#------------------------------------------------------------------------------ #$Date: 2021-08-18 05:11:52 +0300 (Wed, 18 Aug 2021) $ #$Revision: 268121 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/39/2243900.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2243900 loop_ _publ_author_name 'Ma, Jie' 'Zhang, Wen-Zhi' 'Liu, Yong' 'Yi, Wen-Tao' _publ_section_title ; Synthesis, crystal structure and magnetic properties of poly[[diaqua{\m~6~-2-[bis(carboxylatomethyl)amino]terephthalato}dicobalt(II)] 1.6-hydrate] ; _journal_coeditor_code WM5615 _journal_issue 9 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first ; ; _journal_paper_doi 10.1107/S2056989021008355 _journal_volume 77 _journal_year 2021 _chemical_formula_iupac '[Co2 (C12 H7 N O8 )(H2 O)2], (H2 O)1.6' _chemical_formula_moiety '[Co2 (C12 H7 N O8 )(H2 O)2] , 1.6H2 O' _chemical_formula_sum 'C12 H14.2 Co2 N O11.6' _chemical_formula_weight 475.90 _chemical_name_systematic ;Poly[[diaqua{\m~6~-2-[bis(carboxylatomethyl)amino]terephthalato}dicobalt(II)] 1.6-hydrate] ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _cell_angle_alpha 93.859(3) _cell_angle_beta 105.571(4) _cell_angle_gamma 99.483(5) _cell_formula_units_Z 2 _cell_length_a 9.0064(9) _cell_length_b 9.2340(8) _cell_length_c 9.8426(9) _cell_measurement_reflns_used 1889 _cell_measurement_temperature 293.15 _cell_measurement_theta_max 27.5087 _cell_measurement_theta_min 2.2518 _cell_volume 772.37(13) _computing_cell_refinement ; CrystalClear (Rigaku, 2008) ; _computing_data_collection ; CrystalClear (Rigaku, 2008) ; _computing_data_reduction ; CrystalClear (Rigaku, 2008) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS (Sheldrick, 2008) ; _diffrn_ambient_temperature 293.15 _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.963 _diffrn_measured_fraction_theta_max 0.963 _diffrn_measurement_device_type 'Rigaku Saturn70 (4x4 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_unetI/netI 0.0340 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 5012 _diffrn_reflns_theta_full 24.998 _diffrn_reflns_theta_max 24.998 _diffrn_reflns_theta_min 2.957 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 2.217 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.9076 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrystalClear; Rigaku, 2008) ; _exptl_crystal_colour 'clear light red' _exptl_crystal_density_diffrn 2.046 _exptl_crystal_description plate _exptl_crystal_F_000 480 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.798 _refine_diff_density_min -0.413 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 244 _refine_ls_number_reflns 2619 