#------------------------------------------------------------------------------ #$Date: 2021-11-09 03:32:05 +0200 (Tue, 09 Nov 2021) $ #$Revision: 270538 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/10/7061059.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_7061059 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_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/D1NJ04480J _journal_year 2021 _chemical_formula_sum 'C48 H60 Co3 N6 O20' _chemical_formula_weight 1217.81 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _audit_block_doi 10.5517/ccdc.csd.cc28stc8 _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2021-10-19 deposited with the CCDC. 2021-10-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.6060(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 32.8455(2) _cell_length_b 9.70870(10) _cell_length_c 18.40350(10) _cell_measurement_reflns_used 21138 _cell_measurement_temperature 179.99(10) _cell_measurement_theta_max 75.8790 _cell_measurement_theta_min 2.6830 _cell_volume 5857.02(8) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 179.99(10) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.980 _diffrn_measurement_device_type 'XtaLAB Synergy R, HyPix' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_unetI/netI 0.0211 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.980 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 32618 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.980 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.577 _diffrn_reflns_theta_min 1.242 _exptl_absorpt_coefficient_mu 0.914 _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.381 _exptl_crystal_description block _exptl_crystal_F_000 2524 _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _refine_diff_density_max 1.369 _refine_diff_density_min -0.763 _refine_diff_density_rms 0.170 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 350 _refine_ls_number_reflns 6002 _refine_ls_number_restraints 77 _refine_ls_restrained_S_all 1.134 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0805 _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^)+(0.1260P)^2^+58.7195P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2371 _refine_ls_wR_factor_ref 0.2399 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5676 _reflns_number_total 6002 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1nj04480j2.cif _cod_data_source_block 15 _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 7061059 _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 ; 15.res created by SHELXL-2014/7 TITL 15 in C2/c CELL 0.71073 32.8455 9.7087 18.4035 90.000 93.606 90.000 ZERR 4.00 0.0002 0.0001 0.0001 0.000 0.001 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O CO UNIT 192 240 24 80 12 acta L.S. 10 BOND FMAP 2 PLAN 10 BOND CONF bond $h delu 0.01 0.005 n3 c6 c7 c8 n3 c4 DFIX 1.45 N3 C7 N3 C4 N3 C5 N3 C6 C7 C8 C8 O2 DFIX 2.4 C4 