#------------------------------------------------------------------------------ #$Date: 2021-12-07 05:41:14 +0200 (Tue, 07 Dec 2021) $ #$Revision: 271197 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/10/7061058.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_7061058 loop_ _publ_author_name 'Ma, Zhen-Zhen' 'Ma, Yao' 'Liu, Bing' 'Xu, Ling' 'Jiao, Huan' _publ_section_title ; A high-performance Co-MOF non-enzymatic electrochemical sensor for glucose detection ; _journal_issue 45 _journal_name_full 'New Journal of Chemistry' _journal_page_first 21350 _journal_page_last 21358 _journal_paper_doi 10.1039/D1NJ04480J _journal_volume 45 _journal_year 2021 _chemical_formula_sum 'C34 H38 Cl2 Co3 N2 O14' _chemical_formula_weight 946.35 _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 geom _audit_block_doi 10.5517/ccdc.csd.cc28stb7 _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2021-10-20 deposited with the CCDC. 2021-10-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 107.452(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 12.7807(3) _cell_length_b 9.5182(3) _cell_length_c 17.9186(4) _cell_measurement_reflns_used 6795 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 75.1290 _cell_measurement_theta_min 3.7280 _cell_volume 2079.45(10) _computing_cell_refinement 'CrysAlisPro 1.171.40.19a (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.40.19a (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.40.19a (Rigaku OD, 2018)' _computing_structure_refinement 'SHELX-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELX-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.947 _diffrn_measurement_device_type 'XtaLAB Synergy R, HyPix' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_unetI/netI 0.0322 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.947 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 13681 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.947 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 75.442 _diffrn_reflns_theta_min 5.897 _diffrn_source 'Rotating-anode X-ray tube' _exptl_absorpt_coefficient_mu 10.999 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.20925 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.19a (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.511 _exptl_crystal_description block _exptl_crystal_F_000 966 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.154 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.099 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 320 _refine_ls_number_reflns 4075 _refine_ls_number_restraints 113 _refine_ls_restrained_S_all 1.066 _refine_ls_R_factor_all 0.0816 _refine_ls_R_factor_gt 0.0659 _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^)+(0.0883P)^2^+6.1645P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1659 _refine_ls_wR_factor_ref 