#------------------------------------------------------------------------------ #$Date: 2021-11-06 22:15:38 +0200 (Sat, 06 Nov 2021) $ #$Revision: 270463 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/47/1564740.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_1564740 loop_ _publ_author_name 'Duan, Xinde' 'Ren, Shuangshuang' 'Ge, Fayuan' 'Zhu, Xukun' 'Zhang, Mingdao' 'Zheng, Hegen' _publ_section_title ; MOF-derived CoNi,CoO,NiO@N-C bifunctional oxygen electrocatalysts for liquid and all-solid-state Zn-air batteries. ; _journal_issue 41 _journal_name_full Nanoscale _journal_page_first 17655 _journal_page_last 17662 _journal_paper_doi 10.1039/d1nr04537g _journal_volume 13 _journal_year 2021 _chemical_formula_sum 'C50 H44 Co N4 O22' _chemical_formula_weight 1111.82 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-12-30 deposited with the CCDC. 2021-09-27 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.831(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 11.7612(6) _cell_length_b 13.5991(7) _cell_length_c 14.6943(7) _cell_measurement_reflns_used 9194 _cell_measurement_temperature 296.15 _cell_measurement_theta_max 27.51 _cell_measurement_theta_min 2.32 _cell_volume 2300.3(2) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.994 _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 0.0355 _diffrn_reflns_av_unetI/netI 0.0337 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 19744 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.547 _diffrn_reflns_theta_min 2.061 _exptl_absorpt_coefficient_mu 0.470 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6353 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0987 before and 0.0491 after correction. The Ratio of minimum to maximum transmission is 0.8521. The \l/2 correction factor is 0.00150. ; _exptl_crystal_density_diffrn 1.605 _exptl_crystal_description BLOCK _exptl_crystal_F_000 1150 _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.361 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.061 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 372 _refine_ls_number_reflns 5270 _refine_ls_number_restraints 8 _refine_ls_restrained_S_all 1.026 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0375 _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^)+(0.0394P)^2^+1.9545P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0876 _refine_ls_wR_factor_ref 0.0935 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4384 _reflns_number_total 5270 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1nr04537g2.cif _cod_data_source_block 1_a _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'MULTI-SCAN' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas Adding full bibliography for 1564740.cif. ; _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1564740 _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 0.896 _shelx_estimated_absorpt_t_max 0.955 _shelx_res_file ; TITL 1_a.res in P2(1)/n 1_a.res created by SHELXL-2018/3 at 21:12:25 on 18-Jun-2020 CELL 0.71073 11.7612 13.5991 14.6943 90 101.831 90 ZERR 2 0.0006 0.0007 0.0007 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Co N O UNIT 100 88 2 8 44 DFIX 0.85 0.01 O8 H8 DFIX 0.85 0.01 O2 H2 DFIX 0.85 0.01 O11 H11e DFIX 0.85 0.01 O7 H7 DFIX 0.85 0.01 H5 O5 DFIX 0.85 0.01 O11 H11d DFIX 0.85 0.01 O3 H3 DFIX 1.39 0.01 H11e H11d L.S. 10 PLAN 2 SIZE 0.24 0.16 0.1 TEMP 23 CONF BOND $H LIST 4 fmap 2 acta MORE -1 REM REM REM WGHT 0.039400 1.954500 FVAR 0.46169 CO1 3 0.500000 0.500000 0.000000 10.50000 0.01240 0.00928 = 0.01172 -0.00056 0.00342 -0.00134 O9 5 0.822850 0.046084 0.474709 11.00000 0.01276 0.01717 = 0.01862 0.00235 0.00349 0.00406 O1 5 0.476697 0.509122 0.139127 11.00000 0.02206 0.02188 = 0.01426 -0.00090 0.00662 -0.00262 O8 5 0.711188 0.053777 0.604306 11.00000 0.01533 0.02573 = 0.01549 0.00585 0.00444 0.00727 O3 5 0.449690 0.646624 0.370440 11.00000 0.03137 0.01506 = 0.02139 -0.00338 0.01206 -0.00564 O10 5 0.767908 0.142693 0.350425 11.00000 0.01873 0.02762 = 0.01943 0.00732 0.01007 0.00782 O5 5 0.279364 0.515931 0.560351 11.00000 0.03006 0.02483 = 0.01981 -0.00452 0.01407 -0.00299 O7 5 0.587423 0.065836 0.727814 11.00000 0.02349 0.04322 = 0.01590 0.00706 0.00686 0.00815 N1 4 0.446376 0.642749 -0.031839 11.00000 0.01505 0.01191 = 0.01648 -0.00006 0.00244 -0.00001 O11 5 0.224734 0.645641 0.676852 11.00000 0.04938 0.03024 = 0.02891 -0.00844 0.02503 -0.00977 O2 5 0.592345 0.594707 0.250204 11.00000 0.03178 0.04458 = 0.01823 -0.00664 0.01256 -0.02314 O6 5 0.406901 0.114662 0.685554 11.00000 0.02230 0.05959 = 0.02030 0.00746 0.01116 0.00963 O4 5 0.344014 0.653757 0.506574 11.00000 0.04794 0.02091 = 0.03317 -0.00931 0.02271 -0.00772 N2 4 0.441040 0.803967 -0.042993 11.00000 0.01985 0.01097 = 0.01778 0.00051 0.00327 0.00017 C16 1 0.637312 0.119139 0.451276 11.00000 0.01260 0.01067 = 0.01632 -0.00120 0.00470 0.00017 C17 1 0.545879 0.163138 0.389836 11.00000 0.01559 0.01263 = 0.01338 0.00035 0.00426 0.00053 AFIX 43 H17 2 0.556234 0.179770 0.330685 11.00000 -1.20000 AFIX 0 C8 1 0.507380 0.534770 0.220294 11.00000 0.01778 0.01430 = 0.01503 -0.00014 0.00426 0.00047 C20 1 0.494409 0.725637 0.002884 11.00000 0.01715 0.01312 = 0.01907 0.00077 0.00316 0.00097 AFIX 43 H20 2 0.557262 0.729562 0.052796 11.00000 -1.20000 AFIX 0 C12 1 0.439365 0.183337 0.413252 11.00000 0.01286 0.00960 = 0.01659 -0.00023 0.00170 -0.00021 C5 1 0.419081 0.394444 0.285120 11.00000 0.01373 0.01750 = 0.01256 -0.00151 0.00242 0.00207 AFIX 43 H5A 2 0.434882 0.358798 0.235138 11.00000 -1.20000 AFIX 0 C7 1 0.340828 0.403607 0.421329 11.00000 0.01303 0.01790 = 0.01362 0.00341 0.00312 0.00006 AFIX 43 H7A 2 0.306001 0.373848 0.465642 11.00000 -1.20000 AFIX 0 C6 1 0.366969 0.346382 0.349524 11.00000 0.01115 0.01294 = 0.01340 0.00147 0.00075 0.00036 C15 1 0.623799 0.095466 0.541526 11.00000 0.01414 0.01166 = 0.01411 -0.00036 0.00139 -0.00024 C19 1 0.750102 0.101215 0.422559 11.00000 0.01347 0.01461 = 0.01575 -0.00269 0.00333 0.00039 C23 1 0.470625 0.904464 -0.021716 11.00000 0.01774 0.00993 = 0.02108 -0.00010 0.00407 -0.00022 C2 1 0.365227 0.503982 0.428813 11.00000 0.01532 0.01656 = 0.01380 -0.00176 0.00341 0.00045 C4 1 0.448576 0.493828 0.292443 11.00000 0.01255 0.01848 = 0.01285 0.00226 0.00225 -0.00182 C14 1 0.518868 0.117563 0.568117 11.00000 0.01645 0.01484 = 0.01323 -0.00024 0.00460 -0.00012 C3 1 0.422551 0.550301 0.365166 11.00000 0.01573 0.01535 = 0.01355 0.00133 0.00090 -0.00091 C25 1 0.521226 1.063568 -0.068909 11.00000 0.02496 0.01295 = 0.01839 0.00362 0.00727 -0.00003 AFIX 43 H25 2 0.535699 1.106637 -0.114371 11.00000 -1.20000 AFIX 0 C9 1 0.341683 0.235017 0.343522 11.00000 0.01219 0.01280 = 0.01583 0.00118 0.00228 0.00092 C13 1 0.428323 0.160036 0.503273 11.00000 0.01382 0.01500 = 0.01803 -0.00065 0.00612 0.00036 AFIX 43 H13 2 0.358323 0.173147 0.520961 11.00000 -1.20000 AFIX 0 C18 1 0.498952 0.099362 0.663956 11.00000 0.02065 0.02267 = 0.01574 0.00137 0.00455 0.00008 C1 1 0.329135 0.564398 0.501821 11.00000 0.01876 0.02289 = 0.01627 -0.00222 0.00472 -0.00132 C22 1 0.352883 0.768579 -0.111618 11.00000 0.02846 0.01768 = 0.02522 0.00252 -0.00860 0.00122 AFIX 43 H22 2 0.300783 0.805289 -0.154599 11.00000 -1.20000 AFIX 0 C24 1 0.491244 0.966631 -0.091005 11.00000 0.02576 0.01450 = 0.01718 -0.00173 0.00677 0.00099 AFIX 43 H24 2 0.485092 0.943767 -0.151468 11.00000 -1.20000 AFIX 0 C11 1 0.336868 0.196238 0.244311 11.00000 0.02018 0.01615 = 0.01784 -0.00121 -0.00191 0.00115 AFIX 137 H11A 2 0.410998 0.205708 0.227860 11.00000 -1.50000 H11B 2 0.278375 0.231404 0.201407 11.00000 -1.50000 H11C 2 0.318229 0.127433 0.241837 11.00000 -1.50000 AFIX 0 C10 1 0.222253 0.213872 0.365900 11.00000 0.01282 0.01652 = 0.02567 0.00360 0.00268 -0.00018 AFIX 137 H10A 2 0.209648 0.144126 0.365890 11.00000 -1.50000 H10B 2 0.162921 0.244118 0.319774 11.00000 -1.50000 H10C 2 0.219452 0.240139 0.426041 11.00000 -1.50000 AFIX 0 C21 1 0.357536 0.669472 -0.103749 11.00000 0.02445 0.01816 = 0.02485 -0.00092 -0.00435 -0.00334 AFIX 43 H21 2 0.307966 0.625907 -0.141416 11.00000 -1.20000 AFIX 0 H3 2 0.426672 0.667733 0.417675 11.00000 -1.50000 H5 2 0.262310 0.555475 0.600281 11.00000 -1.50000 H8 2 0.762182 0.042806 0.571962 11.00000 -1.50000 H7 2 0.645257 0.058152 0.702041 11.00000 -1.50000 H2 2 0.632618 0.609340 0.209624 11.00000 -1.50000 H11D 2 0.179924 0.640130 0.714997 11.00000 -1.50000 H11E 2 0.242265 0.705735 0.672082 11.00000 -1.50000 HKLF 4 REM 1_a.res in P2(1)/n REM wR2 = 0.0935, GooF = S = 1.027, Restrained GooF = 1.026 for all data REM