C5 C6 C4 C7 C4 C7 C5 C7 C6 DFIX 1.45 C1 N1 C1 N2 C3 N2 C2 N1 ISOR 0.02 0.01 N2 ISOR 0.02 0.01 C2 ISOR 0.02 0.01 C3 ISOR 0.02 0.01 O2 ISOR 0.005 0.0025 N3 ISOR 0.02 0.01 C4 ISOR 0.02 0.01 C5 ISOR 0.01 0.005 C7 ISOR 0.02 0.01 C8 L.S. 100 PLAN 5 CONF acta BOND FMAP 2 bond $h MORE -1 OMIT -3 1 1 OMIT 3 1 2 OMIT -3 1 3 OMIT 7 1 0 OMIT 13 5 0 OMIT 0 2 3 OMIT -15 7 3 OMIT 1 1 5 OMIT -14 6 9 OMIT 31 1 7 OMIT -6 0 2 OMIT -23 3 3 OMIT -9 1 6 OMIT 30 0 8 OMIT -9 1 5 OMIT 2 0 4 OMIT -7 1 5 OMIT -32 0 2 OMIT -2 2 4 OMIT 4 0 6 OMIT 2 4 3 OMIT -3 3 2 OMIT 4 0 2 OMIT -2 0 2 OMIT 8 0 6 OMIT 6 0 6 OMIT 6 4 2 WGHT 0.126000 58.719498 FVAR 0.05149 0.05221 CO1 5 0.152662 0.796472 0.483449 11.00000 0.02323 0.02706 = 0.02620 -0.00030 0.00528 0.00218 CO2 5 0.250000 0.750000 0.500000 10.50000 0.02222 0.02176 = 0.02298 0.00079 0.00469 0.00048 O11 4 0.153050 0.702034 0.579381 11.00000 0.02395 0.04179 = 0.02698 0.01546 0.00785 0.00544 O12 4 0.214472 0.619298 0.557339 11.00000 0.02645 0.02022 = 0.02356 0.00510 0.01101 -0.00113 O13 4 0.158357 0.325604 0.900066 11.00000 0.02150 0.03405 = 0.02663 0.01178 0.00516 -0.00057 O14 4 0.226740 0.320096 0.900562 11.00000 0.02120 0.02869 = 0.01820 0.00479 0.00089 -0.00179 C11 1 0.186434 0.559135 0.667997 11.00000 0.02188 0.02581 = 0.02073 0.00775 0.00422 -0.00184 C12 1 0.151175 0.541102 0.704744 11.00000 0.02166 0.04760 = 0.02823 0.01667 0.00614 0.00436 AFIX 43 H12A 2 0.126369 0.574729 0.685026 11.00000 -1.20000 AFIX 0 C13 1 0.153160 0.472421 0.771255 11.00000 0.01964 0.04979 = 0.02965 0.01725 0.00873 0.00248 AFIX 43 H13A 2 0.129511 0.458966 0.795597 11.00000 -1.20000 AFIX 0 C14 1 0.190048 0.424065 0.801381 11.00000 0.02219 0.02646 = 0.02313 0.00560 0.00373 -0.00109 C15 1 0.225404 0.443856 0.764789 11.00000 0.02088 0.04320 = 0.02500 0.01020 0.00444 0.00323 AFIX 43 H15A 2 0.250313 0.412760 0.785363 11.00000 -1.20000 AFIX 0 C16 1 0.223674 0.509435 0.698093 11.00000 0.02133 0.04066 = 0.02525 0.01018 0.00856 0.00178 AFIX 43 H16A 2 0.247257 0.520487 0.673261 11.00000 -1.20000 AFIX 0 C17 1 0.184749 0.631645 0.596206 11.00000 0.02403 0.02229 = 0.02217 0.00602 0.00446 -0.00504 C18 1 0.192382 0.350685 0.873358 11.00000 0.02320 0.02143 = 0.02087 0.00204 0.00407 -0.00130 O21 4 0.203607 0.907687 0.502321 11.00000 0.01817 0.01317 = 0.02865 0.00120 0.00495 0.00217 O22 4 0.183216 1.006338 0.396805 11.00000 0.04033 0.02585 = 0.03672 0.00503 -0.01246 -0.00392 C21 1 0.228038 1.132297 0.478312 11.00000 0.02511 0.01387 = 0.02882 0.00051 0.00134 0.00170 C22 1 0.246103 1.142175 0.548548 11.00000 0.03249 0.01490 = 0.02763 0.00348 0.00374 -0.00026 AFIX 43 H22A 2 0.243747 1.069637 0.581020 11.00000 -1.20000 AFIX 0 C23 1 0.232553 1.241303 0.429726 11.00000 0.03311 0.02054 = 0.02689 0.00186 -0.00036 -0.00105 AFIX 43 H23A 2 0.221041 1.234992 0.382367 11.00000 -1.20000 AFIX 0 C24 1 0.203613 1.009404 0.455558 11.00000 0.02122 0.01633 = 0.03406 0.00085 0.00350 0.00318 O31 4 