0.1809 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3375 _reflns_number_total 4075 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1nj04480j2.cif _cod_data_source_block 14 _cod_depositor_comments 'Adding full bibliography for 7061058--7061059.cif.' _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7061058 _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_res_file ; 14.res created by SHELXL-2014/7 TITL 14 in P2(1)/n CELL 1.54178 12.7807 9.5182 17.9186 90 107.452 90 ZERR 2 0.0003 0.0003 0.0004 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Cl Co N O UNIT 68 76 4 6 4 28 DFIX 1.25 O1 C1 DFIX 1.5 C1 C2 DFIX 1.5 N1 C2 SADI N1 C3 N1A C3A SADI 0.04 C2 C5 C2A C5A SADI N1 C4 N1A C4A SADI N1 C2 N1A C2A SADI C1 C2 C1A C2A SADI C1 O1 C1A O1A SADI N1 C5 N1A C5A SADI 0.04 C2 C3 C2A C3A SADI 0.04 C3 C5 C3A C5A SADI 0.04 C4 C5 C4A C5A SADI 0.04 C2 C4 C2A C4A SADI 0.04 C2 O1 C2A O1A SADI 0.04 C3 C4 C3A C4A SADI 0.04 N1 C1 N1A C1A RIGU 0.001 0.001 C2A C4A N1A C3A C5A C1A O1A RIGU 0.001 0.001 C3 N1 C2 C4 C5 C1 O1 ISOR 0.01 0.02 O1 isor 0.02 0.01 c1a L.S. 100 PLAN 4 CONF BOND MORE -1 BOND $H fmap 2 acta OMIT 2 0 0 OMIT 3 10 7 OMIT 7 9 0 OMIT 13 4 1 OMIT -4 1 8 OMIT -2 0 2 OMIT -1 1 1 OMIT -1 0 7 OMIT 0 2 4 OMIT -3 1 1 OMIT 0 1 6 omit 0 2 7 omit 0 1 3 omit -1 0 1 omit -1 1 2 REM REM REM > REM REM > REM > REM REM WGHT 0.088300 6.164500 FVAR 0.55151 CO1 4 0.797107 0.536408 0.071716 11.00000 0.01332 0.07256 = 0.02020 -0.00019 0.00695 0.00063 CO2 4 1.000000 0.500000 0.000000 10.50000 0.00965 0.07533 = 0.01314 0.00004 0.00274 0.00017 CL1 3 0.690401 0.636214 0.136099 11.00000 0.03783 0.12763 = 0.06884 -0.03615 0.03477 -0.00326 C11 1 1.045425 0.279290 0.216235 11.00000 0.01942 0.06590 = 0.02058 -0.00325 0.00441 -0.00406 C12 1 1.006329 0.250713 0.278906 11.00000 0.01571 0.07181 = 0.02490 0.00656 0.00580 0.00159 AFIX 43 H12 2 0.934174 0.272952 0.275460 11.00000 -1.20000 AFIX 0 C13 1 1.072791 0.189861 0.346205 11.00000 0.02054 0.07081 = 0.01960 0.00440 0.00775 0.00065 AFIX 43 H13 2 1.045496 0.171378 0.387826 11.00000 -1.20000 AFIX 0 C14 1 1.181257 0.155927 0.351882 11.00000 0.01752 0.07006 = 0.02225 -0.00535 0.00357 -0.00188 C15 1 1.220322 0.180899 0.288064 11.00000 0.01424 0.09155 = 0.02834 -0.00022 0.00556 -0.00081 AFIX 43 H15 2 1.291961 0.156442 0.291186 11.00000 -1.20000 AFIX 0 C16 1 1.153535 0.241589 0.220350 11.00000 0.01988 0.09128 = 0.02324 0.00264 0.00908 -0.00022 AFIX 43 H16 2 1.179785 0.257337 0.177958 11.00000 -1.20000 AFIX 0 C17 1 0.975935 0.351927 0.145680 11.00000 0.01943 0.07275 = 0.02451 -0.00235 0.00519 -0.00528 C18 1 1.254100 0.093615 0.425376 11.00000 0.01495 0.07118 = 0.02802 -0.00268 0.00321 -0.00095 O11 6 0.885913 0.403884 0.150230 11.00000 0.02071 0.09233 = 0.02642 0.01301 0.00712 0.00457 O12 6 1.009503 0.361255 0.086991 11.00000 0.03958 0.08181 = 0.02099 