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.039 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0350 _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^)+(0.0350P)^2^+1.7231P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.0839 _reflns_number_gt 2245 _reflns_number_total 2619 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL a in P-1 P-1 a.res created by SHELXL-2018/3 at 17:01:45 on 29-Jul-2021 REM TRMX 1.000 0.000 0.000 0.000 1.000 0.000 0.000 0.000 1.000 aP 1 REM SPGR P-1 REM a in P-1 P-1 REM 101 parameters refined using 0 restraints REM Highest difference peak 5.326, deepest hole -2.203, 1-sigma level 0.485 REM 109 parameters refined using 0 restraints REM Highest difference peak 2.305, deepest hole -2.391, 1-sigma level 0.365 REM 244 parameters refined using 12 restraints REM Highest difference peak 1.342, deepest hole -0.683, 1-sigma level 0.106 REM Highest difference peak 1.341, deepest hole -0.683, 1-sigma level 0.106 REM 248 parameters refined using 12 restraints REM Highest difference peak 1.301, deepest hole -0.691, 1-sigma level 0.101 REM 242 parameters refined using 12 restraints REM Highest difference peak 0.860, deepest hole -0.593, 1-sigma level 0.091 REM Highest difference peak 0.859, deepest hole -0.593, 1-sigma level 0.091 CELL 0.71073 9.0064 9.234 9.8426 93.859 105.571 99.483 ZERR 2 0.0009 0.0008 0.0009 0.003 0.004 0.005 LATT 1 SFAC C H Co N O UNIT 24 28.4 4 2 23.2 EQIV $1 -1+X,-1+Y,+Z EQIV $2 -X,-Y,-Z L.S. 20 PLAN 20 TEMP 20 CONF HTAB O9 O2_$1 HTAB O9 O3_$2 HTAB O10 O5 HTAB O10 O12 GRID BOND $H MORE -1 fmap 2 ACTA MERG 2 OMIT -2 50 OMIT -3 2 3 OMIT 0 1 0 OMIT 3 1 0 OMIT 0 0 1 OMIT 1 0 0 OMIT -1 0 1 OMIT -3 -1 1 OMIT 3 -3 4 OMIT 4 -1 1 OMIT 0 -3 2 OMIT 0 0 3 OMIT 1 0 4 OMIT 2 6 0 REM REM REM WGHT 0.035000 1.723100 FVAR 0.54727 CO1 3 0.294155 0.459586 0.482401 11.00000 0.01947 0.01950 = 0.01224 0.00157 0.00616 0.00380 O5 5 0.086324 0.319793 0.464457 11.00000 0.02498 0.03494 = 0.01725 0.00125 0.00706 -0.00555 C1 1 0.278579 0.701236 0.312541 11.00000 0.01544 0.02044 = 0.01363 0.00080 0.00395 0.00373 O7 5 0.473889 0.359311 0.464642 11.00000 0.01904 0.01976 = 0.01717 -0.00226 0.00263 0.00345 C2 1 0.292453 0.618515 0.181992 11.00000 0.01592 0.01889 = 0.01408 0.00040 0.00505 0.00257 CO2 3 -0.252682 0.148622 0.472115 11.00000 0.01754 0.01597 = 0.01652 0.00012 0.00816 0.00315 O2 5 0.333561 0.837631 0.340449 11.00000 0.02875 0.01679 = 0.02005 -0.00061 0.01156 0.00238 C3 1 0.337133 0.704226 0.082241 11.00000 0.02748 0.01825 = 0.01810 0.00189 0.00725 0.00593 AFIX 43 H3 2 0.362867 0.806555 0.103109 11.00000 -1.20000 AFIX 0 C4 1 0.343810 0.640155 -0.046351 11.00000 