0.108690 0.936560 0.486355 11.00000 0.02474 0.05632 = 0.06753 0.01467 0.01038 0.01888 O32 4 0.078214 0.737623 0.472221 11.00000 0.04286 0.05650 = 0.07970 -0.02097 -0.00308 0.02442 C31 1 0.036652 0.933863 0.490392 11.00000 0.02373 0.05010 = 0.03405 -0.00196 0.00112 0.01457 C32 1 0.035375 1.074974 0.499617 11.00000 0.02213 0.04603 = 0.07398 0.00134 0.00363 0.00703 AFIX 43 H32A 2 0.059264 1.126313 0.499212 11.00000 -1.20000 AFIX 0 C33 1 0.001403 0.859694 0.490523 11.00000 0.03046 0.04233 = 0.07556 -0.00845 -0.00096 0.01195 AFIX 43 H33A 2 0.002036 0.764756 0.483963 11.00000 -1.20000 AFIX 0 C34 1 0.076702 0.862364 0.482093 11.00000 0.03295 0.05811 = 0.03203 0.00364 0.00484 0.01956 N3 3 0.112672 2.012410 0.236073 11.00000 0.12937 0.11351 = 0.11102 0.02139 -0.03069 -0.00717 C7 1 0.105430 1.887993 0.275197 11.00000 0.16109 0.15430 = 0.12437 0.05014 -0.03169 -0.01739 AFIX 23 H7A 2 0.119761 1.814727 0.251655 11.00000 -1.20000 H7B 2 0.118541 1.898656 0.323584 11.00000 -1.20000 AFIX 0 C5 1 0.084412 2.041837 0.174850 11.00000 0.15720 0.15460 = 0.11423 0.02590 -0.04086 0.00022 AFIX 33 H5A 2 0.057067 2.024699 0.188118 11.00000 -1.50000 H5B 2 0.087000 2.136634 0.161039 11.00000 -1.50000 H5C 2 0.090364 1.983762 0.134653 11.00000 -1.50000 AFIX 0 C4 1 0.153559 2.035128 0.220856 11.00000 0.17698 0.22009 = 0.18581 0.05383 0.01246 -0.02840 AFIX 33 H4A 2 0.155631 2.120145 0.194709 11.00000 -1.50000 H4B 2 0.170118 2.040074 0.265660 11.00000 -1.50000 H4C 2 0.162838 1.960673 0.191813 11.00000 -1.50000 AFIX 0 C6 1 0.103382 2.119346 0.299018 11.00000 0.25109 0.21046 = 0.24002 -0.05919 -0.06869 0.13356 AFIX 33 H6A 2 0.075668 2.108550 0.311775 11.00000 -1.50000 H6B 2 0.121498 2.102128 0.341018 11.00000 -1.50000 H6C 2 0.107403 2.211555 0.282048 11.00000 -1.50000 AFIX 0 O2 4 0.034906 1.790563 0.226301 11.00000 0.31008 0.32299 = 0.30792 -0.00540 0.02864 -0.00171 AFIX 83 H2A 2 0.012071 1.790591 0.241929 11.00000 -1.50000 AFIX 0 C8 1 0.065116 1.840179 0.284004 11.00000 0.24433 0.27618 = 0.27446 0.05365 0.05432 -0.09767 AFIX 23 H8A 2 0.051614 1.914384 0.308320 11.00000 -1.20000 H8B 2 0.068016 1.765627 0.319037 11.00000 -1.20000 AFIX 0 O1 4 0.076086 1.677410 0.115979 11.00000 0.17247 0.11689 = 0.18385 -0.01162 -0.01248 0.04245 N1 3 0.107220 1.585803 0.019963 11.00000 0.10611 0.22063 = 0.19837 0.08187 0.05769 0.06079 AFIX 43 H1A 2 0.102599 1.521482 -0.011614 11.00000 -1.20000 AFIX 0 C1 1 0.078191 1.585564 0.071920 11.00000 0.11088 0.06798 = 0.19672 0.01064 -0.03553 0.00973 C2 1 0.140539 1.659211 0.005660 11.00000 0.13252 0.13043 = 0.17098 0.03753 0.01008 0.00168 AFIX 33 H2B 2 0.151986 1.623266 -0.037167 11.00000 -1.50000 H2C 2 0.133068 1.753879 -0.002237 11.00000 -1.50000 H2D 2 0.160333 1.652854 0.046181 11.00000 -1.50000 AFIX 0 N2 3 0.050391 1.471204 0.078397 11.00000 0.17494 0.20124 = 0.21168 -0.03852 0.02240 -0.01868 AFIX 43 H2E 2 0.052620 1.401441 0.050125 11.00000 -1.20000 AFIX 0 C3 1 