0.00376 0.01353 0.00470 O13 6 1.210284 0.062614 0.478509 11.00000 0.02175 0.08204 = 0.02562 0.00119 0.00451 0.00465 O14 6 1.353161 0.074522 0.429330 11.00000 0.01384 0.08879 = 0.03364 0.00876 -0.00030 -0.00055 C21 1 0.935409 0.886152 0.005408 11.00000 0.01694 0.07024 = 0.03290 -0.00238 0.00857 -0.00051 C22 1 0.891367 0.994524 -0.045707 11.00000 0.01756 0.07595 = 0.04023 0.00438 0.00264 -0.00047 AFIX 43 H22 2 0.818380 0.990757 -0.076266 11.00000 -1.20000 AFIX 0 C23 1 0.955550 1.108566 -0.051533 11.00000 0.02013 0.07768 = 0.03048 0.00546 0.00395 0.00140 AFIX 43 H23 2 0.926002 1.181304 -0.086078 11.00000 -1.20000 AFIX 0 C24 1 0.865741 0.762928 0.011419 11.00000 0.01973 0.08580 = 0.04235 0.00248 0.01229 -0.00170 O21 6 0.914258 0.655778 0.052006 11.00000 0.01929 0.07267 = 0.02421 0.00150 0.01058 0.00230 O22 6 0.765352 0.766613 -0.019957 11.00000 0.01732 0.10046 = 0.10793 0.03104 0.00475 -0.00492 PART 1 N1 5 0.567256 1.225358 0.141840 10.50000 0.03687 0.07128 = 0.09669 0.03074 -0.01561 -0.00128 C1 1 0.710882 1.078378 0.095584 10.50000 0.05280 0.11054 = 0.15062 -0.01504 0.00087 -0.00702 AFIX 43 H1 2 0.784930 1.054980 0.112247 10.50000 -1.20000 AFIX 0 C2 1 0.683086 1.193804 0.140788 10.50000 0.03710 0.07343 = 0.09096 0.03016 -0.01695 -0.00060 AFIX 23 H2A 2 0.710380 1.279223 0.123676 10.50000 -1.20000 H2B 2 0.726385 1.179225 0.194799 10.50000 -1.20000 AFIX 0 C3 1 0.569852 1.329011 0.205605 10.50000 0.04154 0.07480 = 0.10100 0.02900 -0.01231 -0.00120 AFIX 137 H3A 2 0.611609 1.290721 0.255150 10.50000 -1.50000 H3B 2 0.496343 1.347746 0.206299 10.50000 -1.50000 H3C 2 0.603262 1.414800 0.196111 10.50000 -1.50000 AFIX 0 C4 1 0.517486 1.091587 0.157981 10.50000 0.04791 0.07519 = 0.10381 0.03050 -0.01011 -0.00562 AFIX 137 H4A 2 0.478076 1.047823 0.109416 10.50000 -1.50000 H4B 2 0.467971 1.111107 0.187733 10.50000 -1.50000 H4C 2 0.574344 1.029637 0.187194 10.50000 -1.50000 AFIX 0 C5 1 0.507184 1.297878 0.066785 10.50000 0.03548 0.07559 = 0.09906 0.03322 -0.01567 -0.00123 AFIX 137 H5A 2 0.549431 1.376735 0.058812 10.50000 -1.50000 H5B 2 0.437241 1.329939 0.069582 10.50000 -1.50000 H5C 2 0.496478 1.233318 0.023983 10.50000 -1.50000 AFIX 0 O1 6 0.655900 1.004387 0.039125 10.50000 0.06054 0.20990 = 0.23252 -0.10585 -0.01832 0.01218 AFIX 143 H1A 2 0.660399 0.921527 0.052236 10.50000 -1.50000 AFIX 0 PART 2 C4A 1 0.472148 1.095846 0.134752 10.50000 0.04602 0.08924 = 0.05191 0.02484 0.01388 0.00167 AFIX 137 H4AA 2 0.482504 1.071769 0.188514 10.50000 -1.50000 H4AB 2 0.495175 1.018845 0.108826 10.50000 -1.50000 H4AC 2 0.395994 1.115192 0.109533 10.50000 -1.50000 AFIX 0 N1A 5 0.539397 1.224358 0.130635 10.50000 0.04768 0.08845 = 0.05337 0.02250 0.01684 0.00025 C2A 1 0.495536 1.337115 0.172813 10.50000 0.06055 0.09601 = 0.06689 0.01457 0.02552 0.00128 AFIX 23 H2AA 2 0.522292 1.427328 0.161141 10.50000 -1.20000 