0.02449 0.02480 = 0.01600 0.00596 0.00903 0.00609 AFIX 43 H4 2 0.376198 0.698823 -0.110146 11.00000 -1.20000 AFIX 0 C5 1 0.302070 0.488211 -0.079835 11.00000 0.01614 0.02327 = 0.01161 0.00079 0.00427 0.00382 C6 1 0.260316 0.402519 0.019895 11.00000 0.02300 0.01624 = 0.01609 0.00073 0.00630 0.00242 AFIX 43 H6 2 0.232662 0.300415 -0.002608 11.00000 -1.20000 AFIX 0 O9 5 -0.338756 -0.073465 0.410594 11.00000 0.02344 0.02117 = 0.03795 -0.00511 0.01369 0.00162 AFIX 7 H9A 2 -0.294396 -0.105535 0.348644 11.00000 -1.50000 H9B 2 -0.438376 -0.087425 0.364194 11.00000 -1.50000 AFIX 0 C7 1 0.258552 0.464061 0.151362 11.00000 0.01643 0.02234 = 0.01221 0.00284 0.00608 0.00340 C8 1 0.299293 0.415385 -0.222084 11.00000 0.02091 0.02811 = 0.01177 -0.00013 0.00467 0.00539 O8 5 0.534175 0.175719 0.342387 11.00000 0.01978 0.02106 = 0.02349 -0.00179 0.00544 0.00738 C9 1 0.039623 0.331528 0.216492 11.00000 0.01418 0.02874 = 0.01817 0.00476 0.00504 0.00279 AFIX 23 H9C 2 -0.000542 0.253614 0.137501 11.00000 -1.20000 H9D 2 -0.004209 0.417680 0.188115 11.00000 -1.20000 AFIX 0 C10 1 -0.009845 0.280876 0.344396 11.00000 0.01582 0.02036 = 0.02346 0.00278 0.00731 0.00444 O4 5 0.332769 0.500529 -0.308508 11.00000 0.03669 0.03355 = 0.01259 -0.00101 0.01174 -0.00518 C13 1 0.280791 0.230918 0.258520 11.00000 0.02339 0.01657 = 0.01727 0.00012 0.00456 0.00297 AFIX 23 H13A 2 0.285691 0.196842 0.164707 11.00000 -1.20000 H13B 2 0.212473 0.154326 0.287781 11.00000 -1.20000 AFIX 0 C12 1 0.443365 0.257245 0.361627 11.00000 0.02097 0.01566 = 0.01876 0.00517 0.00954 0.00195 O3 5 0.262442 0.277669 -0.245166 11.00000 0.05529 0.02719 = 0.01972 -0.00116 0.01675 0.00979 O6 5 -0.145292 0.203966 0.320025 11.00000 0.01774 0.03454 = 0.02074 0.00433 0.00846 0.00099 O1 5 0.205703 0.637444 0.394090 11.00000 0.02169 0.02094 = 0.01743 -0.00012 0.01067 0.00212 O10 5 -0.042426 0.095732 0.600303 11.00000 0.02630 0.03327 = 0.02748 0.01006 0.00755 0.00673 AFIX 7 H10A 2 -0.052816 0.076051 0.685363 11.00000 -1.50000 H10B 2 0.017174 0.187022 0.599944 11.00000 -1.50000 AFIX 0 N1 4 0.214184 0.368803 0.252308 11.00000 0.01566 0.01768 = 0.01410 0.00374 0.00628 0.00299 O11 5 0.325150 0.027457 0.927749 10.50000 0.06872 O12 5 -0.017070 0.070535 0.892216 10.50000 0.07410 O13 5 0.236536 0.020547 0.918954 10.35000 0.04658 O14 5 0.099916 0.028675 0.899296 10.25000 0.10366 HKLF 4 REM a in P-1 P-1 REM wR2 = 0.0839, GooF = S = 1.039, Restrained GooF = 1.039 for all data REM R1 = 0.0350 for 2245 Fo > 4sig(Fo) and 0.0432 for all 2619 data REM 244 parameters refined using 0 restraints END WGHT 0.0350 1.7231 REM Highest difference peak 0.798, deepest hole -0.413, 1-sigma