#------------------------------------------------------------------------------ #$Date: 2023-11-28 01:41:14 +0200 (Tue, 28 Nov 2023) $ #$Revision: 287819 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/77/7247798.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_7247798 loop_ _publ_author_name 'Yang, Yuanyu' 'Xue, Jian-Hua' 'Yang, Dong-Dong' 'Zhang, Liyang' 'Ma, Qi' 'Zhao, Xuan' _publ_section_title ; Effects of solvents and metal ions on the synthesis, structural diversity and magnetic properties of 5'-nitro-[1,1':3',1''-terphenyl]-3,3'',5,5''-tetracarboxylic acid ligand and a highly sensitive sensor for Fe3+ ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D3CE01076G _journal_year 2023 _chemical_formula_sum 'C32 H27 Co2 N3 O15' _chemical_formula_weight 811.42 _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 mixed _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2020-07-25 deposited with the CCDC. 2023-11-27 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 111.057(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.1756(19) _cell_length_b 11.7383(12) _cell_length_c 15.5273(14) _cell_measurement_reflns_used 5175 _cell_measurement_temperature 297(2) _cell_measurement_theta_max 27.72 _cell_measurement_theta_min 2.91 _cell_volume 3261.6(6) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014 (Sheldrick 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 297(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.989 _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 0.0521 _diffrn_reflns_av_unetI/netI 0.0511 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 17722 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.325 _diffrn_reflns_theta_min 2.913 _exptl_absorpt_coefficient_mu 1.098 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour pink _exptl_crystal_density_diffrn 1.652 _exptl_crystal_description block _exptl_crystal_F_000 1656 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_transmission_factor_max 0.7457 _exptl_transmission_factor_min 0.6827 _refine_diff_density_max 1.489 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.098 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 241 _refine_ls_number_reflns 4021 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0887 _refine_ls_R_factor_gt 0.0545 _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^)+(0.0595P)^2^+13.6669P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1353 _refine_ls_wR_factor_ref 