0.018004 1.468583 0.131866 11.00000 0.27454 0.27899 = 0.26999 0.00159 0.02598 -0.00902 AFIX 33 H3A 2 0.003108 1.383662 0.127024 11.00000 -1.50000 H3B 2 0.030394 1.475865 0.180366 11.00000 -1.50000 H3C 2 -0.000301 1.544536 0.122565 11.00000 -1.50000 AFIX 0 HKLF 4 REM 15 in C2/c REM R1 = 0.0805 for 5676 Fo > 4sig(Fo) and 0.0834 for all 6002 data REM 350 parameters refined using 77 restraints END WGHT 0.1384 55.2577 REM Highest difference peak 1.369, deepest hole -0.763, 1-sigma level 0.170 Q1 1 0.1360 2.1362 0.2525 11.00000 0.05 1.37 Q2 1 0.0524 1.6115 0.3304 11.00000 0.05 1.25 Q3 1 0.0779 2.2359 0.3394 11.00000 0.05 1.18 Q4 1 0.0000 2.1885 0.2500 10.50000 0.05 1.12 Q5 1 0.1253 1.9724 0.2167 11.00000 0.05 1.08 ; _shelx_res_checksum 68126 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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 0.15266(2) 0.79647(7) 0.48345(3) 0.0253(2) Uani 1 1 d . . . . . Co2 Co 0.2500 0.7500 0.5000 0.0222(2) Uani 1 2 d S . P . . O11 O 0.15305(10) 0.7020(4) 0.57938(19) 0.0306(8) Uani 1 1 d . . . . . O12 O 0.21447(9) 0.6193(3) 0.55734(17) 0.0230(6) Uani 1 1 d . . . . . O13 O 0.15836(10) 0.3256(4) 0.90007(18) 0.0272(7) Uani 1 1 d . . . . . O14 O 0.22674(9) 0.3201(3) 0.90056(16) 0.0227(6) Uani 1 1 d . . . . . C11 C 0.18643(13) 0.5591(5) 0.6680(2) 0.0227(9) Uani 1 1 d . . . . . C12 C 0.15117(14) 0.5411(6) 0.7047(3) 0.0323(11) Uani 1 1 d . . . . . H12A H 0.1264 0.5747 0.6850 0.039 Uiso 1 1 calc R U . . . C13 C 0.15316(14) 0.4724(6) 0.7713(3) 0.0327(11) Uani 1 1 d . . . . . H13A H 0.1295 0.4590 0.7956 0.039 Uiso 1 1 calc R U . . . C14 C 0.19005(13) 0.4241(5) 0.8014(2) 0.0238(9) Uani 1 1 d . . . . . C15 C 0.22540(14) 0.4439(6) 0.7648(3) 0.0296(10) Uani 1 1 d . . . . . H15A H 0.2503 0.4128 0.7854 0.035 Uiso 1 1 calc R U . . . C16 C 0.22367(14) 0.5094(5) 0.6981(3) 0.0288(10) Uani 1 1 d . . . . . H16A H 0.2473 0.5205 0.6733 0.035 Uiso 1 1 calc R U . . . C17 C 0.18475(13) 0.6316(5) 0.5962(2) 0.0227(9) Uani 1 1 d . . . . . C18 C 0.19238(13) 0.3507(5) 0.8734(2) 0.0217(8) Uani 1 1 d . . . . . O21 O 0.20361(9) 0.9077(3) 0.50232(17) 0.0198(6) Uani 1 1 d . . . . . O22 O 0.18322(12) 1.0063(4) 0.3968(2) 0.0349(8) Uani 1 1 d . . . . . C21 C 0.22804(13) 1.1323(4) 0.4783(2) 0.0226(9) Uani 1 1 d . . . . . C22 C 0.24610(14) 1.1422(5) 0.5485(2) 0.0249(9) Uani 1 1 d . . . . . H22A H 0.2437 1.0696 0.5810 0.030 Uiso 1 1 calc R U . . . C23 C 0.23255(15) 1.2413(5) 0.4297(3) 0.0269(9) Uani 1 1 d . . . . . H23A H 0.2210 1.2350 0.3824 0.032 Uiso 1 1 calc R U . . . C24 C 0.20361(13) 1.0094(4) 0.4556(3) 0.0238(9) Uani 1 1 d . . . . . O31 O 0.10869(12) 0.9366(5) 0.4864(3) 0.0492(11) Uani 1 1 d . . . . . O32 O 0.07821(15) 0.7376(5) 0.4722(3) 0.0600(14) Uani 1 1 d . . . . . C31 C 0.03665(15) 0.9339(6) 0.4904(3) 0.0360(12) Uani 1 1 d . . . . . C32 C 0.03537(17) 1.0750(7) 0.4996(4) 0.0474(15) Uani 1 1 d . . . . . H32A H 0.0593 1.1263 0.4992 0.057 Uiso 1 1 calc R