level 0.087 Q1 1 0.4228 -0.0053 0.9296 11.00000 0.05 0.80 Q2 1 0.3148 0.1379 0.9136 11.00000 0.05 0.76 Q3 1 0.1648 0.0156 0.9125 11.00000 0.05 0.67 Q4 1 0.0347 0.0426 0.8731 11.00000 0.05 0.65 Q5 1 -0.0686 0.0991 0.8959 11.00000 0.05 0.61 Q6 1 0.2886 0.0236 0.9336 11.00000 0.05 0.45 Q7 1 0.2765 0.5553 -0.0755 11.00000 0.05 0.36 Q8 1 0.2681 0.6622 0.2346 11.00000 0.05 0.33 Q9 1 -0.1485 0.1700 0.5595 11.00000 0.05 0.32 Q10 1 -0.3134 -0.1505 0.3799 11.00000 0.05 0.31 Q11 1 0.0000 0.0000 1.0000 10.50000 0.05 0.29 Q12 1 0.2354 0.5542 0.1579 11.00000 0.05 0.28 Q13 1 0.2329 -0.0632 0.8465 11.00000 0.05 0.28 Q14 1 0.3307 0.5830 0.5368 11.00000 0.05 0.26 Q15 1 0.6082 0.2275 0.3992 11.00000 0.05 0.26 Q16 1 0.2690 0.6626 0.1256 11.00000 0.05 0.26 Q17 1 0.3896 0.0981 0.3659 11.00000 0.05 0.25 Q18 1 0.3400 0.4431 -0.1286 11.00000 0.05 0.25 Q19 1 0.0190 0.2881 0.2773 11.00000 0.05 0.25 Q20 1 0.2475 0.7953 0.2936 11.00000 0.05 0.25 REM The information below was added by Olex2. REM REM R1 = 0.0350 for 2245 Fo > 4sig(Fo) and 0.0432 for all 6139 data REM 244 parameters refined using n/a restraints REM Highest difference peak 0.80, deepest hole -0.41 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0432 REM R1_gt = 0.0350 REM wR_ref = 0.0839 REM GOOF = 1.039 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 6139 REM Reflections_gt = 2245 REM Parameters = 244 REM Hole = -0.41 REM Peak = 0.80 REM Flack = n/a ; _cod_data_source_file wm5615sup1.cif _cod_data_source_block I _cod_original_formula_sum 'C12 H14.20 Co2 N O11.60' _cod_database_code 2243900 _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Co Co1 0.29415(6) 0.45959(5) 0.48240(5) 0.01675(15) Uani d 1 . . O O5 0.0863(3) 0.3198(3) 0.4645(3) 0.0269(6) Uani d 1 . . C C1 0.2786(4) 0.7012(4) 0.3125(4) 0.0166(8) Uani d 1 . . O O7 0.4739(3) 0.3593(3) 0.4646(3) 0.0194(6) Uani d 1 . . C C2 0.2925(4) 0.6185(4) 0.1820(4) 0.0163(8) Uani d 1 . . Co Co2 -0.25268(6) 0.14862(5) 0.47212(5) 0.01611(15) Uani d 1 . . O O2 0.3336(3) 0.8376(3) 0.3404(3) 0.0213(6) Uani d 1 . . C C3 0.3371(5) 0.7042(4) 0.0822(4) 0.0209(8) Uani d 1 . . H H3 0.362867 0.806555 0.103109 0.025 Uiso calc 1 . . C C4 0.3438(5) 0.6402(4) -0.0464(4) 0.0208(8) Uani d 1 . . H H4 0.376198 0.698823 -0.110146 0.025 Uiso calc 1 . . C C5 0.3021(4) 0.4882(4) -0.0798(4) 0.0170(8) Uani d 1 . . C C6 0.2603(4) 0.4025(4) 0.0199(4) 0.0185(8) Uani d 1 . . H H6 0.232662 0.300415 -0.002608 0.022 Uiso calc 1 . . O O9 -0.3388(3) -0.0735(3) 0.4106(3) 0.0273(6) Uani d 1 . . H H9A -0.294396 -0.105535 0.348644 0.041 Uiso d 1 . . H H9B -0.438376 -0.087425 0.364194 0.041 Uiso d 1 . . C C7 0.2586(4) 0.4641(4) 0.1514(4) 