R1 = 0.0375 for 4384 Fo > 4sig(Fo) and 0.0495 for all 5270 data REM 372 parameters refined using 8 restraints END WGHT 0.0394 1.9545 REM Highest difference peak 0.361, deepest hole -0.513, 1-sigma level 0.061 Q1 1 0.3844 0.2031 0.3740 11.00000 0.05 0.36 Q2 1 0.3581 0.2898 0.3533 11.00000 0.05 0.35 ; _shelx_res_checksum 641 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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 0.500000 0.500000 0.000000 0.01099(9) Uani 1 2 d S . P . . O9 O 0.82285(11) 0.04608(9) 0.47471(9) 0.0161(3) Uani 1 1 d . . . . . O1 O 0.47670(12) 0.50912(10) 0.13913(9) 0.0190(3) Uani 1 1 d . . . . . O8 O 0.71119(11) 0.05378(10) 0.60431(9) 0.0187(3) Uani 1 1 d D . . . . O3 O 0.44969(13) 0.64662(10) 0.37044(9) 0.0217(3) Uani 1 1 d D . . . . O10 O 0.76791(11) 0.14269(10) 0.35043(9) 0.0210(3) Uani 1 1 d . . . . . O5 O 0.27936(13) 0.51593(10) 0.56035(9) 0.0236(3) Uani 1 1 d D . . . . O7 O 0.58742(13) 0.06584(12) 0.72781(9) 0.0271(3) Uani 1 1 d D . . . . N1 N 0.44638(13) 0.64275(11) -0.03184(10) 0.0146(3) Uani 1 1 d . . . . . O11 O 0.22473(15) 0.64564(12) 0.67685(11) 0.0338(4) Uani 1 1 d D . . . . O2 O 0.59234(13) 0.59471(12) 0.25020(10) 0.0305(4) Uani 1 1 d D . . . . O6 O 0.40690(13) 0.11466(13) 0.68555(10) 0.0331(4) Uani 1 1 d . . . . . O4 O 0.34401(15) 0.65376(11) 0.50657(10) 0.0320(4) Uani 1 1 d . . . . . N2 N 0.44104(14) 0.80397(11) -0.04299(10) 0.0163(3) Uani 1 1 d . . . . . C16 C 0.63731(15) 0.11914(12) 0.45128(12) 0.0129(3) Uani 1 1 d . . . . . C17 C 0.54588(15) 0.16314(12) 0.38984(12) 0.0137(3) Uani 1 1 d . . . . . H17 H 0.556234 0.179770 0.330685 0.016 Uiso 1 1 calc R U . . . C8 C 0.50738(16) 0.53477(13) 0.22029(12) 0.0156(4) Uani 1 1 d . . . . . C20 C 0.49441(16) 0.72564(13) 0.00288(13) 0.0165(4) Uani 1 1 d . . . . . H20 H 0.557262 0.729562 0.052796 0.020 Uiso 1 1 calc R U . . . C12 C 0.43936(15) 0.18334(12) 0.41325(12) 0.0132(3) Uani 1 1 d . . . . . C5 C 0.41908(15) 0.39444(13) 0.28512(12) 0.0146(3) Uani 1 1 d . . . . . H5A H 0.434882 0.358798 0.235138 0.018 Uiso 1 1 calc R U . . . C7 C 0.34083(15) 0.40361(13) 0.42133(12) 0.0148(3) Uani 1 1 d . . . . . H7A H 0.306001 0.373848 0.465642 0.018 Uiso 1 1 calc R U . . . C6 C 0.36697(15) 0.34638(12) 0.34952(12) 0.0128(3) Uani 1 1 d . . . . . C15 C 0.62380(15) 0.09547(12) 0.54153(12) 0.0135(3) Uani 1 1 d . . . . . C19 C 0.75010(15) 0.10121(13) 0.42256(12) 0.0146(3) Uani 1 1 d . . . . . C23 C 0.47063(16) 0.90446(13) -0.02172(13) 0.0162(4) Uani 1 1 d . . . . . C2 C 0.36523(15) 0.50398(13) 0.42881(12) 0.0152(3) Uani 1 1 d . . . . . C4 C 0.44858(15) 0.49383(13) 0.29244(12) 0.0147(3) Uani 1 1 d . . . . . C14 C 0.51887(16) 0.11756(13) 0.56812(12) 0.0146(3) Uani 1 1 d . . . . . C3 C 0.42255(16) 0.55030(13) 0.36517(12) 0.0152(4) Uani 1 1 d . . . . . C25 C 0.52123(17) 1.06357(13) -0.06891(13) 0.0184(4) Uani 1 1 d . . . . . H25 H 0.535699 1.106637 -0.114371 0.022 Uiso 1 1 calc R U . . . C9 C 0.34168(15) 0.23502(13) 0.34352(12) 0.0137(3) Uani 1 1 d . . . . . C13 C 0.42832(15) 0.16004(13) 0.50327(12) 0.0152(4) Uani 1 1 d . . . . . H13 H 0.358323 0.173147 0.520961 0.018 Uiso 1 1 calc R U . . . C18 C 0.49895(17) 0.09936(14) 0.66396(13) 0.0196(4) Uani 1 1 d . . . . . C1 C 0.32913(17) 0.56440(14) 0.50182(13) 0.0191(4) Uani 1 1 d . . . . . C22 C 0.35288(19) 0.76858(14) -0.11162(14) 0.0258(4) Uani 1 1 d . . . . . H22 H 0.300783 0.805289 -0.154599 0.031 Uiso 1 1 calc R U . . . C24 C 0.49124(17) 0.96663(14) -0.09101(13) 0.0188(4) Uani 1 1 d . . . . . H24 H 0.485092 0.943767 -0.151468 0.023 Uiso 1 1 calc R U . . . C11 C 0.33687(17) 0.19624(13) 0.24431(13) 0.0189(4) Uani 1 1 d . . . . . H11A H 0.410998 0.205708 0.227860 0.028 Uiso 1 1 calc R U . . . H11B H 0.278375 0.231404 0.201407 0.028 Uiso 1 1 calc R U . . . H11C H 0.318229 0.127433 0.241837 0.028 Uiso 1 1 calc R U . . . C10 C 0.22225(16) 0.21387(14) 0.36590(13) 0.0185(4) Uani 1 1 d . . . . . H10A H 0.209648 0.144126 0.365890 0.028 Uiso 1 1 calc R U . . . H10B H 0.162921 0.244118 0.319774 0.028 Uiso 1 1 calc R U . . . H10C H 0.219452 0.240139 0.426041 0.028 Uiso 1 1 calc R U . . . C21 C 0.35754(18) 0.66947(14) -0.10375(14) 0.0238(4) Uani 1 1 d . . . . . H21 H 0.307966 0.625907 -0.141416 0.029 Uiso 1 1 calc R U . . . H3 H 0.427(2) 0.6677(18) 0.4177(12) 0.036 Uiso 1 1 d D U . . . H5 H 0.262(2) 0.5555(15) 0.6003(13) 0.036 Uiso 1 1 d D U . . . H8 H 0.7622(17) 0.0428(19) 0.5720(15) 0.036 Uiso 1 1 d D U . . . H7 H 0.6453(15) 0.0582(19) 0.7020(16) 0.036 Uiso 1 1 d D U . . . H2 H 0.6326(19) 0.6093(18) 0.2096(13) 0.036 Uiso 1 1 d D U . . . H11D H 0.1799(18) 0.6401(16) 0.7150(14) 0.036 Uiso 1 1 d D U . . . H11E H 0.242(2) 0.7057(9) 0.6721(16) 0.036 Uiso 1 1 d D 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 Co1 0.01240(17) 0.00928(16) 0.01172(16) -0.00056(12) 0.00342(12) -0.00134(12) O9 0.0128(6) 0.0172(6) 0.0186(6) 0.0023(5) 0.0035(5) 0.0041(5) O1 0.0221(7) 0.0219(7) 0.0143(6) -0.0009(5) 0.0066(5) -0.0026(5) O8 0.0153(6) 0.0257(7) 0.0155(6) 0.0058(5) 0.0044(5) 0.0073(5) O3 0.0314(8) 0.0151(6) 0.0214(7) -0.0034(5) 0.0121(6) -0.0056(6) O10 0.0187(7) 0.0276(7) 0.0194(6) 0.0073(6) 0.0101(5) 0.0078(6) O5 0.0301(8) 0.0248(8) 0.0198(7) -0.0045(6) 0.0141(6) -0.0030(6) O7 0.0235(8) 0.0432(9) 0.0159(7) 0.0071(6) 0.0069(6) 0.0082(7) N1 0.0150(7) 0.0119(7) 0.0165(7) -0.0001(6) 0.0024(6) 0.0000(6) O11 0.0494(10) 0.0302(8) 0.0289(8) -0.0084(7) 0.0250(7) -0.0098(7) O2 0.0318(8) 0.0446(9) 0.0182(7) -0.0066(6) 0.0126(6) -0.0231(7) O6 0.0223(8) 0.0596(11) 0.0203(7) 0.0075(7) 0.0112(6) 0.0096(7) O4 0.0479(10) 0.0209(8) 0.0332(8) -0.0093(6) 0.0227(7) -0.0077(7) N2 0.0198(8) 0.0110(7) 0.0178(7) 0.0005(6) 0.0033(6) 0.0002(6) C16 0.0126(8) 0.0107(8) 0.0163(8) -0.0012(6) 