H2AB 2 0.416236 1.338414 0.151549 10.50000 -1.20000 AFIX 0 C3A 1 0.504523 1.256098 0.043701 10.50000 0.03815 0.08045 = 0.05437 0.02133 0.01888 0.00613 AFIX 137 H3AA 2 0.474112 1.172986 0.014990 10.50000 -1.50000 H3AB 2 0.567082 1.286173 0.028744 10.50000 -1.50000 H3AC 2 0.450298 1.329226 0.032341 10.50000 -1.50000 AFIX 0 C5A 1 0.657685 1.194384 0.163904 10.50000 0.04833 0.09457 = 0.05646 0.02086 0.01550 0.00176 AFIX 137 H5AA 2 0.670329 1.145621 0.212710 10.50000 -1.50000 H5AB 2 0.697950 1.281057 0.172518 10.50000 -1.50000 H5AC 2 0.681654 1.136991 0.128105 10.50000 -1.50000 AFIX 0 C1A 1 0.524420 1.322749 0.259774 10.50000 0.07936 0.11520 = 0.06603 0.01406 0.02784 -0.00778 AFIX 43 H1AA 2 0.568886 1.386759 0.294230 10.50000 -1.20000 AFIX 0 O1A 6 0.480379 1.208772 0.284038 10.50000 0.08156 0.12392 = 0.07358 0.02212 0.02519 -0.01182 AFIX 147 H1AB 2 0.505652 1.201160 0.331659 10.50000 -1.50000 AFIX 0 HKLF 4 REM 14 in P2(1)/n REM R1 = 0.0659 for 3375 Fo > 4sig(Fo) and 0.0816 for all 4075 data REM 320 parameters refined using 113 restraints END WGHT 0.0945 6.3394 REM Highest difference peak 1.154, deepest hole -0.703, 1-sigma level 0.099 Q1 1 0.4237 1.0965 0.0141 11.00000 0.05 1.15 Q2 1 0.7295 0.6155 0.1761 11.00000 0.05 0.96 Q3 1 0.6470 0.9664 0.0885 11.00000 0.05 0.73 Q4 1 0.6719 1.0460 0.0238 11.00000 0.05 0.65 ; _shelx_res_checksum 41481 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 0.79711(5) 0.53641(9) 0.07172(4) 0.0349(2) Uani 1 1 d . . . . . Co2 Co 1.0000 0.5000 0.0000 0.0329(3) Uani 1 2 d S . P . . Cl1 Cl 0.69040(11) 0.6362(2) 0.13610(10) 0.0740(6) Uani 1 1 d . . . . . C11 C 1.0454(3) 0.2793(6) 0.2162(2) 0.0357(11) Uani 1 1 d . . . . . C12 C 1.0063(3) 0.2507(6) 0.2789(2) 0.0375(11) Uani 1 1 d . . . . . H12 H 0.9342 0.2730 0.2755 0.045 Uiso 1 1 calc R U . . . C13 C 1.0728(3) 0.1899(6) 0.3462(2) 0.0366(11) Uani 1 1 d . . . . . H13 H 1.0455 0.1714 0.3878 0.044 Uiso 1 1 calc R U . . . C14 C 1.1813(3) 0.1559(6) 0.3519(2) 0.0371(11) Uani 1 1 d . . . . . C15 C 1.2203(3) 0.1809(7) 0.2881(3) 0.0449(13) Uani 1 1 d . . . . . H15 H 1.2920 0.1564 0.2912 0.054 Uiso 1 1 calc R U . . . C16 C 1.1535(4) 0.2416(7) 0.2204(3) 0.0442(13) Uani 1 1 d . . . . . H16 H 1.1798 0.2573 0.1780 0.053 Uiso 1 1 calc R U . . . C17 C 0.9759(3) 0.3519(6) 0.1457(3) 0.0392(12) Uani 1 1 d . . . . . C18 C 1.2541(3) 0.0936(6) 0.4254(3) 0.0388(11) Uani 1 1 d . . . . . O11 O 0.8859(2) 0.4039(5) 0.15023(18) 0.0465(9) Uani 1 1 d . . . . . O12 O 1.0095(3) 0.3613(4) 0.08699(18) 0.0465(9) Uani 1 1 d . . . . . O13 O 1.2103(2) 0.0626(4) 0.47851(18) 0.0437(9) Uani 1 1 d . . . . . O14 O 1.3532(2) 0.0745(5) 0.42933(19) 0.0471(9) Uani 1 1 d . . . . . C21 C 0.9354(3) 0.8862(6) 0.0054(3) 0.0398(11) Uani 1 1 d . . . . . C22 C 0.8914(4) 0.9945(7) -0.0457(3) 0.0459(13) Uani 1 1 d . . . . . H22 H 0.8184 0.9908 -0.0763 0.055 Uiso 1 1 