0.0166(8) Uani d 1 . . C C8 0.2993(4) 0.4154(4) -0.2221(4) 0.0203(8) Uani d 1 . . O O8 0.5342(3) 0.1757(3) 0.3424(3) 0.0214(6) Uani d 1 . . C C9 0.0396(4) 0.3315(4) 0.2165(4) 0.0203(8) Uani d 1 . . H H9C -0.000542 0.253614 0.137501 0.024 Uiso calc 1 . . H H9D -0.004209 0.417680 0.188115 0.024 Uiso calc 1 . . C C10 -0.0098(4) 0.2809(4) 0.3444(4) 0.0194(8) Uani d 1 . . O O4 0.3328(3) 0.5005(3) -0.3085(3) 0.0283(7) Uani d 1 . . C C13 0.2808(4) 0.2309(4) 0.2585(4) 0.0195(8) Uani d 1 . . H H13A 0.285691 0.196842 0.164707 0.023 Uiso calc 1 . . H H13B 0.212473 0.154326 0.287781 0.023 Uiso calc 1 . . C C12 0.4434(4) 0.2572(4) 0.3616(4) 0.0177(8) Uani d 1 . . O O3 0.2624(4) 0.2777(3) -0.2452(3) 0.0328(7) Uani d 1 . . O O6 -0.1453(3) 0.2040(3) 0.3200(3) 0.0242(6) Uani d 1 . . O O1 0.2057(3) 0.6374(3) 0.3941(3) 0.0194(6) Uani d 1 . . O O10 -0.0424(3) 0.0957(3) 0.6003(3) 0.0286(6) Uani d 1 . . H H10A -0.052816 0.076051 0.685363 0.043 Uiso d 1 . . H H10B 0.017174 0.187022 0.599944 0.043 Uiso d 1 . . N N1 0.2142(3) 0.3688(3) 0.2523(3) 0.0153(6) Uani d 1 . . O O11 0.3252(12) 0.0275(10) 0.9277(10) 0.069(2) Uiso d 0.5 . . O O12 -0.0171(11) 0.0705(10) 0.8922(10) 0.074(2) Uiso d 0.5 . . O O13 0.2365(15) 0.0205(11) 0.9190(11) 0.047(3) Uiso d 0.35 . . O O14 0.100(3) 0.029(3) 0.899(3) 0.104(7) Uiso d 0.25 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co1 0.0195(3) 0.0195(3) 0.0122(3) 0.0038(2) 0.0062(2) 0.00157(19) O5 0.0250(16) 0.0349(16) 0.0172(14) -0.0055(13) 0.0071(12) 0.0012(12) C1 0.0154(19) 0.0204(19) 0.0136(18) 0.0037(15) 0.0040(15) 0.0008(14) O7 0.0190(14) 0.0198(13) 0.0172(13) 0.0035(11) 0.0026(11) -0.0023(10) C2 0.016(2) 0.0189(18) 0.0141(18) 0.0026(15) 0.0051(15) 0.0004(14) Co2 0.0175(3) 0.0160(3) 0.0165(3) 0.0032(2) 0.0082(2) 0.00012(19) O2 0.0288(16) 0.0168(13) 0.0201(14) 0.0024(12) 0.0116(12) -0.0006(10) C3 0.027(2) 0.0183(18) 0.0181(19) 0.0059(16) 0.0073(16) 0.0019(15) C4 0.024(2) 0.025(2) 0.0160(19) 0.0061(17) 0.0090(16) 0.0060(15) C5 0.0161(19) 0.0233(19) 0.0116(17) 0.0038(16) 0.0043(14) 0.0008(14) C6 0.023(2) 0.0162(17) 0.0161(18) 0.0024(15) 0.0063(15) 0.0007(14) O9 0.0234(16) 0.0212(14) 0.0379(17) 0.0016(12) 0.0137(13) -0.0051(12) C7 0.016(2) 0.0223(19) 0.0122(18) 0.0034(16) 0.0061(15) 0.0028(14) C8 0.021(2) 0.028(2) 0.0118(18) 0.0054(17) 0.0047(15) -0.0001(15) O8 0.0198(14) 0.0211(13) 0.0235(14) 0.0074(12) 0.0054(11) -0.0018(11) C9 0.014(2) 0.029(2) 0.0182(19) 0.0028(16) 0.0050(15) 0.0048(16) C10 0.016(2) 0.0204(19) 0.023(2) 0.0044(16) 0.0073(16) 0.0028(15) O4 0.0367(18) 0.0335(16) 0.0126(13) -0.0052(13) 0.0117(12) -0.0010(11) C13 0.023(2) 0.0166(18) 0.0173(19) 0.0030(16) 0.0046(16) 