0.0047(7) 0.0002(6) C17 0.0156(9) 0.0126(8) 0.0134(8) 0.0003(6) 0.0043(7) 0.0005(6) C8 0.0178(9) 0.0143(8) 0.0150(8) -0.0001(7) 0.0043(7) 0.0005(7) C20 0.0171(9) 0.0131(8) 0.0191(8) 0.0008(7) 0.0032(7) 0.0010(7) C12 0.0129(8) 0.0096(8) 0.0166(8) -0.0002(6) 0.0017(7) -0.0002(6) C5 0.0137(8) 0.0175(9) 0.0126(8) -0.0015(7) 0.0024(7) 0.0021(7) C7 0.0130(8) 0.0179(9) 0.0136(8) 0.0034(7) 0.0031(7) 0.0001(7) C6 0.0112(8) 0.0129(8) 0.0134(8) 0.0015(6) 0.0008(7) 0.0004(6) C15 0.0141(8) 0.0117(8) 0.0141(8) -0.0004(6) 0.0014(7) -0.0002(6) C19 0.0135(8) 0.0146(8) 0.0157(8) -0.0027(7) 0.0033(7) 0.0004(7) C23 0.0177(9) 0.0099(8) 0.0211(9) -0.0001(7) 0.0041(7) -0.0002(7) C2 0.0153(8) 0.0166(8) 0.0138(8) -0.0018(7) 0.0034(7) 0.0004(7) C4 0.0126(8) 0.0185(9) 0.0129(8) 0.0023(7) 0.0023(7) -0.0018(7) C14 0.0164(9) 0.0148(8) 0.0132(8) -0.0002(7) 0.0046(7) -0.0001(7) C3 0.0157(9) 0.0153(9) 0.0135(8) 0.0013(7) 0.0009(7) -0.0009(7) C25 0.0250(10) 0.0130(8) 0.0184(9) 0.0036(7) 0.0073(8) 0.0000(7) C9 0.0122(8) 0.0128(8) 0.0158(8) 0.0012(6) 0.0023(7) 0.0009(6) C13 0.0138(8) 0.0150(8) 0.0180(8) -0.0007(7) 0.0061(7) 0.0004(7) C18 0.0207(10) 0.0227(10) 0.0157(9) 0.0014(7) 0.0045(8) 0.0001(7) C1 0.0188(9) 0.0229(10) 0.0163(9) -0.0022(7) 0.0047(7) -0.0013(7) C22 0.0285(11) 0.0177(10) 0.0252(10) 0.0025(8) -0.0086(9) 0.0012(8) C24 0.0258(10) 0.0145(8) 0.0172(8) -0.0017(7) 0.0068(8) 0.0010(7) C11 0.0202(9) 0.0162(9) 0.0178(9) -0.0012(7) -0.0019(8) 0.0012(7) C10 0.0128(9) 0.0165(9) 0.0257(9) 0.0036(7) 0.0027(8) -0.0002(7) C21 0.0245(10) 0.0182(10) 0.0249(10) -0.0009(8) -0.0044(8) -0.0033(8) 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 N1 Co1 N1 180.0 3_665 . ? N1 Co1 O1 93.99(5) 3_665 3_665 ? N1 Co1 O1 86.01(5) . 3_665 ? N1 Co1 O1 86.01(5) 3_665 . ? N1 Co1 O1 93.99(5) . . ? O1 Co1 O1 180.0 3_665 . ? N1 Co1 O9 90.30(5) 3_665 4_565 ? N1 Co1 O9 89.70(5) . 4_565 ? O1 Co1 O9 97.44(5) 3_665 4_565 ? O1 Co1 O9 82.56(5) . 4_565 ? N1 Co1 O9 89.70(5) 3_665 2_655 ? N1 Co1 O9 90.30(5) . 2_655 ? O1 Co1 O9 82.56(5) 3_665 2_655 ? O1 Co1 O9 97.44(5) . 2_655 ? O9 Co1 O9 180.00(6) 4_565 2_655 ? C19 O9 Co1 142.32(12) . 2_645 ? C8 O1 Co1 152.29(13) . . ? C15 O8 H8 102.5(17) . . ? C3 O3 H3 105.4(18) . . ? C1 O5 H5 109.6(18) . . ? C18 O7 H7 108.0(17) . . ? C20 N1 C21 105.66(15) . . ? C20 N1 Co1 129.09(12) . . ? C21 N1 Co1 124.87(12) . . ? H11D O11 H11E 109.5(14) . . ? C8 O2 H2 114.1(17) . . ? C20 N2 C22 107.11(15) . . ? C20 N2 C23 125.45(15) . . ? C22 N2 C23 127.42(16) . . ? C17 C16 C15 119.32(16) . . ? C17 C16 C19 120.06(16) . . ? C15 C16 C19 120.57(16) . . ? C16 C17 C12 122.67(16) . . ? C16 C17 H17 118.7 . . ? C12 C17 H17 118.7 . . ? O1 C8 O2 124.27(17) . . ? O1 C8 C4 120.04(17) . . ? O2 C8 C4 115.66(15) . . ? N1 C20 N2 111.40(16) . . ? N1 C20 H20 124.3 . . ? N2 C20 H20 124.3 . . ? C13 C12 C17 116.98(16) . . ? C13 C12 C9 