0.1508 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2811 _reflns_number_total 4021 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce01076g2.cif _cod_data_source_block complex2 _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 7247798 _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 ; co-4-4-11_pl.res created by SHELXL-2014/7 TITL co-4-4-11 in Cc New: C2/c CELL 0.71073 19.1756 11.7383 15.5273 90.000 111.057 90.000 ZERR 4 0.0019 0.0012 0.0014 0.000 0.003 0.000 LATT 7 SYMM - X , Y , 0.50000 - Z SFAC C H Co N O UNIT 128 108 8 12 60 L.S. 10 ACTA BOND $H FMAP 2 PLAN 5 WGHT 0.059500 13.666901 FVAR 0.07843 RESI 0 CONF TEMP 24 CO1 3 0.223667 0.170777 0.142062 11.00000 0.03411 0.03011 = 0.02040 0.00039 0.00264 0.01066 C1 1 0.299719 0.255517 0.335335 11.00000 0.03464 0.02548 = 0.01930 -0.00098 0.00394 0.00508 C2 1 0.321123 0.220323 0.434686 11.00000 0.02429 0.02590 = 0.01791 -0.00104 0.00062 0.00276 C3 1 0.288971 0.123715 0.456697 11.00000 0.02527 0.02756 = 0.01959 -0.00619 0.00233 -0.00227 AFIX 43 H3 2 0.253019 0.083148 0.410249 11.00000 -1.20000 AFIX 0 C4 1 0.310296 0.087498 0.547741 11.00000 0.02858 0.02543 = 0.02265 -0.00241 0.00739 -0.00141 C5 1 0.275468 -0.012757 0.575318 11.00000 0.03288 0.03167 = 0.02760 -0.00334 0.01000 -0.00733 C6 1 0.363874 0.148977 0.616303 11.00000 0.02766 0.02918 = 0.01768 0.00231 0.00252 -0.00135 AFIX 43 H6 2 0.378726 0.124058 0.677110 11.00000 -1.20000 AFIX 0 C7 1 0.395813 0.246621 0.596411 11.00000 0.02210 0.02669 = 0.01918 -0.00203 -0.00049 0.00044 C8 1 0.374327 0.281766 0.504961 11.00000 0.02711 0.02351 = 0.02341 -0.00012 0.00430 -0.00222 AFIX 43 H8 2 0.395584 0.346775 0.490479 11.00000 -1.20000 AFIX 0 C9 1 0.450275 0.312010 0.673867 11.00000 0.02671 0.02739 = 0.01790 -0.00144 -0.00030 -0.00207 C10 1 0.500000 0.255004 0.750000 10.50000 0.02667 0.02213 = 0.02382 0.00000 -0.00107 0.00000 AFIX 43 H10 2 0.499998 0.175776 0.750001 10.50000 -1.20000 AFIX 0 C11 1 0.451363 0.430275 0.673248 11.00000 0.02648 0.02757 = 0.02070 0.00121 -0.00290 0.00063 AFIX 43 H11 2 0.420229 0.470883 0.622590 11.00000 -1.20000 AFIX 0 C12 1 0.500000 0.486487 0.750000 10.50000 0.02940 0.02277 = 0.02832 0.00000 0.00158 0.00000 C13 1 0.138194 0.385688 0.137913 11.00000 0.04399 0.04156 = 0.02782 -0.00170 0.00353 0.01307 AFIX 43 H13 2 0.174604 0.395508 0.196157 11.00000 -1.20000 AFIX 0 C14 1 0.083936 0.466743 0.106411 11.00000 0.04482 0.03671 = 0.03219 -0.00586 0.00628 0.01446 AFIX 43 H14 2 0.083412 