0.0001(14) C12 0.021(2) 0.0157(18) 0.0188(19) 0.0019(16) 0.0095(16) 0.0052(15) O3 0.055(2) 0.0272(16) 0.0197(15) 0.0098(14) 0.0167(14) -0.0012(12) O6 0.0177(15) 0.0345(15) 0.0207(14) 0.0010(12) 0.0085(11) 0.0043(12) O1 0.0217(14) 0.0209(13) 0.0174(13) 0.0021(11) 0.0107(11) -0.0001(10) O10 0.0263(16) 0.0333(16) 0.0275(15) 0.0067(13) 0.0076(12) 0.0101(12) N1 0.0157(16) 0.0177(15) 0.0141(15) 0.0030(13) 0.0063(12) 0.0037(12) 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_ _diffrn_refln_index_h _diffrn_refln_index_k _diffrn_refln_index_l 0 0 -1 0 0 1 0 0 -2 0 0 2 0 0 -3 0 0 3 0 0 -4 0 0 4 0 0 -5 0 0 5 0 0 -6 0 0 6 0 0 -7 0 0 7 0 0 -8 0 0 8 0 0 -9 0 0 9 0 0 -10 0 0 10 0 0 -11 0 0 11 0 0 -12 0 1 -12 0 1 -11 0 -1 11 0 1 -10 0 -1 10 0 1 -9 0 -1 9 0 1 -8 0 -1 8 0 1 -7 0 -1 7 0 1 -6 0 -1 6 0 1 -5 0 -1 5 0 1 -4 0 -1 4 0 1 -3 0 -1 3 0 1 -2 0 -1 2 0 1 0 0 -1 -2 0 1 2 0 -1 -3 0 1 3 0 -1 -4 0 1 4 0 -1 -5 0 1 5 0 -1 -6 0 1 6 0 -1 -7 0 1 7 0 -1 -8 0 1 8 0 -1 -9 0 1 9 0 -1 -10 0 1 10 0 -1 -11 0 1 11 0 -1 -12 0 2 -12 0 2 -11 0 -2 11 0 2 -10 0 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3 3 -9 3 2 -9 3 1 -9 3 0 -9 3 -1 -9 3 -2 -9 3 -3 -9 3 -4 -9 3 -5 9 -2 -10 -9 2 10 9 -2 -9 -9 2 9 9 -2 -8 -9 2 8 9 -2 -7 -9 2 7 9 -2 -6 -9 2 6 9 -2 -5 -9 2 5 9 -2 -4 -9 2 4 -9 2 3 -9 2 3 -9 2 2 -9 2 1 -9 2 0 -9 2 -1 -9 2 -2 -9 2 -3 -9 2 -4 -9 2 -5 9 -1 -10 -9 1 10 9 -1 -9 9 -1 -8 -9 1 8 9 -1 -7 -9 1 7 9 -1 -6 -9 1 6 9 -1 -5 -9 1 5 -9 1 5 9 -1 -4 -9 1 4 -9 1 4 -9 1 3 -9 1 2 -9 1 1 -9 1 0 -9 1 -1 -9 1 -2 9 0 -10 -9 0 10 9 0 -9 -9 0 9 9 0 -8 -9 0 8 -9 0 8 9 0 -7 -9 0 7 -9 0 7 9 0 -6 -9 0 6 -9 0 6 9 0 -5 -9 0 5 9 0 -4 -9 0 4 9 0 -3 -9 0 2 9 1 -10 -9 -1 10 -9 -1 10 9 1 -9 -9 -1 9 -9 -1 9 9 1 -8 -9 -1 8 -9 -1 8 9 1 -7 -9 -1 7 -9 -1 6 -9 -1 5 -9 -1 4 -9 -1 3 -9 -2 9 -9 -2 8 -9 -2 7 -9 -2 6 -9 -2 5 -9 -2 4 -9 -2 3 -9 -3 9 -9 -3 8 -9 -3 7 -9 -3 6 -9 -3 5 -9 -3 4 -9 -3 3 -9 -4 8 -9 -4 7 -9 -4 6 -9 -4 5 -9 -4 4 -9 -4 3 9 4 -2 -9 -5 7 -9 -5 6 -9 -5 5 -9 -5 4 9 5 -3 -9 -5 3 9 5 -2 -9 -5 2 9 6 -4 9 6 -3 -10 7 5 -10 7 4 -10 7 3 -10 7 2 -10 7 1 -10 7 0 10 -6 -6 -10 6 6 10 -6 -5 -10 6 5 -10 6 4 -10 6 3 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11 -3 -4 -11 3 3 -11 3 2 -11 3 1 -11 3 0 11 -2 -7 -11 2 7 11 -2 -6 -11 2 6 11 -2 -5 11 -2 -4 -11 2 3 -11 1 7 -11 -1 5 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O5 Co1 O7 . 2_666 170.67(10) ? O5 Co1 O1 . . 99.02(11) ? O5 Co1 N1 . . 76.91(11) ? O7 Co1 O5 . . 115.34(11) ? O7 Co1 O7 . 2_666 71.31(11) ? O7 Co1 O1 . . 133.46(10) ? O7 Co1 N1 . . 78.36(10) ? O4 Co1 O5 1_556 . 91.10(11) ? O4 Co1 O7 1_556 2_666 80.73(10) ? O4 Co1 O7 1_556 . 103.42(11) ? O4 Co1 O1 1_556 . 