122.20(16) . . ? C17 C12 C9 120.71(15) . . ? C6 C5 C4 122.70(16) . . ? C6 C5 H5A 118.7 . . ? C4 C5 H5A 118.7 . . ? C2 C7 C6 122.14(16) . . ? C2 C7 H7A 118.9 . . ? C6 C7 H7A 118.9 . . ? C5 C6 C7 116.64(16) . . ? C5 C6 C9 121.93(15) . . ? C7 C6 C9 121.41(15) . . ? O8 C15 C14 119.20(15) . . ? O8 C15 C16 121.41(16) . . ? C14 C15 C16 119.38(16) . . ? O10 C19 O9 124.49(16) . . ? O10 C19 C16 118.50(16) . . ? O9 C19 C16 116.99(15) . . ? C24 C23 C25 121.87(17) . 3_675 ? C24 C23 N2 119.69(16) . . ? C25 C23 N2 118.44(16) 3_675 . ? C7 C2 C3 120.27(16) . . ? C7 C2 C1 121.02(16) . . ? C3 C2 C1 118.70(16) . . ? C5 C4 C3 120.06(16) . . ? C5 C4 C8 116.91(16) . . ? C3 C4 C8 123.03(16) . . ? C13 C14 C15 119.29(16) . . ? C13 C14 C18 117.73(16) . . ? C15 C14 C18 122.97(16) . . ? O3 C3 C4 119.42(16) . . ? O3 C3 C2 122.46(16) . . ? C4 C3 C2 118.09(16) . . ? C23 C25 C24 119.20(17) 3_675 . ? C23 C25 H25 120.4 3_675 . ? C24 C25 H25 120.4 . . ? C10 C9 C11 106.33(15) . . ? C10 C9 C6 110.25(14) . . ? C11 C9 C6 111.07(14) . . ? C10 C9 C12 111.23(14) . . ? C11 C9 C12 110.51(14) . . ? C6 C9 C12 107.50(14) . . ? C12 C13 C14 122.32(16) . . ? C12 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? O6 C18 O7 119.17(17) . . ? O6 C18 C14 122.78(17) . . ? O7 C18 C14 118.04(16) . . ? O4 C1 O5 122.50(17) . . ? O4 C1 C2 122.12(17) . . ? O5 C1 C2 115.38(17) . . ? C21 C22 N2 105.93(17) . . ? C21 C22 H22 127.0 . . ? N2 C22 H22 127.0 . . ? C23 C24 C25 118.93(17) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C22 C21 N1 109.90(17) . . ? C22 C21 H21 125.1 . . ? N1 C21 H21 125.1 . . ? 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 N1 2.0649(15) 3_665 ? Co1 N1 2.0650(14) . ? Co1 O1 2.1212(12) 3_665 ? Co1 O1 2.1212(12) . ? Co1 O9 2.1341(12) 4_565 ? Co1 O9 2.1341(12) 2_655 ? O9 C19 1.270(2) . ? O1 C8 1.224(2) . ? O8 C15 1.356(2) . ? O8 H8 0.851(10) . ? O3 C3 1.347(2) . ? O3 H3 0.845(10) . ? O10 C19 1.256(2) . ? O5 C1 1.313(2) . ? O5 H5 0.850(10) . ? O7 C18 1.331(2) . ? O7 H7 0.850(10) . ? N1 C20 1.316(2) . ? N1 C21 1.374(2) . ? O11 H11D 0.848(9) . ? O11 H11E 0.849(9) . ? O2 C8 1.295(2) . ? O2 H2 0.858(10) . ? O6 C18 1.207(2) . ? O4 C1 1.228(2) . ? N2 C20 1.345(2) . ? N2 C22 1.376(2) . ? N2 C23 1.429(2) . ? C16 C17 1.390(2) . ? C16 C15 1.405(2) . ? C16 C19 1.492(2) . ? C17 C12 1.393(2) . ? C17 H17 0.9300 . ? C8 C4 1.488(2) . ? C20 H20 0.9300 . ? C12 C13 1.392(2) . ? C12 C9 1.543(2) . ? C5 C6 1.392(2) . ? C5 C4 1.394(3) . ? C5 H5A 0.9300 . ? C7 C2 1.395(3) . ? C7 C6 1.395(2) . ? C7 H7A 0.9300 . ? C6 C9 1.542(2) . ? C15 C14 1.401(2) . ? C23 C24 1.383(3) . ? C23 C25 1.385(3) 3_675 ? C2 C3 1.409(2) . ? C2 C1 1.481(2) . ? C4 C3 1.400(2) . ? C14 C13 1.400(2) . ? C14 C18 1.495(2) . ? C25 C24 1.386(3) . ? C25 H25 0.9300 . ? C9 C10 1.534(2) . ? C9 C11 1.540(2) . ? C13 H13 0.9300 . ? C22 C21 1.353(3) . ? C22 H22 0.9300 . ? C24 H24 