#------------------------------------------------------------------------------ #$Date: 2019-08-14 03:28:12 +0300 (Wed, 14 Aug 2019) $ #$Revision: 217516 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/22/1552220.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_1552220 loop_ _publ_author_name 'Gransbury, Gemma K.' 'Boulon, Marie-Emmanuelle' 'Mole, Richard A.' 'Gable, Robert W.' 'Moubaraki, Boujemaa' 'Murray, Keith S.' 'Sorace, Lorenzo' 'Soncini, Alessandro' 'Boskovic, Colette' _publ_section_title ; Single-ion anisotropy and exchange coupling in cobalt(ii)-radical complexes: insights from magnetic and ab initio studies ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/C9SC00914K _journal_year 2019 _chemical_formula_moiety 'C27 H24 Br4 Co0.06 N4 O2 Zn0.94' _chemical_formula_sum 'C27 H24 Br4 Co0.06 N4 O2 Zn0.94' _chemical_formula_weight 821.12 _chemical_name_systematic (3,4,5,6-tetrabromocatecholato)-(tris(6-methyl-2-pyridylmethyl)amine)-cobalt(II):zinc(II) _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_block_doi 10.5517/ccdc.csd.cc21n7xw _audit_creation_date 2018-03-05 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2019-08-07 deposited with the CCDC. 2019-08-13 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.5500(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.3060(2) _cell_length_b 13.5277(2) _cell_length_c 18.5746(3) _cell_measurement_reflns_used 11416 _cell_measurement_temperature 130.00(10) _cell_measurement_theta_max 76.8690 _cell_measurement_theta_min 4.0250 _cell_volume 2838.06(8) _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 130.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.2273 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.9969 _diffrn_measured_fraction_theta_max 0.9887 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -50.00 10.00 1.00 1.00 -- -40.81 38.00 90.00 60 2 \w -46.00 25.00 1.00 1.00 -- -40.81 38.00 -90.00 71 3 \w 23.00 91.00 1.00 1.00 -- 40.81-125.00 0.00 68 4 \w 35.00 116.00 1.00 2.50 -- 113.00-111.00 -60.00 81 5 \w 77.00 105.00 1.00 2.50 -- 113.00 -94.00-150.00 28 6 \w 39.00 72.00 1.00 2.50 -- 113.00 -30.00 -60.00 33 7 \w 34.00 144.00 1.00 2.50 -- 113.00 -77.00 -30.00 110 8 \w 90.00 116.00 1.00 2.50 -- 113.00-111.00 60.00 26 9 \w 42.00 143.00 1.00 2.50 -- 113.00 -61.00 120.00 101 10 \w 85.00 177.00 1.00 2.50 -- 113.00 45.00 120.00 92 11 \w 105.00 177.00 1.00 2.50 -- 113.00 111.00 60.00 72 12 \w 97.00 178.00 1.00 2.50 -- 113.00 30.00-120.00 81 13 \w 82.00 178.00 1.00 2.50 -- 113.00 30.00-180.00 96 14 \w 39.00 86.00 1.00 1.00 -- 40.81-125.00-180.00 47 15 \w 30.00 58.00 1.00 2.50 -- 113.00 -94.00-150.00 28 16 \w 37.00 68.00 1.00 2.50 -- 113.00-111.00 60.00 31 17 \w 38.00 116.00 1.00 2.50 -- 113.00-111.00 150.00 78 18 \w 58.00 123.00 1.00 2.50 -- 113.00 178.00 150.00 65 19 \w -122.00 -5.00 1.00 1.00 -- -40.81 -19.00 90.00 117 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0540835000 _diffrn_orient_matrix_UB_12 -0.1008685000 _diffrn_orient_matrix_UB_13 -0.0186044000 _diffrn_orient_matrix_UB_21 0.0573640000 _diffrn_orient_matrix_UB_22 0.0466672000 _diffrn_orient_matrix_UB_23 -0.0656021000 _diffrn_orient_matrix_UB_31 0.1112307000 _diffrn_orient_matrix_UB_32 0.0249650000 _diffrn_orient_matrix_UB_33 0.0473826000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_unetI/netI 0.0247 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 20997 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 77.061 _diffrn_reflns_theta_min 4.044 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 8.279 _exptl_absorpt_correction_T_max 0.540 _exptl_absorpt_correction_T_min 0.224 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear orange' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.922 _exptl_crystal_description block _exptl_crystal_F_000 1599.3 _exptl_crystal_recrystallization_method 