#------------------------------------------------------------------------------ #$Date: 2023-11-02 01:43:29 +0200 (Thu, 02 Nov 2023) $ #$Revision: 287232 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247649.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_7247649 loop_ _publ_author_name 'Ovcharenko, Victor' 'Fursova, Elena' 'Letyagin, Gleb' 'Morozov, Vitaly' 'Bogomyakov, Artem' 'Romanenko, Galina' _publ_section_title ; Alternating [ML2(MeOH)2] and [ML2(EtOH)2] layers in low-temperature ferromagnets [ML2(MeOH)2][ML2(EtOH)2] (M = CoII, NiII or CoII0.5NiII0.5) ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D3CE00912B _journal_year 2023 _chemical_formula_sum 'C23 H36 Co F6 N4 O6' _chemical_formula_weight 637.49 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_block_doi 10.5517/ccdc.csd.cc2bjd3d _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2022-03-22 deposited with the CCDC. 2023-10-12 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 120.86(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 18.514(4) _cell_length_b 15.792(3) _cell_length_c 11.787(2) _cell_measurement_reflns_used 6442 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.64 _cell_measurement_theta_min 2.58 _cell_volume 2958.3(14) _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-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.991 _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 0.0544 _diffrn_reflns_av_unetI/netI 0.0743 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 26411 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.128 _diffrn_reflns_theta_min 1.281 _exptl_absorpt_coefficient_mu 0.660 _exptl_absorpt_correction_T_max 0.2963 _exptl_absorpt_correction_T_min 0.2327 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.431 _exptl_crystal_description cube _exptl_crystal_F_000 1324 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.406 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.059 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.698 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 370 _refine_ls_number_reflns 7881 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.698 _refine_ls_R_factor_all 0.1077 _refine_ls_R_factor_gt 0.0427 _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^)+(0.1354P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1222 _refine_ls_wR_factor_ref 0.1678 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3843 _reflns_number_total 7881 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce00912b1.cif _cod_data_source_block z699s _cod_original_cell_volume 2958.3(13) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7247649 _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 ; z699s.res created by SHELXL-2014/7 TITL z699s in P2(1)/c CELL 0.71073 18.5137 15.7925 11.7867 90.000 120.860 90.000 ZERR 