calc R U . . . C23 C 0.9556(4) 1.1086(7) -0.0515(3) 0.0436(13) Uani 1 1 d . . . . . H23 H 0.9260 1.1813 -0.0861 0.052 Uiso 1 1 calc R U . . . C24 C 0.8657(4) 0.7629(7) 0.0114(3) 0.0486(14) Uani 1 1 d . . . . . O21 O 0.9143(2) 0.6558(4) 0.05201(17) 0.0378(8) Uani 1 1 d . . . . . O22 O 0.7654(3) 0.7666(6) -0.0200(3) 0.0783(15) Uani 1 1 d . . . . . N1 N 0.5673(9) 1.2254(15) 0.1418(10) 0.076(3) Uani 0.5 1 d D U P A 1 C1 C 0.7109(13) 1.078(2) 0.0956(12) 0.111(6) Uani 0.5 1 d D U P A 1 H1 H 0.7849 1.0550 0.1122 0.133 Uiso 0.5 1 calc R U P A 1 C2 C 0.6831(10) 1.1938(16) 0.1408(9) 0.075(3) Uani 0.5 1 d D U P A 1 H2A H 0.7104 1.2792 0.1237 0.090 Uiso 0.5 1 calc R U P A 1 H2B H 0.7264 1.1792 0.1948 0.090 Uiso 0.5 1 calc R U P A 1 C3 C 0.5699(11) 1.3290(15) 0.2056(9) 0.080(3) Uani 0.5 1 d D U P A 1 H3A H 0.6116 1.2907 0.2551 0.120 Uiso 0.5 1 calc R U P A 1 H3B H 0.4963 1.3477 0.2063 0.120 Uiso 0.5 1 calc R U P A 1 H3C H 0.6033 1.4148 0.1961 0.120 Uiso 0.5 1 calc R U P A 1 C4 C 0.5175(12) 1.0916(16) 0.1580(11) 0.083(3) Uani 0.5 1 d D U P A 1 H4A H 0.4781 1.0478 0.1094 0.124 Uiso 0.5 1 calc R U P A 1 H4B H 0.4680 1.1111 0.1877 0.124 Uiso 0.5 1 calc R U P A 1 H4C H 0.5743 1.0296 0.1872 0.124 Uiso 0.5 1 calc R U P A 1 C5 C 0.5072(13) 1.2979(18) 0.0668(10) 0.078(3) Uani 0.5 1 d D U P A 1 H5A H 0.5494 1.3767 0.0588 0.117 Uiso 0.5 1 calc R U P A 1 H5B H 0.4372 1.3299 0.0696 0.117 Uiso 0.5 1 calc R U P A 1 H5C H 0.4965 1.2333 0.0240 0.117 Uiso 0.5 1 calc R U P A 1 O1 O 0.6559(11) 1.004(2) 0.0391(12) 0.181(7) Uani 0.5 1 d D U P A 1 H1A H 0.6604 0.9215 0.0522 0.272 Uiso 0.5 1 calc R U P A 1 C4A C 0.4721(11) 1.0958(15) 0.1348(8) 0.063(2) Uani 0.5 1 d D U P B 2 H4AA H 0.4825 1.0718 0.1885 0.094 Uiso 0.5 1 calc R U P B 2 H4AB H 0.4952 1.0188 0.1088 0.094 Uiso 0.5 1 calc R U P B 2 H4AC H 0.3960 1.1152 0.1095 0.094 Uiso 0.5 1 calc R U P B 2 N1A N 0.5394(9) 1.2244(15) 0.1306(8) 0.063(2) Uani 0.5 1 d D U P B 2 C2A C 0.4955(12) 1.3371(16) 0.1728(7) 0.073(2) Uani 0.5 1 d D U P B 2 H2AA H 0.5223 1.4273 0.1611 0.088 Uiso 0.5 1 calc R U P B 2 H2AB H 0.4162 1.3384 0.1515 0.088 Uiso 0.5 1 calc R U P B 2 C3A C 0.5045(13) 1.2561(18) 0.0437(7) 0.057(3) Uani 0.5 1 d D U P B 2 H3AA H 0.4741 1.1730 0.0150 0.085 Uiso 0.5 1 calc R U P B 2 H3AB H 0.5671 1.2862 0.0287 0.085 Uiso 0.5 1 calc R U P B 2 H3AC H 0.4503 1.3292 0.0323 0.085 Uiso 0.5 1 calc R U P B 2 C5A C 0.6577(11) 1.1944(19) 0.1639(8) 0.066(3) Uani 0.5 1 d D U P B 2 H5AA H 0.6703 1.1456 0.2127 0.100 Uiso 0.5 1 calc R U P B 2 H5AB H 0.6980 1.2811 0.1725 0.100 Uiso 0.5 1 calc R U P B 2 H5AC H 0.6817 1.1370 0.1281 0.100 Uiso 0.5 1 calc R U P B 2 C1A C 0.5244(14) 1.3227(18) 0.2598(8) 0.086(3) Uani 0.5 1 d D U P B 2 H1AA H 0.5689 1.3868 0.2942 0.103 Uiso 0.5 1 calc R U P B 2 O1A O 0.4804(10) 1.2088(14) 0.2840(6) 0.093(3) Uani 0.5 1 d D U P B 2 H1AB H 0.5057 1.2012 0.3317 