0.528745 0.143461 11.00000 -1.20000 AFIX 0 C15 1 0.029543 0.456616 0.019070 11.00000 0.02931 0.02679 = 0.03276 0.00310 0.00851 0.00878 C16 1 0.034614 0.363035 -0.031225 11.00000 0.06891 0.07413 = 0.04181 -0.02811 -0.02336 0.04683 AFIX 43 H16 2 0.000220 0.352480 -0.090673 11.00000 -1.20000 AFIX 0 C17 1 0.090845 0.284719 0.006638 11.00000 0.07632 0.06464 = 0.04741 -0.02955 -0.02146 0.04830 AFIX 43 H17 2 0.092876 0.221827 -0.028810 11.00000 -1.20000 AFIX 0 N1 4 0.500000 0.611228 0.750000 10.50000 0.03916 0.02706 = 0.03880 0.00000 -0.00732 0.00000 N2 4 0.141974 0.293574 0.090142 11.00000 0.03587 0.03343 = 0.02772 0.00026 0.00532 0.01119 O1 5 0.247456 0.199417 0.278004 11.00000 0.03772 0.04285 = 0.01733 -0.00394 0.00168 -0.00530 O2 5 0.334238 0.334827 0.314934 11.00000 0.07955 0.03909 = 0.02577 0.00035 0.00934 -0.02237 O3 5 0.225428 -0.071190 0.516978 11.00000 0.04685 0.03733 = 0.03148 -0.00529 0.00974 -0.01714 O4 5 0.296626 -0.036354 0.660400 11.00000 0.05367 0.04537 = 0.02592 0.00218 0.00676 -0.02248 O5 5 0.479426 0.659716 0.677535 11.00000 0.11896 0.03161 = 0.05395 0.01522 -0.01210 -0.00284 O6 5 0.136476 0.057318 0.147319 11.00000 0.04631 0.03620 = 0.06799 0.00146 0.02130 -0.00201 AFIX 3 H6A 2 0.163230 0.067724 0.116630 11.00000 -1.50000 H6B 2 0.124823 -0.013993 0.138686 11.00000 -1.50000 AFIX 0 O7 5 0.306032 0.287565 0.135609 11.00000 0.05145 0.05187 = 0.03380 0.00937 0.01392 0.00398 AFIX 3 H7A 2 0.322600 0.319994 0.185586 11.00000 -1.50000 H7B 2 0.291194 0.337041 0.095967 11.00000 -1.50000 AFIX 0 O8 5 0.041096 0.586155 0.269137 10.50000 0.15316 0.14476 = 0.10669 -0.03207 0.01189 0.06202 AFIX 3 H8A 2 0.086079 0.573380 0.292096 10.50000 -1.50000 H8B 2 0.032489 0.643541 0.293736 10.50000 -1.50000 AFIX 0 HKLF 4 REM co-4-4-11 in Cc New: C2/c REM R1 = 0.0545 for 2811 Fo > 4sig(Fo) and 0.0887 for all 4021 data REM 241 parameters refined using 0 restraints END WGHT 0.0618 13.1082 REM Highest difference peak 1.489, deepest hole -0.467, 1-sigma level 0.098 Q1 1 -0.0018 -0.0207 0.0093 11.00000 0.05 1.49 Q2 1 0.3443 0.2477 0.4706 11.00000 0.05 0.38 Q3 1 0.0290 0.3753 0.0020 11.00000 0.05 0.35 Q4 1 0.1069 0.3434 0.1346 11.00000 0.05 0.33 Q5 1 0.2992 0.1219 0.5057 11.00000 0.05 0.33 ; _shelx_res_checksum 22947 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 0.22367(3) 0.17078(4) 0.14206(3) 0.03017(17) Uani 1 1 d . . . . . C1 C 0.2997(2) 0.2555(3) 0.3353(2) 0.0281(8) Uani 1 1 d . . . . . C2 C 0.32112(19) 0.2203(3) 0.4347(2) 