0.9300 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C21 H21 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 C15 C16 C17 C12 -1.3(3) . . . . ? C19 C16 C17 C12 -178.81(16) . . . . ? Co1 O1 C8 O2 10.5(4) . . . . ? Co1 O1 C8 C4 -167.24(19) . . . . ? C21 N1 C20 N2 0.0(2) . . . . ? Co1 N1 C20 N2 173.04(12) . . . . ? C22 N2 C20 N1 0.0(2) . . . . ? C23 N2 C20 N1 178.87(16) . . . . ? C16 C17 C12 C13 1.8(3) . . . . ? C16 C17 C12 C9 178.23(16) . . . . ? C4 C5 C6 C7 2.4(3) . . . . ? C4 C5 C6 C9 -176.25(16) . . . . ? C2 C7 C6 C5 0.0(3) . . . . ? C2 C7 C6 C9 178.70(16) . . . . ? C17 C16 C15 O8 -179.03(16) . . . . ? C19 C16 C15 O8 -1.6(3) . . . . ? C17 C16 C15 C14 -0.6(3) . . . . ? C19 C16 C15 C14 176.85(16) . . . . ? Co1 O9 C19 O10 10.7(3) 2_645 . . . ? Co1 O9 C19 C16 -167.76(13) 2_645 . . . ? C17 C16 C19 O10 13.3(2) . . . . ? C15 C16 C19 O10 -164.12(16) . . . . ? C17 C16 C19 O9 -168.14(16) . . . . ? C15 C16 C19 O9 14.4(2) . . . . ? C20 N2 C23 C24 127.6(2) . . . . ? C22 N2 C23 C24 -53.8(3) . . . . ? C20 N2 C23 C25 -51.8(3) . . . 3_675 ? C22 N2 C23 C25 126.7(2) . . . 3_675 ? C6 C7 C2 C3 -2.8(3) . . . . ? C6 C7 C2 C1 175.66(16) . . . . ? C6 C5 C4 C3 -2.1(3) . . . . ? C6 C5 C4 C8 178.03(16) . . . . ? O1 C8 C4 C5 39.3(3) . . . . ? O2 C8 C4 C5 -138.63(18) . . . . ? O1 C8 C4 C3 -140.56(19) . . . . ? O2 C8 C4 C3 41.5(3) . . . . ? O8 C15 C14 C13 -179.61(16) . . . . ? C16 C15 C14 C13 2.0(3) . . . . ? O8 C15 C14 C18 1.4(3) . . . . ? C16 C15 C14 C18 -177.02(16) . . . . ? C5 C4 C3 O3 -178.83(16) . . . . ? C8 C4 C3 O3 1.1(3) . . . . ? C5 C4 C3 C2 -0.7(3) . . . . ? C8 C4 C3 C2 179.15(16) . . . . ? C7 C2 C3 O3 -178.89(17) . . . . ? C1 C2 C3 O3 2.6(3) . . . . ? C7 C2 C3 C4 3.1(3) . . . . ? C1 C2 C3 C4 -175.40(16) . . . . ? C5 C6 C9 C10 -139.02(17) . . . . ? C7 C6 C9 C10 42.4(2) . . . . ? C5 C6 C9 C11 -21.4(2) . . . . ? C7 C6 C9 C11 159.99(16) . . . . ? C5 C6 C9 C12 99.58(19) . . . . ? C7 C6 C9 C12 -79.0(2) . . . . ? C13 C12 C9 C10 -26.3(2) . . . . ? C17 C12 C9 C10 157.52(16) . . . . ? C13 C12 C9 C11 -144.13(17) . . . . ? C17 C12 C9 C11 39.7(2) . . . . ? C13 C12 C9 C6 94.51(19) . . . . ? C17 C12 C9 C6 -81.70(19) . . . . ? C17 C12 C13 C14 -0.4(3) . . . . ? C9 C12 C13 C14 -176.78(16) . . . . ? C15 C14 C13 C12 -1.4(3) . . . . ? C18 C14 C13 C12 177.60(16) . . . . ? C13 C14 C18 O6 4.2(3) . . . . ? C15 C14 C18 O6 -176.82(19) . . . . ? C13 C14 C18 O7 -175.10(17) . . . . ? C15 C14 C18 O7 3.9(3) . . . . ? C7 C2 C1 O4 -175.93(19) . . . . ? C3 C2 C1 O4 2.5(3) . . . . ? C7 C2 C1 O5 3.5(3) . . . . ? C3 C2 C1 O5 -178.03(16) . . . . ? C20 N2 C22 C21 -0.1(2) . . . . ? C23 N2 C22 C21 -178.86(18) . . . . ? C25 C23 C24 C25 0.2(3) 3_675 . . . ? N2 C23 C24 C25 -179.22(17) . . . . ? C23 C25 C24 C23 -0.2(3) 3_675 . . . ? N2 C22 C21 N1 0.1(2) . . . . ? C20 N1 C21 C22 0.0(2) . . . . ? Co1 N1 C21 C22 -173.46(14) . . . . ?