U . . . C33 C 0.00140(18) 0.8597(7) 0.4905(4) 0.0496(15) Uani 1 1 d . . . . . H33A H 0.0020 0.7648 0.4840 0.060 Uiso 1 1 calc R U . . . C34 C 0.07670(17) 0.8624(7) 0.4821(3) 0.0409(13) Uani 1 1 d . . . . . N3 N 0.1127(3) 2.0124(12) 0.2361(6) 0.120(3) Uani 1 1 d D U . . . C7 C 0.1054(5) 1.8880(15) 0.2752(8) 0.148(5) Uani 1 1 d D U . . . H7A H 0.1198 1.8147 0.2517 0.178 Uiso 1 1 calc R U . . . H7B H 0.1185 1.8987 0.3236 0.178 Uiso 1 1 calc R U . . . C5 C 0.0844(4) 2.0418(17) 0.1749(8) 0.144(5) Uani 1 1 d D U . . . H5A H 0.0571 2.0247 0.1881 0.216 Uiso 1 1 calc R U . . . H5B H 0.0870 2.1366 0.1610 0.216 Uiso 1 1 calc R U . . . H5C H 0.0904 1.9838 0.1347 0.216 Uiso 1 1 calc R U . . . C4 C 0.1536(4) 2.035(2) 0.2209(10) 0.194(7) Uani 1 1 d D U . . . H4A H 0.1556 2.1201 0.1947 0.291 Uiso 1 1 calc R U . . . H4B H 0.1701 2.0401 0.2657 0.291 Uiso 1 1 calc R U . . . H4C H 0.1628 1.9607 0.1918 0.291 Uiso 1 1 calc R U . . . C6 C 0.1034(6) 2.1193(19) 0.2990(11) 0.237(11) Uani 1 1 d D U . . . H6A H 0.0757 2.1086 0.3118 0.356 Uiso 1 1 calc R U . . . H6B H 0.1215 2.1021 0.3410 0.356 Uiso 1 1 calc R U . . . H6C H 0.1074 2.2116 0.2820 0.356 Uiso 1 1 calc R U . . . O2 O 0.0349(7) 1.791(3) 0.2263(13) 0.313(12) Uani 1 1 d D U . . . H2A H 0.0121 1.7906 0.2419 0.470 Uiso 1 1 calc R U . . . C8 C 0.0651(7) 1.840(3) 0.2840(16) 0.263(13) Uani 1 1 d D U . . . H8A H 0.0516 1.9144 0.3083 0.316 Uiso 1 1 calc R U . . . H8B H 0.0680 1.7656 0.3190 0.316 Uiso 1 1 calc R U . . . O1 O 0.0761(4) 1.6774(12) 0.1160(8) 0.159(5) Uani 1 1 d . . . . . N1 N 0.1072(4) 1.5858(18) 0.0200(9) 0.173(7) Uani 1 1 d D . . . . H1A H 0.1026 1.5215 -0.0116 0.208 Uiso 1 1 calc R U . . . C1 C 0.0782(4) 1.5856(14) 0.0719(10) 0.127(6) Uani 1 1 d D . . . . C2 C 0.1405(5) 1.6592(17) 0.0057(11) 0.145(6) Uani 1 1 d D U . . . H2B H 0.1520 1.6233 -0.0372 0.217 Uiso 1 1 calc R U . . . H2C H 0.1331 1.7539 -0.0022 0.217 Uiso 1 1 calc R U . . . H2D H 0.1603 1.6529 0.0462 0.217 Uiso 1 1 calc R U . . . N2 N 0.0504(5) 1.471(2) 0.0784(11) 0.196(7) Uani 1 1 d D U . . . H2E H 0.0526 1.4014 0.0501 0.235 Uiso 1 1 calc R U . . . C3 C 0.0180(9) 1.469(3) 0.1319(16) 0.274(15) Uani 1 1 d D U . . . H3A H 0.0031 1.3837 0.1270 0.411 Uiso 1 1 calc R U . . . H3B H 0.0304 1.4759 0.1804 0.411 Uiso 1 1 calc R U . . . H3C H -0.0003 1.5445 0.1226 0.411 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0232(4) 0.0271(4) 0.0262(4) -0.0003(2) 0.0053(2) 0.0022(2) Co2 0.0222(4) 0.0218(5) 0.0230(4) 0.0008(3) 0.0047(3) 0.0005(3) O11 0.0239(16) 0.042(2) 0.0270(17) 0.0155(15) 0.0078(13) 0.0054(14) O12 0.0265(16) 0.0202(15) 0.0236(15) 0.0051(12) 0.0110(12) -0.0011(12) O13 0.0215(15) 0.0341(18) 0.0266(16) 0.0118(14) 0.0052(12) -0.0006(13) O14 0.0212(15) 0.0287(16) 0.0182(14) 0.0048(12) 0.0009(11) -0.0018(12) C11 0.022(2) 0.026(2) 0.021(2) 0.0078(17) 0.0042(16) -0.0018(17) C12 0.022(2) 0.048(3) 0.028(2) 0.017(2) 0.0061(18) 0.004(2) C13 0.020(2) 0.050(3) 