4.00 0.0037 0.0032 0.0024 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O F Co UNIT 92 144 16 24 24 4 L.S. 20 acta htab EQIV $1 -x, y-1/2, -z+5/2 HTAB O1S O13A_$1 EQIV $2 x, -y+1/2, z+1/2 HTAB O1T O13B_$2 BOND FMAP 2 PLAN 20 WGHT 0.135400 FVAR 0.19051 CO1 6 0.000000 0.500000 1.000000 10.50000 0.02953 0.02455 = 0.02860 -0.00118 0.01276 0.00155 O1S 4 -0.052256 0.447014 1.112607 11.00000 0.06437 0.03562 = 0.07094 0.01253 0.04800 0.00699 H1S 2 -0.045798 0.405799 1.126983 11.00000 -1.20000 C1S 1 -0.123208 0.479671 1.114695 11.00000 0.08415 0.06738 = 0.09990 0.02312 0.07059 0.01394 AFIX 33 H1SA 2 -0.134040 0.445392 1.171625 11.00000 -1.50000 H1SB 2 -0.111963 0.536819 1.147013 11.00000 -1.50000 H1SC 2 -0.171483 0.478833 1.026856 11.00000 -1.50000 AFIX 0 O1A 4 -0.117897 0.525278 0.851300 11.00000 0.03379 0.03730 = 0.03717 -0.00677 0.00779 0.00581 C2A 1 -0.162662 0.591527 0.829575 11.00000 0.03323 0.03842 = 0.03006 0.00343 0.01468 0.00566 C3A 1 -0.250066 0.582295 0.709985 11.00000 0.03743 0.05105 = 0.04675 -0.00120 0.01268 0.00711 F4A 5 -0.292494 0.520868 0.726775 11.00000 0.04570 0.10578 = 0.10522 0.01113 0.01704 -0.02074 F5A 5 -0.298247 0.650316 0.680176 11.00000 0.05671 0.08408 = 0.08308 -0.01004 -0.01034 0.03440 F6A 5 -0.248215 0.562623 0.602596 11.00000 0.05945 0.13593 = 0.03906 -0.02401 0.00742 0.00470 C7A 1 -0.141190 0.664895 0.900338 11.00000 0.03885 0.03536 = 0.03636 0.00213 0.01616 0.00904 AFIX 43 H7AA 2 -0.180340 0.708663 0.869192 11.00000 -1.20000 AFIX 0 C8A 1 -0.062860 0.678996 1.018702 11.00000 0.03932 0.03104 = 0.03311 -0.00055 0.02003 0.00285 C9A 1 -0.047576 0.762406 1.090892 11.00000 0.05011 0.03139 = 0.04590 -0.00553 0.02104 0.00880 C10A 1 -0.037440 0.835498 1.015282 11.00000 0.10723 0.03619 = 0.08544 0.00284 0.03088 -0.00545 AFIX 33 H10A 2 -0.090957 0.848375 0.938563 11.00000 -1.50000 H10B 2 -0.016641 0.884467 1.071314 11.00000 -1.50000 H10C 2 0.001648 0.819587 0.988453 11.00000 -1.50000 AFIX 0 C11A 1 -0.111876 0.782856 1.129750 11.00000 0.06696 0.09084 = 0.09488 -0.04247 0.04378 0.00694 AFIX 33 H11A 2 -0.164853 0.795784 1.051977 11.00000 -1.50000 H11B 2 -0.118447 0.734963 1.173828 11.00000 -1.50000 H11C 2 -0.093116 0.830792 1.188094 11.00000 -1.50000 AFIX 0 N12A 3 0.033406 0.742558 1.207416 11.00000 0.05659 0.03716 = 0.04939 -0.01823 0.01444 0.00702 O13A 4 0.071747 0.790190 1.308899 11.00000 0.08827 0.06032 = 0.07051 -0.03935 0.00689 0.01190 C14A 1 0.067913 0.659643 1.199902 11.00000 0.04936 0.03309 = 0.04000 -0.01082 0.01429 0.00220 C15A 1 0.146481 0.673187 1.191739 11.00000 0.04017 0.05027 = 0.08857 -0.02312 0.01918 -0.01135 AFIX 33 H15A 2 0.190530 0.695861 1.273954 11.00000 -1.50000 H15B 2 0.164268 0.620080 1.174522 11.00000 -1.50000 H15C 2 0.134222 0.712167 1.121591 11.00000 -1.50000 AFIX 0 C16A 1 0.084129 0.606466 1.317691 11.00000 0.08537 0.05640 = 0.03262 -0.00346 0.01439 0.02344 AFIX 33 H16A 2 0.129606 0.630723 1.396963 11.00000 -1.50000 H16B 2 0.034343 0.605094 1.323666 11.00000 -1.50000 H16C 2 0.098713 0.549886 1.307081 11.00000 -1.50000 AFIX 0 N17A 3 -0.001630 0.624777 1.075456 11.00000 0.03256 0.02669 = 0.03110 -0.00280 0.01278 0.00089 CO2 6 0.500000 0.500000 2.000000 10.50000 0.02693 0.02798 = 0.03190 -0.00185 0.01127 0.00228 O1T 4 0.456189 0.405380 2.080780 11.00000 0.05624 0.03683 = 0.07833 0.01430 0.04303 0.00727 H1T 2 0.472583 0.365198 2.104097 11.00000 -1.20000 C1T 1 0.383491 0.406100 2.091668 11.00000 0.07132 0.05134 = 0.09660 0.00484 0.05819 -0.00187 AFIX 23 H1TA 2 0.366232 0.464350 2.089587 11.00000 -1.20000 H1TB 2 0.397823 0.382462 2.176674 11.00000 -1.20000 AFIX 0 C2T 1 0.312697 0.358855 1.987912 11.00000 0.08217 0.09601 = 0.10743 0.01829 0.05090 -0.00037 AFIX 33 H2TA 2 0.265876 0.362062 2.001470 11.00000 -1.50000 H2TB 2 0.296989 0.382685 1.903384 11.00000 -1.50000 H2TC 2 0.328614 0.300708 1.990566 11.00000 -1.50000 AFIX 0 O1B 4 0.617170 0.486284 2.155803 11.00000 0.03208 0.04541 = 0.03706 -0.00865 0.00882 0.00870 C2B 1 0.673445 0.432181 2.174912 11.00000 0.02968 0.03293 = 0.03300 0.00143 0.01194 0.00173 C3B 1 0.752876 0.441686 2.308270 11.00000 0.03398 0.04892 = 0.03801 -0.00028 0.01118 0.00558 F4B 5 0.788901 0.516833 2.318090 11.00000 0.05493 0.07362 = 0.08102 -0.00199 -0.00015 -0.02282 F5B 5 0.736971 0.438588 2.405394 11.00000 0.05581 0.13964 = 0.03236 -0.00332 0.01670 0.01014 F6B 5 0.812052 0.385223 2.335986 11.00000 0.04674 0.09286 = 0.05152 -0.00231 0.00291 0.03277 C7B 1 0.669789 0.369672 2.092034 11.00000 0.03481 0.03762 = 0.03849 0.00208 0.01455 0.01121 AFIX 43 H7BA 2 0.715951 0.333843 2.122380 11.00000 -1.20000 AFIX 0 C8B 1 0.600311 0.355677 1.962719 11.00000 0.03738 0.02961 = 0.04152 -0.00113 0.02055 0.00173 C9B 1 0.604689 0.285625 1.879067 11.00000 0.03986 0.03738 = 0.04748 -0.00792 0.02012 0.00552 C10B 1 0.678571 0.295073 1.855708 11.00000 0.05894 0.07229 = 0.07000 -0.02240 0.03637 -0.00085 AFIX 33 H10D 2 0.730461 0.284732 1.936841 11.00000 -1.50000 H10E 2 0.672524 0.254965 1.790178 11.00000 -1.50000 H10F 2 0.678943 0.351433 1.825494 11.00000 -1.50000 AFIX 0 C11B 1 0.604147 0.197739 1.934257 11.00000 0.08373 0.03778 = 0.07915 -0.00355 0.03744 0.00992 AFIX 33 H11D 2 0.656568 0.188600 2.015065 11.00000 -1.50000 H11E 2 0.558725 0.194480 1.951175 11.00000 -1.50000 H11F 2 0.596808 0.155173 1.871046 11.00000 -1.50000 AFIX 0 N12B 3 0.525531 0.301306 1.755845 11.00000 0.04695 0.04111 = 0.04668 -0.01639 0.01946 0.00039 O13B 4 0.502705 0.261551 1.648055 11.00000 0.06903 0.05067 = 0.05225 -0.02231 0.02676 -0.00330 C14B 1 0.475108 0.369243 1.767521 11.00000 0.03953 0.04113 = 0.04111 -0.01319 0.01456 -0.00058 C15B 1 0.393607 0.330849 1.748368 11.00000 0.04452 0.06415 = 0.08497 -0.03503 0.02665 -0.01027 AFIX 33 H15D 2 