0.139 Uiso 0.5 1 calc R U P B 2 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 0.0133(3) 0.0726(6) 0.0202(3) -0.0002(3) 0.0069(3) 0.0006(3) Co2 0.0097(4) 0.0753(8) 0.0131(4) 0.0000(4) 0.0027(3) 0.0002(4) Cl1 0.0378(7) 0.1276(15) 0.0688(9) -0.0361(10) 0.0348(7) -0.0033(8) C11 0.0194(19) 0.066(3) 0.0206(19) -0.003(2) 0.0044(16) -0.004(2) C12 0.0157(19) 0.072(3) 0.025(2) 0.007(2) 0.0058(16) 0.002(2) C13 0.021(2) 0.071(3) 0.0196(19) 0.004(2) 0.0077(16) 0.001(2) C14 0.0175(19) 0.070(3) 0.0223(19) -0.005(2) 0.0036(16) -0.002(2) C15 0.0142(19) 0.092(4) 0.028(2) 0.000(2) 0.0056(17) -0.001(2) C16 0.020(2) 0.091(4) 0.023(2) 0.003(2) 0.0091(17) 0.000(2) C17 0.019(2) 0.073(4) 0.025(2) -0.002(2) 0.0052(16) -0.005(2) C18 0.0149(19) 0.071(3) 0.028(2) -0.003(2) 0.0032(16) -0.001(2) O11 0.0207(15) 0.092(3) 0.0264(15) 0.0130(17) 0.0071(12) 0.0046(17) O12 0.0396(18) 0.082(3) 0.0210(14) 0.0038(16) 0.0135(13) 0.0047(18) O13 0.0218(15) 0.082(3) 0.0256(15) 0.0012(16) 0.0045(12) 0.0046(16) O14 0.0138(14) 0.089(3) 0.0336(17) 0.0088(18) -0.0003(12) -0.0005(16) C21 0.0169(19) 0.070(3) 0.033(2) -0.002(2) 0.0086(17) -0.001(2) C22 0.018(2) 0.076(4) 0.040(3) 0.004(2) 0.0026(19) 0.000(2) C23 0.020(2) 0.078(4) 0.030(2) 0.005(2) 0.0040(18) 0.001(2) C24 0.020(2) 0.086(4) 0.042(3) 0.002(3) 0.012(2) -0.002(2) O21 0.0193(14) 0.073(2) 0.0242(14) 0.0015(15) 0.0106(12) 0.0023(15) O22 0.0173(17) 0.100(4) 0.108(4) 0.031(3) 0.005(2) -0.005(2) N1 0.037(4) 0.071(5) 0.097(6) 0.031(4) -0.016(3) -0.001(3) C1 0.053(5) 0.111(9) 0.151(10) -0.015(8) 0.001(5) -0.007(5) C2 0.037(4) 0.073(5) 0.091(6) 0.030(4) -0.017(3) -0.001(3) C3 0.042(5) 0.075(5) 0.101(6) 0.029(4) -0.012(4) -0.001(4) C4 0.048(5) 0.075(5) 0.104(7) 0.030(4) -0.010(4) -0.006(4) C5 0.035(5) 0.076(6) 0.099(6) 0.033(4) -0.016(4) -0.001(4) O1 0.061(7) 0.210(11) 0.233(11) -0.106(10) -0.018(7) 0.012(7) C4A 0.046(5) 0.089(5) 0.052(5) 0.025(3) 0.014(4) 0.002(4) N1A 0.048(4) 0.088(5) 0.053(4) 0.022(3) 0.017(3) 0.000(3) C2A 0.061(5) 0.096(5) 0.067(4) 0.015(3) 0.026(3) 0.001(4) C3A 0.038(5) 0.080(6) 0.054(3) 0.021(3) 0.019(3) 0.006(4) C5A 0.048(4) 0.095(6) 0.056(5) 0.021(4) 0.016(3) 0.002(4) C1A 0.079(7) 0.115(6) 0.066(4) 0.014(3) 0.028(3) -0.008(5) O1A 0.082(7) 0.124(7) 0.074(5) 0.022(4) 0.025(5) -0.012(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 O13 Co1 O11 111.07(17) 4_565 . ? O13 Co1 O21 112.87(13) 4_565 . ? O11 Co1 O21 100.86(14) . . ? O13 Co1 Cl1 111.57(11) 4_565 . ? O11 Co1 Cl1 102.25(11) . . ? O21 Co1 Cl1 117.02(12) . . ? O12 Co2 O12 180.0 3_765 . ? O12 Co2 O14 85.26(15) 3_765 4_565 ? O12 Co2 O14 94.74(15) . 4_565 ? O12 Co2 O14 94.74(15) 3_765 2_755 ? O12 Co2 O14 85.26(15) . 2_755 ? O14 Co2 O14 180.00(18) 4_565 2_755 ? O12 Co2 O21 87.94(13) 3_765 . ? O12 Co2 O21 92.06(13) . . ? O14 Co2 O21 90.85(13) 4_565 . ? O14 Co2 O21 89.15(13) 2_755 . ? O12 Co2 O21 92.06(13) 3_765 3_765 ? O12 Co2 O21 87.94(13) . 