0.030(2) 0.017(2) 0.0087(18) 0.002(2) C14 0.022(2) 0.026(2) 0.023(2) 0.0056(17) 0.0037(16) -0.0011(17) C15 0.021(2) 0.043(3) 0.025(2) 0.010(2) 0.0044(17) 0.0032(19) C16 0.021(2) 0.041(3) 0.025(2) 0.010(2) 0.0086(17) 0.0018(19) C17 0.024(2) 0.022(2) 0.022(2) 0.0060(16) 0.0045(16) -0.0050(16) C18 0.023(2) 0.021(2) 0.021(2) 0.0020(16) 0.0041(16) -0.0013(16) O21 0.0182(14) 0.0132(13) 0.0286(15) 0.0012(11) 0.0050(11) 0.0022(11) O22 0.040(2) 0.0259(18) 0.0367(19) 0.0050(14) -0.0125(16) -0.0039(15) C21 0.025(2) 0.0139(19) 0.029(2) 0.0005(16) 0.0013(17) 0.0017(16) C22 0.032(2) 0.015(2) 0.028(2) 0.0035(16) 0.0037(18) -0.0003(17) C23 0.033(2) 0.021(2) 0.027(2) 0.0019(18) -0.0004(18) -0.0010(18) C24 0.021(2) 0.016(2) 0.034(2) 0.0008(17) 0.0035(17) 0.0032(16) O31 0.0247(19) 0.056(3) 0.068(3) 0.015(2) 0.0104(18) 0.0189(18) O32 0.043(3) 0.057(3) 0.080(3) -0.021(3) -0.003(2) 0.024(2) C31 0.024(2) 0.050(3) 0.034(3) -0.002(2) 0.0011(19) 0.015(2) C32 0.022(2) 0.046(3) 0.074(4) 0.001(3) 0.004(3) 0.007(2) C33 0.030(3) 0.042(3) 0.076(4) -0.008(3) -0.001(3) 0.012(2) C34 0.033(3) 0.058(4) 0.032(3) 0.004(2) 0.005(2) 0.020(3) N3 0.129(5) 0.114(5) 0.111(5) 0.021(4) -0.031(4) -0.007(4) C7 0.161(8) 0.154(8) 0.124(8) 0.050(7) -0.032(7) -0.017(7) C5 0.157(9) 0.155(9) 0.114(8) 0.026(7) -0.041(7) 0.000(8) C4 0.177(9) 0.220(11) 0.186(10) 0.054(8) 0.012(8) -0.028(8) C6 0.25(2) 0.210(13) 0.24(2) -0.059(17) -0.069(14) 0.134(18) O2 0.310(14) 0.323(14) 0.308(14) -0.005(9) 0.029(9) -0.002(9) C8 0.244(15) 0.276(19) 0.27(2) 0.054(16) 0.054(16) -0.098(15) O1 0.172(11) 0.117(8) 0.184(12) -0.012(8) -0.012(9) 0.042(8) N1 0.106(9) 0.221(17) 0.198(15) 0.082(13) 0.058(10) 0.061(10) C1 0.111(10) 0.068(7) 0.197(17) 0.011(9) -0.036(11) 0.010(7) C2 0.133(9) 0.130(9) 0.171(10) 0.038(8) 0.010(8) 0.002(7) N2 0.175(13) 0.201(14) 0.212(14) -0.039(12) 0.022(11) -0.019(12) C3 0.275(17) 0.279(17) 0.270(17) 0.002(10) 0.026(10) -0.009(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O13 Co1 O31 122.76(18) 6_565 . ? O13 Co1 O11 114.91(16) 6_565 . ? O31 Co1 O11 104.82(17) . . ? O13 Co1 O21 110.02(13) 6_565 . ? O31 Co1 O21 103.12(16) . . ? O11 Co1 O21 97.81(14) . . ? O14 Co2 O14 180.0 6_565 4_556 ? O14 Co2 O12 86.48(13) 6_565 7_566 ? O14 Co2 O12 93.52(13) 4_556 7_566 ? O14 Co2 O12 93.52(13) 6_565 . ? O14 Co2 O12 86.48(13) 4_556 . ? O12 Co2 O12 180.00(14) 7_566 . ? O14 Co2 O21 88.33(12) 6_565 7_566 ? O14 Co2 O21 91.67(12) 4_556 7_566 ? O12 Co2 O21 90.20(12) 7_566 7_566 ? O12 Co2 O21 89.80(12) . 7_566 ? O14 Co2 O21 91.67(12) 6_565 . ? O14 Co2 O21 88.33(12) 4_556 . ? O12 Co2 O21 89.81(12) 7_566 . ? O12 Co2 O21 90.20(12) . . ? O21 Co2 O21 180.0 7_566 . ? C17 O11 Co1 115.1(3) . . ? C17 O12 Co2 136.2(3) . . ? C18 O13 Co1 123.3(3) . 6_566 ? C18 O14 Co2 135.7(3) . 