0.0246(7) Uani 1 1 d . . . . . C3 C 0.28897(19) 0.1237(3) 0.4567(2) 0.0257(7) Uani 1 1 d . . . . . H3 H 0.2530 0.0831 0.4102 0.031 Uiso 1 1 calc R U . . . C4 C 0.3103(2) 0.0875(3) 0.5477(2) 0.0261(7) Uani 1 1 d . . . . . C5 C 0.2755(2) -0.0128(3) 0.5753(3) 0.0310(8) Uani 1 1 d . . . . . C6 C 0.3639(2) 0.1490(3) 0.6163(2) 0.0264(8) Uani 1 1 d . . . . . H6 H 0.3787 0.1241 0.6771 0.032 Uiso 1 1 calc R U . . . C7 C 0.39581(19) 0.2466(3) 0.5964(2) 0.0248(7) Uani 1 1 d . . . . . C8 C 0.3743(2) 0.2818(3) 0.5050(2) 0.0260(7) Uani 1 1 d . . . . . H8 H 0.3956 0.3468 0.4905 0.031 Uiso 1 1 calc R U . . . C9 C 0.4503(2) 0.3120(3) 0.6739(2) 0.0263(8) Uani 1 1 d . . . . . C10 C 0.5000 0.2550(4) 0.7500 0.0270(11) Uani 1 2 d S T P . . H10 H 0.5000 0.1758 0.7500 0.032 Uiso 1 2 calc R U P . . C11 C 0.4514(2) 0.4303(3) 0.6732(2) 0.0280(8) Uani 1 1 d . . . . . H11 H 0.4202 0.4709 0.6226 0.034 Uiso 1 1 calc R U . . . C12 C 0.5000 0.4865(4) 0.7500 0.0292(11) Uani 1 2 d S T P . . C13 C 0.1382(2) 0.3857(4) 0.1379(3) 0.0404(10) Uani 1 1 d . . . . . H13 H 0.1746 0.3955 0.1962 0.048 Uiso 1 1 calc R U . . . C14 C 0.0839(2) 0.4667(4) 0.1064(3) 0.0400(10) Uani 1 1 d . . . . . H14 H 0.0834 0.5287 0.1435 0.048 Uiso 1 1 calc R U . . . C15 C 0.0295(2) 0.4566(3) 0.0191(3) 0.0303(8) Uani 1 1 d . . . . . C16 C 0.0346(3) 0.3630(5) -0.0312(3) 0.074(2) Uani 1 1 d . . . . . H16 H 0.0002 0.3525 -0.0907 0.088 Uiso 1 1 calc R U . . . C17 C 0.0908(3) 0.2847(5) 0.0066(3) 0.075(2) Uani 1 1 d . . . . . H17 H 0.0929 0.2218 -0.0288 0.090 Uiso 1 1 calc R U . . . N1 N 0.5000 0.6112(4) 0.7500 0.0409(12) Uani 1 2 d S T P . . N2 N 0.14197(19) 0.2936(3) 0.0901(2) 0.0340(7) Uani 1 1 d . . . . . O1 O 0.24746(15) 0.1994(2) 0.27800(17) 0.0349(6) Uani 1 1 d . . . . . O2 O 0.3342(2) 0.3348(3) 0.31493(19) 0.0508(9) Uani 1 1 d . . . . . O3 O 0.22543(16) -0.0712(2) 0.51698(18) 0.0397(7) Uani 1 1 d . . . . . O4 O 0.29663(17) -0.0364(3) 0.66040(18) 0.0437(8) Uani 1 1 d . . . . . O5 O 0.4794(3) 0.6597(3) 0.6775(3) 0.0800(14) Uani 1 1 d . . . . . O6 O 0.13648(17) 0.0573(3) 0.1473(2) 0.0500(8) Uani 1 1 d . . . . . H6A H 0.1632 0.0677 0.1166 0.075 Uiso 1 1 d R U . . . H6B H 0.1248 -0.0140 0.1387 0.075 Uiso 1 1 d R U . . . O7 O 0.30603(17) 0.2876(3) 0.1356(2) 0.0461(8) Uani 1 1 d . . . . . H7A H 0.3226 0.3200 0.1856 0.069 Uiso 1 1 d R U . . . H7B H 0.2912 0.3370 0.0960 0.069 Uiso 1 1 d R U . . . O8 O 0.0411(7) 0.5862(11) 0.2691(8) 0.144(5) Uani 0.5 1 d . . P . . H8A H 0.0861 0.5734 0.2921 0.217 Uiso 0.5 1 d R U P . . H8B H 0.0325 0.6435 0.2937 0.217 Uiso 0.5 1 d R U P . . 