3_765 ? O14 Co2 O21 89.15(13) 4_565 3_765 ? O14 Co2 O21 90.85(13) 2_755 3_765 ? O21 Co2 O21 180.0 . 3_765 ? C12 C11 C16 119.6(4) . . ? C12 C11 C17 120.9(4) . . ? C16 C11 C17 119.5(4) . . ? C13 C12 C11 121.0(4) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C12 C13 C14 119.9(4) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C13 C14 C15 119.4(4) . . ? C13 C14 C18 120.0(4) . . ? C15 C14 C18 120.6(4) . . ? C16 C15 C14 120.7(4) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C11 119.3(4) . . ? C15 C16 H16 120.3 . . ? C11 C16 H16 120.3 . . ? O12 C17 O11 124.6(4) . . ? O12 C17 C11 118.8(4) . . ? O11 C17 C11 116.6(4) . . ? O14 C18 O13 125.7(4) . . ? O14 C18 C14 117.3(4) . . ? O13 C18 C14 117.0(4) . . ? C17 O11 Co1 122.6(3) . . ? C17 O12 Co2 137.6(4) . . ? C18 O13 Co1 119.1(3) . 4_666 ? C18 O14 Co2 143.4(3) . 2_745 ? C22 C21 C23 120.2(5) . 3_775 ? C22 C21 C24 120.0(4) . . ? C23 C21 C24 119.8(5) 3_775 . ? C21 C22 C23 120.2(5) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C21 119.6(5) . 3_775 ? C22 C23 H23 120.2 . . ? C21 C23 H23 120.2 3_775 . ? O22 C24 O21 122.2(6) . . ? O22 C24 C21 120.2(6) . . ? O21 C24 C21 117.5(4) . . ? C24 O21 Co1 106.8(3) . . ? C24 O21 Co2 120.4(3) . . ? Co1 O21 Co2 100.73(16) . . ? C3 N1 C4 109.1(14) . . ? C3 N1 C5 105.5(12) . . ? C4 N1 C5 115.7(11) . . ? C3 N1 C2 109.9(11) . . ? C4 N1 C2 108.0(12) . . ? C5 N1 C2 108.6(14) . . ? O1 C1 C2 133.7(15) . . ? O1 C1 H1 113.1 . . ? C2 C1 H1 113.1 . . ? C1 C2 N1 123.6(13) . . ? C1 C2 H2A 106.4 . . ? N1 C2 H2A 106.4 . . ? C1 C2 H2B 106.4 . . ? N1 C2 H2B 106.4 . . ? H2A C2 H2B 106.5 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C1 O1 H1A 109.5 . . ? N1A C4A H4AA 109.5 . . ? N1A C4A H4AB 109.5 . . ? H4AA C4A H4AB 109.5 . . ? N1A C4A H4AC 109.5 . . ? H4AA C4A H4AC 109.5 . . ? H4AB C4A H4AC 109.5 . . ? C5A N1A C3A 113.8(12) . . ? C5A N1A C4A 110.6(11) . . ? C3A N1A C4A 102.4(11) . . ? C5A N1A C2A 115.0(13) . . ? C3A N1A C2A 109.4(11) . . ? C4A N1A C2A 104.4(11) . . ? C1A C2A N1A 116.3(13) . . ? C1A C2A H2AA 108.2 . . ? N1A C2A H2AA 108.2 . . ? C1A C2A H2AB 108.2 . . ? N1A C2A H2AB 108.2 . . ? H2AA C2A H2AB 107.4 . . ? N1A C3A H3AA 109.5 . . ? N1A C3A H3AB 109.5 . . ? H3AA C3A H3AB 109.5 . . ? N1A C3A H3AC 109.5 . . ? H3AA C3A H3AC 109.5 . . ? H3AB C3A H3AC 109.5 . . ? N1A C5A H5AA 109.5 . . ? N1A C5A H5AB 109.5 . . ? H5AA C5A H5AB 109.5 . . ? N1A C5A H5AC 109.5 . . ? H5AA C5A H5AC 109.5 . . ? H5AB C5A H5AC 109.5 . . ? O1A C1A C2A 114.3(13) . . ? O1A C1A H1AA 122.8 . . ? C2A C1A H1AA 122.8 . . ? C1A O1A H1AB 109.5 . . ? 