4_546 ? C12 C11 C16 120.0(4) . . ? C12 C11 C17 120.3(4) . . ? C16 C11 C17 119.7(4) . . ? C11 C12 C13 119.6(4) . . ? C11 C12 H12A 120.2 . . ? C13 C12 H12A 120.2 . . ? C14 C13 C12 120.5(4) . . ? C14 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? C13 C14 C15 119.7(4) . . ? C13 C14 C18 120.6(4) . . ? C15 C14 C18 119.6(4) . . ? C16 C15 C14 120.3(4) . . ? C16 C15 H15A 119.8 . . ? C14 C15 H15A 119.8 . . ? C15 C16 C11 119.9(4) . . ? C15 C16 H16A 120.1 . . ? C11 C16 H16A 120.1 . . ? O12 C17 O11 124.8(4) . . ? O12 C17 C11 118.2(4) . . ? O11 C17 C11 117.0(4) . . ? O14 C18 O13 126.6(4) . . ? O14 C18 C14 117.6(4) . . ? O13 C18 C14 115.7(4) . . ? C24 O21 Co1 109.1(3) . . ? C24 O21 Co2 119.4(3) . . ? Co1 O21 Co2 101.36(12) . . ? C22 C21 C23 119.0(4) . . ? C22 C21 C24 120.6(4) . . ? C23 C21 C24 120.3(4) . . ? C23 C22 C21 120.4(4) 7_576 . ? C23 C22 H22A 119.8 7_576 . ? C21 C22 H22A 119.8 . . ? C22 C23 C21 120.6(5) 7_576 . ? C22 C23 H23A 119.7 7_576 . ? C21 C23 H23A 119.7 . . ? O22 C24 O21 122.3(4) . . ? O22 C24 C21 121.3(4) . . ? O21 C24 C21 116.3(4) . . ? C34 O31 Co1 102.1(4) . . ? C33 C31 C32 119.4(5) . . ? C33 C31 C34 120.3(6) . . ? C32 C31 C34 120.3(5) . . ? C31 C32 C33 120.2(6) . 5_576 ? C31 C32 H32A 119.9 . . ? C33 C32 H32A 119.9 5_576 . ? C31 C33 C32 120.4(6) . 5_576 ? C31 C33 H33A 119.8 . . ? C32 C33 H33A 119.8 5_576 . ? O32 C34 O31 121.8(5) . . ? O32 C34 C31 121.0(6) . . ? O31 C34 C31 117.2(6) . . ? C4 N3 C7 115.0(11) . . ? C4 N3 C5 112.9(11) . . ? C7 N3 C5 116.1(10) . . ? C4 N3 C6 105.7(11) . . ? C7 N3 C6 97.9(10) . . ? C5 N3 C6 107.1(13) . . ? C8 C7 N3 121.2(17) . . ? C8 C7 H7A 107.0 . . ? N3 C7 H7A 107.0 . . ? C8 C7 H7B 107.0 . . ? N3 C7 H7B 107.0 . . ? H7A C7 H7B 106.8 . . ? N3 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C4 H4A 109.5 . . ? N3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C6 H6A 109.5 . . ? N3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 O2 H2A 109.5 . . ? C7 C8 O2 127(2) . . ? C7 C8 H8A 105.4 . . ? O2 C8 H8A 105.4 . . ? C7 C8 H8B 105.4 . . ? O2 C8 H8B 105.4 . . ? H8A C8 H8B 106.0 . . ? C2 N1 C1 137.4(19) . . ? C2 N1 H1A 111.3 . . ? C1 N1 H1A 111.3 . . ? O1 C1 N1 122.0(16) . . ? O1 C1 N2 116.6(17) . . ? N1 C1 N2 121.4(16) . . ? N1 C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C2 H2D 109.5 . . ? H2B C2 H2D 109.5 . . ? H2C C2 H2D 109.5 . . ? C1 N2 C3 123(2) . . ? C1 N2 H2E 118.4 . . ? C3 N2 H2E 118.4 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 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 1.957(3) 6_565 ? Co1 O31 1.987(4) . ? Co1 O11 1.989(3) . ? Co1 O21 2.003(3) . ? Co2 O14 2.054(3) 6_565 ? Co2 O14 2.054(3) 4_556 ? Co2 O12 2.059(3) 7_566 ? Co2 O12 2.059(3) . ? Co2 O21 2.162(3) 7_566 ? Co2 O21 2.162(3) . ? O11 C17 1.267(6) . ? O12 C17 1.252(5) . ? O13 C18 1.272(5) . ? O13 Co1 1.957(3) 6_566 ? O14 C18 1.242(5) . ? O14 Co2 2.054(3) 4_546 ? C11 C12 1.388(6) . ? C11 C16 1.397(6) . ? C11 C17 1.495(6) . ? C12 C13 1.392(7) . ? C12 H12A 0.9300 . ? C13 C14 1.382(6) . ? C13 H13A 0.9300 . ? C14 C15 1.392(6) . ? C14 C18 1.502(6) . ? C15 C16 