0.359053 0.312155 1.658595 11.00000 -1.50000 H15E 2 0.406848 0.283533 1.806950 11.00000 -1.50000 H15F 2 0.363837 0.372796 1.767553 11.00000 -1.50000 AFIX 0 C16B 1 0.458756 0.438243 1.667661 11.00000 0.06881 0.05686 = 0.03724 -0.00557 0.01266 0.01324 AFIX 33 H16D 2 0.422586 0.416781 1.579967 11.00000 -1.50000 H16E 2 0.432188 0.485573 1.682713 11.00000 -1.50000 H16F 2 0.511138 0.456064 1.677077 11.00000 -1.50000 AFIX 0 N17B 3 0.530615 0.399059 1.904488 11.00000 0.03415 0.02985 = 0.03536 -0.00485 0.01320 0.00112 HKLF 4 REM z699s in P2(1)/c REM R1 = 0.0427 for 3843 Fo > 4sig(Fo) and 0.1077 for all 7881 data REM 370 parameters refined using 0 restraints END WGHT 0.0651 0.0000 REM Instructions for potential hydrogen bonds HTAB O1S O13A_$1 EQIV $3 -x, -y+1, -z+2 HTAB C15A O1A_$3 EQIV $4 -x+1, -y+1, -z+4 HTAB C16A F5B_$4 HTAB C16A O1A_$3 HTAB O1T O13B_$2 HTAB C15B O1B_$4 HTAB C16B O1B_$4 REM Highest difference peak 0.406, deepest hole -0.526, 1-sigma level 0.059 Q1 1 -0.2782 0.4980 0.6747 11.00000 0.05 0.38 Q2 1 -0.2688 0.5095 0.6330 11.00000 0.05 0.38 Q3 1 0.4789 0.4993 2.0867 11.00000 0.05 0.35 Q4 1 -0.3079 0.5859 0.7133 11.00000 0.05 0.34 Q5 1 0.7603 0.5084 2.3742 11.00000 0.05 0.34 Q6 1 -0.1393 0.5326 1.0679 11.00000 0.05 0.30 Q7 1 -0.2598 0.6584 0.6455 11.00000 0.05 0.29 Q8 1 -0.0201 0.5017 1.0867 11.00000 0.05 0.29 Q9 1 -0.2519 0.4687 0.6758 11.00000 0.05 0.28 Q10 1 -0.0596 0.4588 1.0049 11.00000 0.05 0.26 Q11 1 -0.0359 0.5961 1.0877 11.00000 0.05 0.26 Q12 1 0.4729 0.2422 1.6752 11.00000 0.05 0.26 Q13 1 0.0102 0.5708 1.0664 11.00000 0.05 0.25 Q14 1 0.3367 0.4190 1.8317 11.00000 0.05 0.25 Q15 1 -0.1270 0.4716 0.8299 11.00000 0.05 0.25 Q16 1 0.0291 0.7679 1.3211 11.00000 0.05 0.24 Q17 1 -0.0045 0.4397 1.0438 11.00000 0.05 0.24 Q18 1 0.5093 0.4363 1.9416 11.00000 0.05 0.23 Q19 1 -0.1006 0.4883 1.2359 11.00000 0.05 0.23 Q20 1 -0.1683 0.4382 1.0833 11.00000 0.05 0.22 ; _shelx_res_checksum 29428 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 0.0000 0.5000 1.0000 0.02855(14) Uani 1 2 d S . P . . O1S O -0.05226(14) 0.44701(12) 1.1126(2) 0.0508(6) Uani 1 1 d . . . . . H1S H -0.046(2) 0.406(2) 1.127(4) 0.061 Uiso 1 1 d . U . . . C1S C -0.1232(2) 0.4797(2) 1.1147(4) 0.0730(11) Uani 1 1 d . . . . . H1SA H -0.1340 0.4454 1.1716 0.109 Uiso 1 1 calc R U . . . H1SB H -0.1120 0.5368 1.1470 0.109 Uiso 1 1 calc R U . . . H1SC H -0.1715 0.4788 1.0269 0.109 Uiso 1 1 calc R U . . . O1A O -0.11790(11) 0.52528(12) 0.85130(18) 0.0409(5) Uani 1 1 d . . . . . C2A C -0.16266(16) 0.59153(16) 0.8296(3) 0.0346(6) Uani 1 1 d . . . . . C3A C -0.25007(18) 0.58229(19) 0.7100(3) 0.0492(7) Uani 1 1 d . . . . . F4A F -0.29249(13) 0.52087(16) 0.7268(3) 0.0956(8) Uani 1 1 d . . . . . F5A F -0.29825(12) 0.65032(14) 0.6802(2) 0.0961(8) Uani 1 1 d . . . . . F6A F -0.24822(12) 0.56262(15) 0.60260(19) 0.0864(7) Uani 1 1 d . . . . . C7A C -0.14119(16) 0.66490(16) 0.9003(3) 0.0383(6) Uani 1 1 d . . . . . H7AA H -0.1803 0.7087 0.8692 0.046 Uiso 1 1 calc R U . . . C8A C -0.06286(16) 0.67900(15) 1.0187(2) 0.0338(6) Uani 1 1 d . . . . . C9A C -0.04758(17) 0.76241(16) 1.0909(3) 0.0441(7) Uani 1 1 d . . . . . C10A C -0.0374(3) 0.8355(2) 1.0153(4) 0.0849(12) Uani 1 1 d . . . . . H10A H -0.0910 0.8484 0.9386 0.127 Uiso 1 1 calc R U . . . H10B H -0.0166 0.8845 1.0713 0.127 Uiso 1 1 calc R U . . . H10C H 0.0016 0.8196 0.9885 0.127 Uiso 1 1 calc R U . . . C11A C -0.1119(2) 0.7829(2) 1.1298(4) 0.0832(13) Uani 1 1 d . . . . . H11A H -0.1649 0.7958 1.0520 0.125 Uiso 1 1 calc R U . . . H11B H -0.1184 0.7350 1.1738 0.125 Uiso 1 1 calc R U . . . H11C H -0.0931 0.8308 1.1881 0.125 Uiso 1 1 calc R U . . . N12A N 0.03341(15) 0.74256(14) 1.2074(2) 0.0536(7) Uani 1 1 d . . . . . O13A O 0.07175(16) 0.79019(15) 1.3089(3) 0.0887(9) Uani 1 1 d . . . . . C14A C 0.06791(17) 0.65964(16) 1.1999(3) 0.0448(7) Uani 1 1 d . . . . . C15A C 0.14648(18) 0.67319(19) 1.1917(4) 0.0661(10) Uani 1 1 d . . . . . H15A H 0.1905 0.6959 1.2740 0.099 Uiso 1 1 calc R U . . . H15B H 0.1643 0.6201 1.1745 0.099 Uiso 1 1 calc R U . . . H15C H 0.1342 0.7122 1.1216 0.099 Uiso 1 1 calc R U . . . C16A C 0.0841(2) 0.6065(2) 1.3177(3) 0.0655(10) Uani 1 1 d . . . . . H16A H 0.1296 0.6307 1.3970 0.098 Uiso 1 1 calc R U . . . H16B H 0.0343 0.6051 1.3237 0.098 Uiso 1 1 calc R U . . . H16C H 0.0987 0.5499 1.3071 0.098 Uiso 1 1 calc R U . . . N17A N -0.00163(12) 0.62478(12) 1.0755(2) 0.0318(5) Uani 1 1 d . . . . . Co2 Co 0.5000 0.5000 2.0000 0.03071(14) Uani 1 2 d S . P . . O1T O 0.45619(14) 0.40538(12) 2.0808(2) 0.0532(6) Uani 1 1 d . . . . . H1T H 0.473(2) 0.365(2) 2.104(4) 0.064 Uiso 1 1 d . U . . . C1T C 0.3835(2) 0.4061(2) 2.0917(4) 0.0661(10) Uani 1 1 d . . . . . H1TA H 0.3662 0.4644 2.0896 0.079 Uiso 1 1 calc R U . . . H1TB H 0.3978 0.3825 2.1767 0.079 Uiso 1 1 calc R U . . . C2T C 0.3127(3) 0.3589(3) 1.9879(5) 0.0941(13) Uani 1 1 d . . . . . H2TA H 0.2659 0.3621 2.0015 0.141 Uiso 1 1 calc R U . . . H2TB H 0.2970 0.3827 1.9034 0.141 Uiso 1 1 calc R U . . . H2TC H 0.3286 0.3007 1.9906 0.141 Uiso 1 1 calc R U . . . O1B O 0.61717(12) 0.48628(11) 2.15580(19) 0.0423(5) Uani 1 1 d . . . . . C2B C 0.67345(15) 0.43218(15) 2.1749(3) 0.0338(6) Uani 1 1 d . . . . . C3B C 0.75288(17) 0.44169(18) 2.3083(3) 0.0437(7) Uani 1 1 d . . . . . F4B F 0.78890(13) 0.51683(14) 2.3181(2) 0.0861(8) Uani 1 1 d . . . . . F5B F 0.73697(12) 0.43859(15) 2.40539(18) 0.0787(6) Uani 1 1 d . . . . . F6B F 0.81205(11) 0.38522(13) 2.33599(18) 0.0740(6) Uani 1 1 d . . . . . C7B C 0.66979(16) 0.36967(16) 2.0920(3) 0.0389(6) Uani 1 1 d . . . . . H7BA H 0.7160 0.3338 2.1224 0.047 Uiso 1 1 calc R U . . . C8B C 0.60031(16) 0.35568(15) 1.9627(3) 0.0360(6) Uani 1 1 d . . . . . C9B C 0.60469(17) 0.28563(16) 