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 O13 1.949(3) 4_565 ? Co1 O11 1.975(3) . ? Co1 O21 1.994(3) . ? Co1 Cl1 2.2443(14) . ? Co2 O12 2.019(3) 3_765 ? Co2 O12 2.019(3) . ? Co2 O14 2.050(3) 4_565 ? Co2 O14 2.050(3) 2_755 ? Co2 O21 2.209(3) . ? Co2 O21 2.209(3) 3_765 ? C11 C12 1.386(6) . ? C11 C16 1.408(6) . ? C11 C17 1.480(6) . ? C12 C13 1.377(6) . ? C12 H12 0.9300 . ? C13 C14 1.397(6) . ? C13 H13 0.9300 . ? C14 C15 1.399(6) . ? C14 C18 1.489(6) . ? C15 C16 1.383(7) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O12 1.252(5) . ? C17 O11 1.277(6) . ? C18 O14 1.260(5) . ? C18 O13 1.276(6) . ? O13 Co1 1.949(3) 4_666 ? O14 Co2 2.050(3) 2_745 ? C21 C22 1.382(8) . ? C21 C23 1.392(6) 3_775 ? C21 C24 1.496(8) . ? C22 C23 1.383(8) . ? C22 H22 0.9300 . ? C23 C21 1.392(6) 3_775 ? C23 H23 0.9300 . ? C24 O22 1.237(6) . ? C24 O21 1.297(7) . ? N1 C3 1.502(19) . ? N1 C4 1.490(14) . ? N1 C5 1.502(16) . ? N1 C2 1.516(13) . ? C1 O1 1.260(13) . ? C1 C2 1.470(14) . ? C1 H1 0.9300 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? O1 H1A 0.8200 . ? C4A N1A 1.509(14) . ? C4A H4AA 0.9600 . ? C4A H4AB 0.9600 . ? C4A H4AC 0.9600 . ? N1A C5A 1.477(15) . ? N1A C3A 1.517(16) . ? N1A C2A 1.514(17) . ? C2A C1A 1.496(16) . ? C2A H2AA 0.9700 . ? C2A H2AB 0.9700 . ? C3A H3AA 0.9600 . ? C3A H3AB 0.9600 . ? C3A H3AC 0.9600 . ? C5A H5AA 0.9600 . ? C5A H5AB 0.9600 . ? C5A H5AC 0.9600 . ? C1A O1A 1.353(15) . ? C1A H1AA 0.9300 . ? O1A H1AB 0.8200 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 C11 C12 C13 2.0(8) . . . . ? C17 C11 C12 C13 -176.5(5) . . . . ? C11 C12 C13 C14 -0.1(8) . . . . ? C12 C13 C14 C15 -1.7(8) . . . . ? C12 C13 C14 C18 178.4(5) . . . . ? C13 C14 C15 C16 1.5(9) . . . . ? C18 C14 C15 C16 -178.6(5) . . . . ? C14 C15 C16 C11 0.5(9) . . . . ? C12 C11 C16 C15 -2.2(8) . . . . ? C17 C11 C16 C15 176.4(5) . . . . ? C12 C11 C17 O12 -171.9(5) . . . . ? C16 C11 C17 O12 9.6(8) . . . . ? C12 C11 C17 O11 9.7(8) . . . . ? C16 C11 C17 O11 -168.9(5) . . . . ? C13 C14 C18 O14 -175.0(5) . . . . ? C15 C14 C18 O14 5.1(8) . . . . ? C13 C14 C18 O13 5.8(8) . . . . ? C15 C14 C18 O13 -174.1(5) . . . . ? O12 C17 O11 Co1 -11.1(8) . . . . ? C11 C17 O11 Co1 167.2(3) . . . . ? O11 C17 O12 Co2 32.1(8) . . . . ? C11 C17 O12 Co2 -146.2(4) . . . . ? O14 C18 O13 Co1 -5.2(8) . . . 4_666 ? C14 C18 O13 Co1 173.9(4) . . . 4_666 ? O13 C18 O14 Co2 -0.1(11) . . . 2_745 ? C14 C18 O14 Co2 -179.2(4) . . . 2_745 ? C23 C21 C22 C23 0.3(9) 3_775 . . . ? C24 C21 C22 C23 -179.9(5) . . . . ? C21 C22 C23 C21 -0.3(9) . . . 3_775 ? C22 C21 C24 O22 -10.9(8) . . . . ? C23 C21 C24 O22 168.9(6) 3_775 . . . ? C22 C21 C24 O21 170.9(5) . . . . ? C23 C21 C24 O21 -9.3(7) 3_775 . . . ? O22 C24 O21 Co1 -13.0(7) . . . . ? C21 C24 O21 Co1 165.2(4) . . . . ? O22 C24 O21 Co2 100.7(6) . . . . ? C21 C24 O21 Co2 -81.1(5) . . . . ? O1 C1 C2 N1 18(4) . . . . ? C3 N1 C2 C1 168.4(16) . . . . ? C4 N1 C2 C1 50(2) . . . . ? C5 N1 C2 C1 -76.6(19) . . . . ? C5A N1A C2A C1A -49.5(16) . . . . ? C3A N1A C2A C1A -179.0(12) . . . . ? C4A N1A C2A C1A 72.0(15) . . . . ? N1A C2A C1A O1A -65.6(18) . . . . ?