1.381(6) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? O21 C24 1.310(5) . ? O22 C24 1.236(6) . ? C21 C22 1.391(6) . ? C21 C23 1.399(6) . ? C21 C24 1.483(6) . ? C22 C23 1.377(7) 7_576 ? C22 H22A 0.9300 . ? C23 C22 1.377(7) 7_576 ? C23 H23A 0.9300 . ? O31 C34 1.272(8) . ? O32 C34 1.226(8) . ? C31 C33 1.364(9) . ? C31 C32 1.381(9) . ? C31 C34 1.504(7) . ? C32 C33 1.386(8) 5_576 ? C32 H32A 0.9300 . ? C33 C32 1.386(8) 5_576 ? C33 H33A 0.9300 . ? N3 C4 1.406(13) . ? N3 C7 1.434(12) . ? N3 C5 1.443(11) . ? N3 C6 1.599(14) . ? C7 C8 1.422(16) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? O2 C8 1.487(18) . ? O2 H2A 0.8200 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? O1 C1 1.210(18) . ? N1 C2 1.346(14) . ? N1 C1 1.392(15) . ? N1 H1A 0.8600 . ? C1 N2 1.447(15) . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C2 H2D 0.9600 . ? N2 C3 1.494(17) . ? N2 H2E 0.8600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? 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 -0.5(8) . . . . ? C17 C11 C12 C13 179.5(5) . . . . ? C11 C12 C13 C14 1.0(9) . . . . ? C12 C13 C14 C15 -0.2(9) . . . . ? C12 C13 C14 C18 179.6(5) . . . . ? C13 C14 C15 C16 -1.1(8) . . . . ? C18 C14 C15 C16 179.1(5) . . . . ? C14 C15 C16 C11 1.6(8) . . . . ? C12 C11 C16 C15 -0.8(8) . . . . ? C17 C11 C16 C15 179.2(5) . . . . ? Co2 O12 C17 O11 47.4(7) . . . . ? Co2 O12 C17 C11 -132.4(4) . . . . ? Co1 O11 C17 O12 0.1(6) . . . . ? Co1 O11 C17 C11 179.8(3) . . . . ? C12 C11 C17 O12 -164.2(5) . . . . ? C16 C11 C17 O12 15.8(7) . . . . ? C12 C11 C17 O11 16.1(7) . . . . ? C16 C11 C17 O11 -163.9(5) . . . . ? Co2 O14 C18 O13 -11.7(8) 4_546 . . . ? Co2 O14 C18 C14 168.7(3) 4_546 . . . ? Co1 O13 C18 O14 -10.9(7) 6_566 . . . ? Co1 O13 C18 C14 168.7(3) 6_566 . . . ? C13 C14 C18 O14 -174.0(5) . . . . ? C15 C14 C18 O14 5.8(7) . . . . ? C13 C14 C18 O13 6.4(7) . . . . ? C15 C14 C18 O13 -173.8(5) . . . . ? C23 C21 C22 C23 1.2(8) . . . 7_576 ? C24 C21 C22 C23 -177.5(4) . . . 7_576 ? C22 C21 C23 C22 -1.2(8) . . . 7_576 ? C24 C21 C23 C22 177.5(4) . . . 7_576 ? Co1 O21 C24 O22 -22.1(5) . . . . ? Co2 O21 C24 O22 93.7(5) . . . . ? Co1 O21 C24 C21 155.1(3) . . . . ? Co2 O21 C24 C21 -89.1(4) . . . . ? C22 C21 C24 O22 170.8(4) . . . . ? C23 C21 C24 O22 -7.9(7) . . . . ? C22 C21 C24 O21 -6.5(6) . . . . ? C23 C21 C24 O21 174.8(4) . . . . ? C33 C31 C32 C33 0.5(12) . . . 5_576 ? C34 C31 C32 C33 -178.0(6) . . . 5_576 ? C32 C31 C33 C32 -0.5(12) . . . 5_576 ? C34 C31 C33 C32 178.0(6) . . . 5_576 ? Co1 O31 C34 O32 -5.5(7) . . . . ? Co1 O31 C34 C31 174.0(4) . . . . ? C33 C31 C34 O32 3.1(9) . . . . ? C32 C31 C34 O32 -178.3(6) . . . . ? C33 C31 C34 O31 -176.3(6) . . . . ? C32 C31 C34 O31 2.2(8) . . . . ? C4 N3 C7 C8 -170(2) . . . . ? C5 N3 C7 C8 -35(2) . . . . ? C6 N3 C7 C8 79(2) . . . . ? N3 C7 C8 O2 66(4) . . . . ? C2 N1 C1 O1 9(3) . . . . ? C2 N1 C1 N2 -167.4(19) . . . . ? O1 C1 N2 C3 5(3) . . . . ? N1 C1 N2 C3 -178(2) . . . . ?