1.8791(3) 0.0426(7) Uani 1 1 d . . . . . C10B C 0.6786(2) 0.2951(2) 1.8557(3) 0.0655(9) Uani 1 1 d . . . . . H10D H 0.7305 0.2847 1.9368 0.098 Uiso 1 1 calc R U . . . H10E H 0.6725 0.2550 1.7902 0.098 Uiso 1 1 calc R U . . . H10F H 0.6789 0.3514 1.8255 0.098 Uiso 1 1 calc R U . . . C11B C 0.6041(2) 0.19774(18) 1.9343(4) 0.0689(10) Uani 1 1 d . . . . . H11D H 0.6566 0.1886 2.0151 0.103 Uiso 1 1 calc R U . . . H11E H 0.5587 0.1945 1.9512 0.103 Uiso 1 1 calc R U . . . H11F H 0.5968 0.1552 1.8710 0.103 Uiso 1 1 calc R U . . . N12B N 0.52553(14) 0.30131(14) 1.7558(2) 0.0470(6) Uani 1 1 d . . . . . O13B O 0.50271(13) 0.26155(13) 1.6481(2) 0.0593(6) Uani 1 1 d . . . . . C14B C 0.47511(17) 0.36924(17) 1.7675(3) 0.0434(7) Uani 1 1 d . . . . . C15B C 0.39361(19) 0.3308(2) 1.7484(4) 0.0676(10) Uani 1 1 d . . . . . H15D H 0.3591 0.3122 1.6586 0.101 Uiso 1 1 calc R U . . . H15E H 0.4068 0.2835 1.8069 0.101 Uiso 1 1 calc R U . . . H15F H 0.3638 0.3728 1.7676 0.101 Uiso 1 1 calc R U . . . C16B C 0.4588(2) 0.43824(19) 1.6677(3) 0.0611(9) Uani 1 1 d . . . . . H16D H 0.4226 0.4168 1.5800 0.092 Uiso 1 1 calc R U . . . H16E H 0.4322 0.4856 1.6827 0.092 Uiso 1 1 calc R U . . . H16F H 0.5111 0.4561 1.6771 0.092 Uiso 1 1 calc R U . . . N17B N 0.53062(13) 0.39906(12) 1.9045(2) 0.0353(5) Uani 1 1 d . . . . . 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 0.0295(3) 0.0245(2) 0.0286(3) -0.00118(19) 0.0128(2) 0.00155(18) O1S 0.0644(14) 0.0356(11) 0.0709(15) 0.0125(11) 0.0480(12) 0.0070(10) C1S 0.084(3) 0.067(2) 0.100(3) 0.023(2) 0.071(3) 0.0139(19) O1A 0.0338(10) 0.0373(9) 0.0372(11) -0.0068(8) 0.0078(8) 0.0058(8) C2A 0.0332(14) 0.0384(14) 0.0301(14) 0.0034(11) 0.0147(11) 0.0057(11) C3A 0.0374(17) 0.0510(18) 0.0467(19) -0.0012(14) 0.0127(14) 0.0071(14) F4A 0.0457(12) 0.1058(17) 0.105(2) 0.0111(15) 0.0170(12) -0.0207(12) F5A 0.0567(12) 0.0841(15) 0.0831(16) -0.0100(12) -0.0103(11) 0.0344(11) F6A 0.0595(13) 0.136(2) 0.0391(12) -0.0240(12) 0.0074(10) 0.0047(12) C7A 0.0389(15) 0.0354(14) 0.0364(15) 0.0021(11) 0.0162(12) 0.0090(11) C8A 0.0393(15) 0.0310(12) 0.0331(14) -0.0006(11) 0.0200(12) 0.0029(11) C9A 0.0501(18) 0.0314(14) 0.0459(17) -0.0055(12) 0.0210(14) 0.0088(12) C10A 0.107(3) 0.0362(18) 0.085(3) 0.0028(18) 0.031(2) -0.0055(19) C11A 0.067(2) 0.091(3) 0.095(3) -0.042(2) 0.044(2) 0.007(2) N12A 0.0566(16) 0.0372(13) 0.0494(15) -0.0182(11) 0.0144(13) 0.0070(11) O13A 0.0883(18) 0.0603(14) 0.0705(17) -0.0394(13) 0.0069(14) 0.0119(13) C14A 0.0494(17) 0.0331(14) 0.0400(17) -0.0108(12) 0.0143(14) 0.0022(12) C15A 0.0402(18) 0.0503(18) 0.089(3) -0.0231(18) 0.0192(17) -0.0113(14) C16A 0.085(3) 0.056(2) 0.0326(17) -0.0035(14) 0.0144(17) 0.0234(17) N17A 0.0326(11) 0.0267(10) 0.0311(12) -0.0028(9) 0.0128(9) 0.0009(9) Co2 0.0269(3) 0.0280(3) 0.0319(3) -0.00185(19) 0.0113(2) 0.00228(19) O1T 0.0562(14) 0.0368(11) 