(12) 0.00273(12) Cl2 0.0348(3) 0.0289(3) 0.0277(3) 0.0077(2) 0.0001(2) -0.0007(2) Cl3 0.0312(3) 0.0399(3) 0.0366(3) 0.0090(2) 0.0050(2) 0.0105(2) O14 0.0308(8) 0.0314(8) 0.0238(8) 0.0116(6) 0.0003(6) 0.0042(6) O11 0.0320(8) 0.0286(7) 0.0247(8) 0.0105(6) 0.0012(6) -0.0024(6) N4 0.0275(9) 0.0239(8) 0.0206(8) 0.0077(7) 0.0062(7) 0.0077(7) N15 0.0299(9) 0.0286(9) 0.0223(9) 0.0115(7) 0.0041(7) 0.0098(7) N21 0.0320(10) 0.0251(9) 0.0230(9) 0.0088(7) 0.0036(7) 0.0089(7) N28 0.0317(10) 0.0247(9) 0.0240(9) 0.0073(7) 0.0066(8) 0.0007(7) N12 0.0298(9) 0.0269(9) 0.0243(9) 0.0103(7) 0.0075(7) 0.0032(7) C9 0.0289(11) 0.0252(10) 0.0220(10) 0.0075(8) 0.0060(8) 0.0125(8) C23 0.0326(11) 0.0217(10) 0.0227(10) 0.0064(8) 0.0076(9) 0.0020(8) C13 0.0319(11) 0.0248(10) 0.0232(10) 0.0079(8) 0.0076(9) 0.0126(9) C5 0.0276(10) 0.0230(10) 0.0231(10) 0.0064(8) 0.0092(8) 0.0079(8) C16 0.0337(11) 0.0248(10) 0.0218(10) 0.0067(8) 0.0050(9) 0.0130(9) C10 0.0312(11) 0.0242(10) 0.0220(10) 0.0067(8) 0.0087(9) 0.0077(9) C6 0.0272(11) 0.0275(10) 0.0302(11) 0.0085(9) 0.0097(9) 0.0063(9) C8 0.0279(11) 0.0312(11) 0.0243(11) 0.0072(9) 0.0031(9) 0.0111(9) C17 0.0344(12) 0.0330(11) 0.0278(12) 0.0112(9) 0.0034(9) 0.0123(10) C24 0.0328(12) 0.0329(12) 0.0350(13) 0.0166(10) 0.0079(10) 0.0026(9) C7 0.0244(11) 0.0319(11) 0.0326(12) 0.0045(10) 0.0035(9) 0.0065(9) C27 0.0458(14) 0.0291(11) 0.0286(12) 0.0142(10) 0.0092(10) 0.0013(10) C18 0.0341(12) 0.0327(11) 0.0351(13) 0.0111(10) 0.0080(10) 0.0082(10) C29 0.0306(12) 0.0415(13) 0.0316(12) 0.0140(10) 0.0095(10) -0.0009(10) C25 0.0337(13) 0.0392(13) 0.0428(14) 0.0157(11) 0.0013(11) 0.0038(10) C20 0.0464(14) 0.0308(11) 0.0241(11) 0.0133(9) 0.0043(10) 0.0130(10) C22 0.0341(12) 0.0367(12) 0.0310(12) 0.0140(10) -0.0006(10) 0.0077(10) C19 0.0445(14) 0.0335(12) 0.0284(12) 0.0153(10) 0.0090(10) 0.0094(10) C26 0.0439(14) 0.0411(13) 0.0306(13) 0.0183(11) 0.0002(11) 0.0051(11) 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' Cl Cl 0.1484 0.1585 '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 Cl3 Co1 Cl2 119.54(2) . . ? O14 Co1 Cl2 97.98(4) . . ? O14 Co1 Cl3 98.69(4) . . ? O11 Co1 Cl2 96.80(4) . . ? O11 Co1 Cl3 94.51(4) . . ? O11 Co1 O14 151.97(5) . . ? N4 Co1 Cl2 125.11(5) . . ? N4 Co1 Cl3 115.28(5) . . ? N4 Co1 O14 76.10(6) . . ? N4 Co1 O11 75.91(6) . . ? C13 O14 Co1 113.40(13) . . ? C10 O11 Co1 113.85(12) . . ? C9 N4 Co1 119.49(13) . . ? C9 N4 C5 120.66(18) . . ? C5 N4 Co1 119.72(13) . . ? C13 N15 C16 122.29(18) . . ? C16 N21 C22 119.43(17) . . ? C20 N21 C16 122.02(18) . . ? C20 N21 C22 118.54(17) . . ? C23 N28 C29 119.54(17) . . ? C27 N28 C23 121.69(18) . . ? C27 N28 