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 0.0341(3) 0.0301(3) 0.0204(2) 0.0004(2) 0.00264(19) 0.0107(2) C1 0.035(2) 0.0255(18) 0.0193(16) -0.0010(14) 0.0039(14) 0.0051(16) C2 0.0243(17) 0.0259(17) 0.0179(16) -0.0010(13) 0.0006(13) 0.0028(15) C3 0.0253(18) 0.0276(18) 0.0196(16) -0.0062(14) 0.0023(13) -0.0023(15) C4 0.0286(18) 0.0254(18) 0.0226(16) -0.0024(14) 0.0074(14) -0.0014(15) C5 0.033(2) 0.032(2) 0.0276(18) -0.0033(15) 0.0100(15) -0.0073(17) C6 0.0277(18) 0.0292(19) 0.0177(15) 0.0023(13) 0.0025(13) -0.0014(15) C7 0.0221(17) 0.0267(17) 0.0192(16) -0.0020(14) -0.0005(13) 0.0004(14) C8 0.0271(18) 0.0235(17) 0.0234(17) -0.0001(14) 0.0043(14) -0.0022(15) C9 0.0267(18) 0.0274(18) 0.0179(15) -0.0014(13) -0.0003(13) -0.0021(15) C10 0.027(3) 0.022(2) 0.024(2) 0.000 -0.001(2) 0.000 C11 0.0265(18) 0.0276(18) 0.0207(16) 0.0012(14) -0.0029(13) 0.0006(15) C12 0.029(3) 0.023(2) 0.028(3) 0.000 0.002(2) 0.000 C13 0.044(2) 0.042(2) 0.0278(19) -0.0017(18) 0.0035(17) 0.013(2) C14 0.045(2) 0.037(2) 0.032(2) -0.0059(17) 0.0063(18) 0.0145(19) C15 0.0293(19) 0.0268(18) 0.0328(19) 0.0031(16) 0.0085(15) 0.0088(16) C16 0.069(4) 0.074(4) 0.042(3) -0.028(3) -0.023(2) 0.047(3) C17 0.076(4) 0.065(3) 0.047(3) -0.030(3) -0.021(3) 0.048(3) N1 0.039(3) 0.027(2) 0.039(3) 0.000 -0.007(2) 0.000 N2 0.0359(18) 0.0334(17) 0.0277(16) 0.0003(14) 0.0053(14) 0.0112(15) O1 0.0377(15) 0.0428(16) 0.0173(12) -0.0039(11) 0.0017(11) -0.0053(13) O2 0.080(2) 0.0391(17) 0.0258(14) 0.0003(13) 0.0093(14) -0.0224(17) O3 0.0468(17) 0.0373(16) 0.0315(14) -0.0053(12) 0.0097(12) -0.0171(14) O4 0.0537(19) 0.0454(17) 0.0259(14) 0.0022(12) 0.0068(13) -0.0225(15) O5 0.119(4) 0.0316(18) 0.054(2) 0.0152(16) -0.012(2) -0.003(2) O6 0.0463(18) 0.0362(16) 0.068(2) 0.0015(15) 0.0213(16) -0.0020(14) O7 0.0514(19) 0.0519(19) 0.0338(16) 0.0094(14) 0.0139(14) 0.0040(15) O8 0.153(11) 0.145(11) 0.107(9) -0.032(8) 0.012(8) 0.062(9) 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 O1 Co1 O4 95.50(11) . 6 ? O1 Co1 N2 98.42(12) . . ? O4 Co1 N2 165.92(12) 6 . ? O1 Co1 O7 92.83(11) . . ? O4 Co1 O7 91.22(13) 6 . ? N2 Co1 O7 90.21(13) . . ? O1 Co1 O6 87.16(12) . . ? O4 Co1 O6 91.09(13) 6 . ? N2 Co1 O6 87.50(13) . . ? O7 Co1 O6 177.68(12) . . ? O1 Co1 O3 155.38(11) . 6 ? O4 Co1 O3 60.47(10) 6 6 ? N2 Co1 O3 105.46(11) . 6 ? O7 Co1 O3 92.98(12) . 6 ? O6 Co1 O3 87.97(12) . 6 ? O1 Co1 C5 125.63(12) . 