0.0783(16) 0.0143(11) 0.0430(13) 0.0073(10) C1T 0.071(2) 0.0513(19) 0.097(3) 0.0048(19) 0.058(2) -0.0019(17) C2T 0.082(3) 0.096(3) 0.107(4) 0.018(3) 0.051(3) 0.000(3) O1B 0.0321(10) 0.0454(11) 0.0371(11) -0.0087(8) 0.0088(8) 0.0087(8) C2B 0.0297(14) 0.0329(13) 0.0330(14) 0.0014(11) 0.0119(11) 0.0017(11) C3B 0.0340(16) 0.0489(17) 0.0380(16) -0.0003(13) 0.0112(13) 0.0056(13) F4B 0.0549(13) 0.0736(13) 0.0810(16) -0.0020(12) -0.0002(11) -0.0228(10) F5B 0.0558(12) 0.140(2) 0.0324(10) -0.0033(11) 0.0167(9) 0.0101(12) F6B 0.0467(10) 0.0929(15) 0.0515(11) -0.0023(10) 0.0029(9) 0.0328(10) C7B 0.0348(14) 0.0376(14) 0.0385(15) 0.0021(12) 0.0146(12) 0.0112(11) C8B 0.0374(15) 0.0296(13) 0.0415(16) -0.0011(11) 0.0205(13) 0.0017(11) C9B 0.0399(16) 0.0374(14) 0.0475(17) -0.0079(12) 0.0201(14) 0.0055(12) C10B 0.059(2) 0.072(2) 0.070(2) -0.0224(18) 0.0364(19) -0.0009(17) C11B 0.084(3) 0.0378(17) 0.079(3) -0.0036(17) 0.037(2) 0.0099(16) N12B 0.0469(14) 0.0411(13) 0.0467(15) -0.0164(11) 0.0195(12) 0.0004(11) O13B 0.0690(15) 0.0507(12) 0.0523(13) -0.0223(10) 0.0268(11) -0.0033(10) C14B 0.0395(16) 0.0411(15) 0.0411(16) -0.0132(13) 0.0146(13) -0.0006(12) C15B 0.0445(18) 0.064(2) 0.085(3) -0.0350(19) 0.0267(18) -0.0103(16) C16B 0.069(2) 0.057(2) 0.0372(18) -0.0056(14) 0.0127(16) 0.0132(16) N17B 0.0342(12) 0.0298(11) 0.0354(12) -0.0049(9) 0.0132(10) 0.0011(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' 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' F F 0.0171 0.0103 '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 O1A Co1 O1A 180.0 3_567 . ? O1A Co1 O1S 90.88(9) 3_567 . ? O1A Co1 O1S 89.12(9) . . ? O1A Co1 O1S 89.12(9) 3_567 3_567 ? O1A Co1 O1S 90.88(9) . 3_567 ? O1S Co1 O1S 180.0 . 3_567 ? O1A Co1 N17A 86.56(7) 3_567 3_567 ? O1A Co1 N17A 93.44(7) . 3_567 ? O1S Co1 N17A 90.28(8) . 3_567 ? O1S Co1 N17A 89.72(8) 3_567 3_567 ? O1A Co1 N17A 93.44(7) 3_567 . ? O1A Co1 N17A 86.56(7) . . ? O1S Co1 N17A 89.72(8) . . ? O1S Co1 N17A 90.28(8) 3_567 . ? N17A Co1 N17A 180.0 3_567 . ? C1S O1S Co1 125.14(19) . . ? C2A O1A Co1 129.66(17) . . ? O1A C2A C7A 128.2(2) . . ? O1A C2A C3A 112.5(2) . . ? C7A C2A C3A 119.3(2) . . ? F4A C3A F5A 105.3(3) . . ? F4A C3A F6A 106.2(3) . . ? F5A C3A F6A 106.4(3) . . ? F4A C3A C2A 111.4(3) . . ? F5A C3A C2A 115.0(2) . . ? F6A C3A C2A 112.0(2) . . ? C2A C7A C8A 124.3(2) . . ? N17A C8A C7A 125.7(2) . . ? N17A C8A C9A 115.0(2) . . ? C7A C8A C9A 119.3(2) . . ? N12A C9A C11A 110.5(3) . . ? N12A C9A C8A 98.5(2) . . ? C11A C9A C8A 114.0(3) . . ? N12A C9A C10A 109.7(3) . . ? C11A C9A C10A 111.5(3) . . ? C8A C9A C10A 111.9(3) . . ? O13A N12A C9A 124.4(2) . . ? O13A N12A C14A 121.9(2) . . ? C9A N12A C14A 113.7(2) . . ? N17A C14A C16A 111.5(2) . . ? N17A C14A N12A 101.9(2) . . ? C16A C14A N12A 108.9(2) . . ? N17A C14A C15A 111.4(2) . . ? C16A C14A C15A 112.9(3) . . ? N12A C14A C15A 109.6(2) . . ? C8A N17A C14A 110.6(2) . . ? C8A N17A Co1 125.44(16) . . ? C14A N17A Co1 123.95(15) . . ? O1B Co2 O1B 180.0 . 