106.43(11) ? O4 Co1 N1 1_556 . 167.23(11) ? O1 Co1 O7 . 2_666 79.19(9) ? O1 Co1 N1 . . 80.14(10) ? N1 Co1 O7 . 2_666 111.56(10) ? C10 O5 Co1 . . 119.4(2) ? O2 C1 C2 . . 119.7(3) ? O2 C1 O1 . . 118.9(3) ? O1 C1 C2 . . 121.4(3) ? Co1 O7 Co1 . 2_666 108.69(10) ? C12 O7 Co1 . 2_666 120.4(2) ? C12 O7 Co1 . . 116.8(2) ? C3 C2 C1 . . 116.4(3) ? C3 C2 C7 . . 118.8(3) ? C7 C2 C1 . . 124.8(3) ? O2 Co2 O1 2_566 2_566 59.97(9) ? O9 Co2 O2 . 2_566 96.68(10) ? O9 Co2 O8 . 1_455 84.76(11) ? O9 Co2 O1 . 2_566 156.66(10) ? O9 Co2 O10 . . 89.06(11) ? O8 Co2 O2 1_455 2_566 92.24(10) ? O8 Co2 O1 1_455 2_566 95.29(10) ? O8 Co2 O10 1_455 . 173.82(11) ? O6 Co2 O2 . 2_566 161.71(11) ? O6 Co2 O9 . . 101.55(11) ? O6 Co2 O8 . 1_455 90.90(11) ? O6 Co2 O1 . 2_566 101.79(10) ? O6 Co2 O10 . . 90.63(11) ? O10 Co2 O2 . 2_566 88.17(11) ? O10 Co2 O1 . 2_566 90.26(10) ? C1 O2 Co2 . 2_566 92.0(2) ? C2 C3 H3 . . 119.3 ? C4 C3 C2 . . 121.5(3) ? C4 C3 H3 . . 119.3 ? C3 C4 H4 . . 120.2 ? C3 C4 C5 . . 119.7(3) ? C5 C4 H4 . . 120.2 ? C4 C5 C6 . . 119.0(3) ? C4 C5 C8 . . 121.1(3) ? C6 C5 C8 . . 119.9(3) ? C5 C6 H6 . . 118.9 ? C7 C6 C5 . . 122.2(3) ? C7 C6 H6 . . 118.9 ? Co2 O9 H9A . . 109.7 ? Co2 O9 H9B . . 109.8 ? H9A O9 H9B . . 104.3 ? C2 C7 N1 . . 121.3(3) ? C6 C7 C2 . . 118.7(3) ? C6 C7 N1 . . 119.9(3) ? O4 C8 C5 . . 116.2(3) ? O3 C8 C5 . . 118.0(3) ? O3 C8 O4 . . 125.8(3) ? C12 O8 Co2 . 1_655 130.6(2) ? H9C C9 H9D . . 108.2 ? C10 C9 H9C . . 109.6 ? C10 C9 H9D . . 109.6 ? N1 C9 H9C . . 109.6 ? N1 C9 H9D . . 109.6 ? N1 C9 C10 . . 110.1(3) ? O5 C10 C9 . . 117.6(3) ? O5 C10 O6 . . 125.6(3) ? O6 C10 C9 . . 116.8(3) ? C8 O4 Co1 . 1_554 129.3(2) ? H13A C13 H13B . . 108.0 ? C12 C13 H13A . . 109.4 ? C12 C13 H13B . . 109.4 ? N1 C13 H13A . . 109.4 ? N1 C13 H13B . . 109.4 ? N1 C13 C12 . . 111.1(3) ? O7 C12 C13 . . 116.7(3) ? O8 C12 O7 . . 125.3(3) ? O8 C12 C13 . . 117.9(3) ? C10 O6 Co2 . . 124.7(2) ? Co1 O1 Co2 . 2_566 119.35(12) ? C1 O1 Co1 . . 115.4(2) ? C1 O1 Co2 . 2_566 89.1(2) ? Co2 O10 H10A . . 110.5 ? Co2 O10 H10B . . 93.8 ? H10A O10 H10B . . 114.8 ? C7 N1 Co1 . . 117.5(2) ? C7 N1 C9 . . 109.1(3) ? C7 N1 C13 . . 113.8(3) ? C9 N1 Co1 . . 105.0(2) ? C9 N1 C13 . . 110.2(3) ? C13 N1 Co1 . . 100.6(2) ? O11 O13 O14 . . 171(2) ? O12 O14 O13 . . 164(2) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 O5 . 2.049(3) y Co1 O7 . 2.033(3) y Co1 O7 2_666 2.362(3) y Co1 O4 1_556 1.992(3) y Co1 O1 . 2.083(3) y Co1 N1 . 2.241(3) y O5 C10 . 1.252(5) ? C1 C2 . 1.495(5) ? C1 O2 . 1.258(4) ? C1 O1 . 1.281(4) ? O7 C12 . 1.276(4) ? C2 C3 . 1.401(5) ? C2 C7 . 1.403(5) ? Co2 O2 2_566 2.161(2) y Co2 O9 . 2.057(3) y Co2 O8 1_455 2.065(3) y Co2 O6 . 