6 ? O4 Co1 C5 30.34(11) 6 6 ? N2 Co1 C5 135.60(12) . 6 ? O7 Co1 C5 92.66(13) . 6 ? O6 Co1 C5 89.22(13) . 6 ? O3 Co1 C5 30.14(11) 6 6 ? O1 Co1 H6A 104.6 . . ? O4 Co1 H6A 81.5 6 . ? N2 Co1 H6A 92.9 . . ? O7 Co1 H6A 161.7 . . ? O6 Co1 H6A 19.2 . . ? O3 Co1 H6A 68.8 6 . ? C5 Co1 H6A 72.6 6 . ? O2 C1 O1 124.8(3) . . ? O2 C1 C2 119.4(3) . . ? O1 C1 C2 115.8(3) . . ? C3 C2 C8 119.5(3) . . ? C3 C2 C1 119.6(3) . . ? C8 C2 C1 120.8(3) . . ? C4 C3 C2 120.3(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C6 C4 C3 119.2(3) . . ? C6 C4 C5 118.4(3) . . ? C3 C4 C5 122.4(3) . . ? O3 C5 O4 120.5(4) . . ? O3 C5 C4 121.8(3) . . ? O4 C5 C4 117.7(3) . . ? O3 C5 Co1 65.2(2) . 6_556 ? O4 C5 Co1 55.29(19) . 6_556 ? C4 C5 Co1 172.7(3) . 6_556 ? C7 C6 C4 121.6(3) . . ? C7 C6 H6 119.2 . . ? C4 C6 H6 119.2 . . ? C6 C7 C8 118.7(3) . . ? C6 C7 C9 118.9(3) . . ? C8 C7 C9 122.4(3) . . ? C7 C8 C2 120.6(3) . . ? C7 C8 H8 119.7 . . ? C2 C8 H8 119.7 . . ? C11 C9 C10 118.6(3) . . ? C11 C9 C7 121.1(3) . . ? C10 C9 C7 120.3(3) . . ? C9 C10 C9 122.6(5) 2_656 . ? C9 C10 H10 118.7 2_656 . ? C9 C10 H10 118.7 . . ? C12 C11 C9 118.5(3) . . ? C12 C11 H11 120.8 . . ? C9 C11 H11 120.8 . . ? C11 C12 C11 123.2(5) 2_656 . ? C11 C12 N1 118.4(2) 2_656 . ? C11 C12 N1 118.4(2) . . ? N2 C13 C14 123.7(4) . . ? N2 C13 H13 118.1 . . ? C14 C13 H13 118.1 . . ? C13 C14 C15 120.0(4) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 116.3(4) . . ? C16 C15 C15 121.6(4) . 5_565 ? C14 C15 C15 122.1(4) . 5_565 ? C15 C16 C17 119.8(4) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? N2 C17 C16 123.9(4) . . ? N2 C17 H17 118.0 . . ? C16 C17 H17 118.0 . . ? O5 N1 O5 123.1(5) 2_656 . ? O5 N1 C12 118.5(3) 2_656 . ? O5 N1 C12 118.5(3) . . ? C17 N2 C13 116.3(4) . . ? C17 N2 Co1 121.3(3) . . ? C13 N2 Co1 122.4(3) . . ? C1 O1 Co1 130.4(3) . . ? C5 O3 Co1 84.7(2) . 6_556 ? C5 O4 Co1 94.4(2) . 6_556 ? Co1 O6 H6A 40.3 . . ? Co1 O6 H6B 138.7 . . ? H6A O6 H6B 103.5 . . ? Co1 O7 H7A 107.3 . . ? Co1 O7 H7B 115.5 . . ? H7A O7 H7B 107.1 . . ? O8 O8 H8A 169.2 2 . ? O8 O8 H8B 79.8 2 . ? H8A O8 H8B 107.7 . . ? 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 O1 2.021(2) . ? Co1 O4 2.060(3) 6 ? Co1 N2 2.067(3) . ? Co1 O7 2.121(3) . ? Co1 O6 2.162(3) . ? Co1 O3 2.277(3) 6 ? Co1 C5 2.498(4) 6 ? Co1 H6A 1.6228 . ? C1 O2 1.247(5) . ? C1 O1 1.261(4) . ? C1 C2 1.505(5) . ? C2 C3 1.391(5) . ? C2 C8 1.397(5) . ? C3 C4 1.390(5) . ? C3 H3 0.9300 . ? C4 C6 1.387(5) . ? C4 C5 1.490(5) . ? C5 