3_669 ? O1B Co2 O1T 90.23(9) . 3_669 ? O1B Co2 O1T 89.77(9) 3_669 3_669 ? O1B Co2 O1T 89.77(9) . . ? O1B Co2 O1T 90.23(9) 3_669 . ? O1T Co2 O1T 180.00(11) 3_669 . ? O1B Co2 N17B 92.95(8) . 3_669 ? O1B Co2 N17B 87.05(8) 3_669 3_669 ? O1T Co2 N17B 88.71(9) 3_669 3_669 ? O1T Co2 N17B 91.29(9) . 3_669 ? O1B Co2 N17B 87.05(8) . . ? O1B Co2 N17B 92.95(8) 3_669 . ? O1T Co2 N17B 91.29(9) 3_669 . ? O1T Co2 N17B 88.71(9) . . ? N17B Co2 N17B 180.0 3_669 . ? C1T O1T Co2 128.96(18) . . ? O1T C1T C2T 114.0(3) . . ? C2B O1B Co2 129.42(17) . . ? O1B C2B C7B 128.4(2) . . ? O1B C2B C3B 112.8(2) . . ? C7B C2B C3B 118.7(2) . . ? F6B C3B F4B 105.4(3) . . ? F6B C3B F5B 106.7(2) . . ? F4B C3B F5B 106.3(3) . . ? F6B C3B C2B 115.6(2) . . ? F4B C3B C2B 110.7(2) . . ? F5B C3B C2B 111.5(2) . . ? C2B C7B C8B 124.4(2) . . ? N17B C8B C7B 126.2(2) . . ? N17B C8B C9B 114.3(2) . . ? C7B C8B C9B 119.5(2) . . ? N12B C9B C8B 99.3(2) . . ? N12B C9B C11B 110.7(2) . . ? C8B C9B C11B 111.8(2) . . ? N12B C9B C10B 109.7(2) . . ? C8B C9B C10B 113.4(2) . . ? C11B C9B C10B 111.4(2) . . ? O13B N12B C9B 123.8(2) . . ? O13B N12B C14B 123.2(2) . . ? C9B N12B C14B 113.0(2) . . ? N17B C14B N12B 102.4(2) . . ? N17B C14B C16B 111.7(2) . . ? N12B C14B C16B 109.5(3) . . ? N17B C14B C15B 111.6(3) . . ? N12B C14B C15B 108.7(2) . . ? C16B C14B C15B 112.4(3) . . ? C8B N17B C14B 110.7(2) . . ? C8B N17B Co2 124.07(18) . . ? C14B N17B Co2 125.18(16) . . ? 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 O1A 2.018(2) 3_567 ? Co1 O1A 2.018(2) . ? Co1 O1S 2.171(2) . ? Co1 O1S 2.171(2) 3_567 ? Co1 N17A 2.1685(19) 3_567 ? Co1 N17A 2.1685(19) . ? O1S C1S 1.423(4) . ? O1A C2A 1.276(3) . ? C2A C7A 1.362(3) . ? C2A C3A 1.512(4) . ? C3A F4A 1.325(4) . ? C3A F5A 1.323(3) . ? C3A F6A 1.321(4) . ? C7A C8A 1.422(4) . ? C8A N17A 1.299(3) . ? C8A C9A 1.514(3) . ? C9A N12A 1.456(4) . ? C9A C11A 1.513(4) . ? C9A C10A 1.528(4) . ? N12A O13A 1.276(3) . ? N12A C14A 1.479(3) . ? C14A N17A 1.475(3) . ? C14A C16A 1.515(4) . ? C14A C15A 1.521(4) . ? Co2 O1B 2.010(2) . ? Co2 O1B 2.010(2) 3_669 ? Co2 O1T 2.142(2) 3_669 ? Co2 O1T 2.142(2) . ? Co2 N17B 2.187(2) 3_669 ? Co2 N17B 2.187(2) . ? O1T C1T 1.416(4) . ? C1T C2T 1.458(5) . ? O1B C2B 1.275(3) . ? C2B C7B 1.366(4) . ? C2B C3B 1.511(4) . ? C3B F6B 1.317(3) . ? C3B F4B 1.337(3) . ? C3B F5B 1.321(3) . ? C7B C8B 1.420(4) . ? C8B N17B 1.303(3) . ? C8B C9B 1.511(4) . ? C9B N12B 1.461(3) . ? C9B C11B 1.535(4) . ? C9B C10B 1.535(4) . ? N12B O13B 1.279(3) . ? N12B C14B 1.474(3) . ? C14B N17B 1.477(3) . ? C14B C16B 1.516(4) . ? C14B C15B 1.532(4) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1S H1S O13A 0.67(3) 2.12(3) 2.732(3) 152(4) 2_547 O1T H1T O13B 0.70(3) 2.07(3) 2.760(3) 171(4) 4_566