2.038(3) y Co2 O1 2_566 2.212(2) y Co2 O10 . 2.126(3) y C3 H3 . 0.9300 ? C3 C4 . 1.381(5) ? C4 H4 . 0.9300 ? C4 C5 . 1.384(5) ? C5 C6 . 1.391(5) ? C5 C8 . 1.504(5) ? C6 H6 . 0.9300 ? C6 C7 . 1.383(5) ? O9 H9A . 0.8744 ? O9 H9B . 0.8742 ? C7 N1 . 1.461(4) ? C8 O4 . 1.258(5) ? C8 O3 . 1.249(5) ? O8 C12 . 1.240(4) ? C9 H9C . 0.9700 ? C9 H9D . 0.9700 ? C9 C10 . 1.521(5) ? C9 N1 . 1.491(5) ? C10 O6 . 1.259(5) ? C13 H13A . 0.9700 ? C13 H13B . 0.9700 ? C13 C12 . 1.512(5) ? C13 N1 . 1.492(5) ? O10 H10A . 0.8942 ? O10 H10B . 0.9225 ? O11 O13 . 0.771(12) ? O12 O14 . 1.17(3) ? O13 O14 . 1.21(3) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O9 H9A O3 2 0.87 1.93 2.701(4) 145.7 yes O9 H9B O2 1_445 0.87 2.00 2.809(4) 153.2 yes O10 H10A O12 . 0.89 1.98 2.849(10) 163.7 yes O10 H10B O5 . 0.92 2.02 2.798(4) 140.9 yes 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Co1 O5 C10 C9 . . . . 4.5(4) ? Co1 O5 C10 O6 . . . . -174.9(3) ? Co1 O7 C12 O8 2_666 . . . 51.6(4) ? Co1 O7 C12 O8 . . . . -173.0(3) ? Co1 O7 C12 C13 . . . . 4.5(4) ? Co1 O7 C12 C13 2_666 . . . -130.8(3) ? O5 C10 O6 Co2 . . . . 9.2(5) ? C1 C2 C3 C4 . . . . -175.7(3) ? C1 C2 C7 C6 . . . . 173.2(3) ? C1 C2 C7 N1 . . . . -3.7(6) ? C2 C1 O2 Co2 . . . 2_566 178.1(3) ? C2 C1 O1 Co1 . . . . 59.6(4) ? C2 C1 O1 Co2 . . . 2_566 -178.0(3) ? C2 C3 C4 C5 . . . . 1.6(6) ? C2 C7 N1 Co1 . . . . -24.7(4) ? C2 C7 N1 C9 . . . . 94.7(4) ? C2 C7 N1 C13 . . . . -141.8(3) ? Co2 O8 C12 O7 1_655 . . . 9.3(5) ? Co2 O8 C12 C13 1_655 . . . -168.3(2) ? O2 C1 C2 C3 . . . . -13.0(5) ? O2 C1 C2 C7 . . . . 169.5(3) ? O2 C1 O1 Co1 . . . . -123.4(3) ? O2 C1 O1 Co2 . . . 2_566 -1.0(3) ? C3 C2 C7 C6 . . . . -4.3(5) ? C3 C2 C7 N1 . . . . 178.9(3) ? C3 C4 C5 C6 . . . . -2.6(6) ? C3 C4 C5 C8 . . . . 176.6(3) ? C4 C5 C6 C7 . . . . 0.2(6) ? C4 C5 C8 O4 . . . . -1.8(5) ? C4 C5 C8 O3 . . . . 179.1(4) ? C5 C6 C7 C2 . . . . 3.3(6) ? C5 C6 C7 N1 . . . . -179.8(3) ? C5 C8 O4 Co1 . . . 1_554 -163.4(2) ? C6 C5 C8 O4 . . . . 177.4(4) ? C6 C5 C8 O3 . . . . -1.7(5) ? C6 C7 N1 Co1 . . . . 158.5(3) ? C6 C7 N1 C9 . . . . -82.2(4) ? C6 C7 N1 C13 . . . . 41.4(5) ? C7 C2 C3 C4 . . . . 1.9(6) ? C8 C5 C6 C7 . . . . -179.0(3) ? C9 C10 O6 Co2 . . . . -170.2(2) ? C10 C9 N1 Co1 . . . . -33.2(3) ? C10 C9 N1 C7 . . . . -160.1(3) ? C10 C9 N1 C13 . . . . 74.3(4) ? C12 C13 N1 Co1 . . . . -40.3(3) ? C12 C13 N1 C7 . . . . 86.3(4) ? C12 C13 N1 C9 . . . . -150.7(3) ? O3 C8 O4 Co1 . . . 1_554 15.5(6) ? O1 C1 C2 C3 . . . . 164.0(3) ? O1 C1 C2 C7 . . . . -13.6(6) ? O1 C1 O2 Co2 . . . 2_566 1.1(3) ? N1 C9 C10 O5 . . . . 22.0(5) ? N1 C9 C10 O6 . . . . -158.6(3) ? N1 C13 C12 O7 . . . . 27.9(4) ? N1 C13 C12 O8 . . . . -154.3(3) ?