O3 1.260(4) . ? C5 O4 1.265(5) . ? C5 Co1 2.498(4) 6_556 ? C6 C7 1.386(5) . ? C6 H6 0.9300 . ? C7 C8 1.391(5) . ? C7 C9 1.491(5) . ? C8 H8 0.9300 . ? C9 C11 1.388(5) . ? C9 C10 1.394(4) . ? C10 C9 1.394(4) 2_656 ? C10 H10 0.9300 . ? C11 C12 1.388(4) . ? C11 H11 0.9300 . ? C12 C11 1.388(4) 2_656 ? C12 N1 1.464(7) . ? C13 N2 1.328(5) . ? C13 C14 1.364(6) . ? C13 H13 0.9300 . ? C14 C15 1.387(5) . ? C14 H14 0.9300 . ? C15 C16 1.371(6) . ? C15 C15 1.480(7) 5_565 ? C16 C17 1.378(6) . ? C16 H16 0.9300 . ? C17 N2 1.319(5) . ? C17 H17 0.9300 . ? N1 O5 1.194(4) 2_656 ? N1 O5 1.194(4) . ? O3 Co1 2.277(3) 6_556 ? O4 Co1 2.060(3) 6_556 ? O6 H6A 0.8251 . ? O6 H6B 0.8643 . ? O7 H7A 0.8191 . ? O7 H7B 0.8193 . ? O8 O8 1.47(2) 2 ? O8 H8A 0.8201 . ? O8 H8B 0.8199 . ? 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 O2 C1 C2 C3 -172.5(4) . . . . ? O1 C1 C2 C3 6.5(5) . . . . ? O2 C1 C2 C8 5.8(5) . . . . ? O1 C1 C2 C8 -175.1(3) . . . . ? C8 C2 C3 C4 -0.9(5) . . . . ? C1 C2 C3 C4 177.5(3) . . . . ? C2 C3 C4 C6 0.1(5) . . . . ? C2 C3 C4 C5 177.6(3) . . . . ? C6 C4 C5 O3 178.6(4) . . . . ? C3 C4 C5 O3 1.1(6) . . . . ? C6 C4 C5 O4 0.2(5) . . . . ? C3 C4 C5 O4 -177.3(4) . . . . ? C3 C4 C6 C7 1.0(6) . . . . ? C5 C4 C6 C7 -176.6(3) . . . . ? C4 C6 C7 C8 -1.3(5) . . . . ? C4 C6 C7 C9 177.0(3) . . . . ? C6 C7 C8 C2 0.5(5) . . . . ? C9 C7 C8 C2 -177.7(3) . . . . ? C3 C2 C8 C7 0.6(5) . . . . ? C1 C2 C8 C7 -177.8(3) . . . . ? C6 C7 C9 C11 -141.6(4) . . . . ? C8 C7 C9 C11 36.6(6) . . . . ? C6 C7 C9 C10 36.5(5) . . . . ? C8 C7 C9 C10 -145.2(3) . . . . ? C11 C9 C10 C9 1.2(3) . . . 2_656 ? C7 C9 C10 C9 -177.0(4) . . . 2_656 ? C10 C9 C11 C12 -2.4(5) . . . . ? C7 C9 C11 C12 175.8(3) . . . . ? C9 C11 C12 C11 1.2(3) . . . 2_656 ? C9 C11 C12 N1 -178.8(3) . . . . ? N2 C13 C14 C15 -1.4(7) . . . . ? C13 C14 C15 C16 -0.3(7) . . . . ? C13 C14 C15 C15 -178.7(5) . . . 5_565 ? C14 C15 C16 C17 1.2(9) . . . . ? C15 C15 C16 C17 179.5(6) 5_565 . . . ? C15 C16 C17 N2 -0.3(11) . . . . ? C11 C12 N1 O5 -24.9(3) 2_656 . . 2_656 ? C11 C12 N1 O5 155.1(3) . . . 2_656 ? C11 C12 N1 O5 155.1(3) 2_656 . . . ? C11 C12 N1 O5 -24.9(3) . . . . ? C16 C17 N2 C13 -1.4(10) . . . . ? C16 C17 N2 Co1 179.2(6) . . . . ? C14 C13 N2 C17 2.2(7) . . . . ? C14 C13 N2 Co1 -178.4(4) . . . . ? O2 C1 O1 Co1 24.4(6) . . . . ? C2 C1 O1 Co1 -154.5(3) . . . . ? O4 C5 O3 Co1 0.7(4) . . . 6_556 ? C4 C5 O3 Co1 -177.6(4) . . . 6_556 ? O3 C5 O4 Co1 -0.8(4) . . . 6_556 ? C4 C5 O4 Co1 177.6(3) . . . 6_556 ?