C29 118.75(18) . . ? C10 N12 C23 121.00(18) . . ? N4 C9 C13 113.48(17) . . ? N4 C9 C8 120.96(18) . . ? C8 C9 C13 125.55(18) . . ? N28 C23 C24 116.98(18) . . ? N12 C23 N28 114.09(18) . . ? N12 C23 C24 128.74(19) . . ? O14 C13 N15 130.02(19) . . ? O14 C13 C9 117.42(17) . . ? N15 C13 C9 112.56(17) . . ? N4 C5 C10 112.97(17) . . ? N4 C5 C6 121.11(19) . . ? C6 C5 C10 125.90(18) . . ? N15 C16 N21 113.50(18) . . ? N15 C16 C17 130.01(19) . . ? N21 C16 C17 116.46(18) . . ? O11 C10 N12 129.52(19) . . ? O11 C10 C5 117.24(17) . . ? N12 C10 C5 113.24(18) . . ? C5 C6 H6 120.8 . . ? C5 C6 C7 118.46(19) . . ? C7 C6 H6 120.8 . . ? C9 C8 H8 120.7 . . ? C7 C8 C9 118.64(19) . . ? C7 C8 H8 120.7 . . ? C16 C17 H17 119.3 . . ? C18 C17 C16 121.5(2) . . ? C18 C17 H17 119.3 . . ? C23 C24 H24 119.4 . . ? C25 C24 C23 121.2(2) . . ? C25 C24 H24 119.4 . . ? C6 C7 H7 119.9 . . ? C8 C7 C6 120.14(19) . . ? C8 C7 H7 119.9 . . ? N28 C27 H27 119.3 . . ? C26 C27 N28 121.5(2) . . ? C26 C27 H27 119.3 . . ? C17 C18 H18 120.2 . . ? C17 C18 C19 119.7(2) . . ? C19 C18 H18 120.2 . . ? N28 C29 H29A 109.5 . . ? N28 C29 H29B 109.5 . . ? N28 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C24 C25 H25 120.2 . . ? C24 C25 C26 119.7(2) . . ? C26 C25 H25 120.2 . . ? N21 C20 H20 119.3 . . ? C19 C20 N21 121.5(2) . . ? C19 C20 H20 119.3 . . ? N21 C22 H22A 109.5 . . ? N21 C22 H22B 109.5 . . ? N21 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C19 H19 120.5 . . ? C20 C19 C18 118.9(2) . . ? C20 C19 H19 120.5 . . ? C27 C26 C25 118.9(2) . . ? C27 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? 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 Cl2 2.2619(6) . ? Co1 Cl3 2.2491(6) . ? Co1 O14 2.2250(14) . ? Co1 O11 2.2171(14) . ? Co1 N4 2.0181(16) . ? O14 C13 1.256(2) . ? O11 C10 1.253(2) . ? N4 C9 1.339(2) . ? N4 C5 1.343(2) . ? N15 C13 1.332(2) . ? N15 C16 1.351(3) . ? N21 C16 1.377(2) . ? N21 C20 1.356(3) . ? N21 C22 1.476(3) . ? N28 C23 1.373(2) . ? N28 C27 1.357(3) . ? N28 C29 1.468(3) . ? N12 C23 1.355(3) . ? N12 C10 1.331(3) . ? C9 C13 1.506(3) . ? C9 C8 1.385(3) . ? C23 C24 1.405(3) . ? C5 C10 1.508(3) . ? C5 C6 1.380(3) . ? C16 C17 1.406(3) . ? C6 H6 0.9300 . ? C6 C7 1.386(3) . ? C8 H8 0.9300 . ? C8 C7 1.380(3) . ? C17 H17 0.9300 . ? C17 C18 1.369(3) . ? C24 H24 0.9300 . ? C24 C25 1.367(3) . ? C7 H7 0.9300 . ? C27 H27 0.9300 . ? C27 C26 1.353(3) . ? C18 H18 0.9300 . ? C18 C19 1.392(3) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C25 H25 0.9300 . ? C25 C26 1.394(3) . ? C20 H20 0.9300 . ? C20 C19 1.354(3) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C19 H19 0.9300 . ? C26 H26 0.9300 . ?