'Crystallised from hot DMF/diethyl ether (1:2)' _exptl_crystal_size_max 0.255 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.105 _refine_diff_density_max 0.418 _refine_diff_density_min -0.700 _refine_diff_density_rms 0.079 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 347 _refine_ls_number_reflns 5938 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.067 _refine_ls_R_factor_all 0.0255 _refine_ls_R_factor_gt 0.0237 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+1.3943P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0622 _refine_ls_wR_factor_ref 0.0634 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5622 _reflns_number_total 5938 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc00914k2.cif _cod_data_source_block 1-co5-zn95 _cod_database_code 1552220 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula 'C27 H24 Br4 Co0.047 N4 O2 Zn0.953' _chemical_oxdiff_usercomment 'Co-doped Zn roughly 0.05. orange block' _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_estimated_absorpt_t_max 0.477 _shelx_estimated_absorpt_t_min 0.227 _reflns_odcompleteness_completeness 99.69 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 75.12 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Shared sites {Zn1, Co} 3. Uiso/Uaniso restraints and constraints Uanis(Zn1) = Uanis(Co) 4. Others Sof(Co)=1-FVAR(1) Sof(Zn1)=FVAR(1) 5.a Secondary CH2 refined with riding coordinates: C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B) 5.b Aromatic/amide H refined with riding coordinates: C8(H8), C9(H9), C10(H10), C14(H14), C15(H15), C16(H16), C20(H20), C21(H21), C22(H22) 5.c Idealised Me refined as rotating group: C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C) ; _shelx_res_file ; 1-co5-zn95.res created by SHELXL-2014/7 TITL 1-Co5-Zn95_a.res in P2(1)/n REM Old TITL GG2-077-reproc-gau in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.113, Rweak 0.007, Alpha 0.020, Orientation as input REM Formula found by SHELXT: C28 N3 O2 Co Br4 CELL 1.54184 11.306 13.5277 18.5746 90 92.55 90 ZERR 4 0.0002 0.0002 0.0003 0 0.001 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Br Co N O Zn UNIT 108 96 16 0.24 16 8 3.76 EADP Zn1 Co EXYZ Zn1 Co L.S. 20 PLAN 5 SIZE 0.105 0.15 0.255 BOND $H list 4 fmap 2 acta REM REM REM WGHT 0.034200 1.394300 FVAR 0.25805 0.93909 BR1 3 0.970759 0.411535 0.606154 11.00000 0.02479 0.03134 = 0.04428 -0.00901 0.01027 -0.00614 BR2 3 0.984460 0.226328 0.490369 11.00000 0.03431 0.03451 = 0.03453 -0.00380 0.01958 0.00088 BR3 3 0.755805 0.075314 0.467851 11.00000 0.03835 0.02660 = 0.02154 -0.00740 0.00603 0.00261 BR4 3 0.514744 0.116018 0.561111 11.00000 0.02354 0.02723 = 0.02535 -0.00586 -0.00219 -0.00227 PART 1 ZN1 7 0.573127 0.404689 0.725150 21.00000 0.01977 0.02135 = 0.02177 -0.00566 0.00368 0.00068 PART 0 PART 2 CO 4 0.573127 0.404689 0.725150 -21.00000 0.01977 0.02135 = 0.02177 -0.00566 0.00368 0.00068 PART 0 O1 6 0.542665 0.299596 0.652949 11.00000 0.02018 0.02460 = 0.02225 -0.00564 0.00322 0.00055 O2 6 0.734579 0.414691 0.677693 11.00000 0.02182 0.02497 = 0.02920 -0.00847 0.00767 -0.00179 N1 5 0.630754 0.511862 0.803554 11.00000 0.02097 0.01916 = 0.02293 -0.00285 0.00418 -0.00183 N2 5 0.401494 0.431826 0.777270 11.00000 0.01968 0.01921 = 0.02359 -0.00045 0.00478 0.00084 N3 5 0.647901 0.311445 0.819495 11.00000 0.01881 0.02335 = 0.02211 -0.00327 0.00210 0.00170 N4 5 0.513042 0.554331 0.670924 11.00000 0.02832 0.02459 = 0.02566 0.00464 0.00670 0.00291 C1 1 0.638519 0.280593 0.618151 11.00000 0.02087 0.02085 = 0.01648 0.00065 0.00051 0.00336 C2 1 0.740830 0.344356 0.630609 11.00000 0.02184 0.02085 = 0.01870 0.00001 0.00182 0.00247 C3 1 0.840422 0.324673 0.591008 11.00000 0.02223 0.02078 = 0.02230 0.00152 0.00386 -0.00017 C4 1 0.846152 0.245607 0.542535 11.00000 0.02437 0.02574 = 0.01855 0.00052 0.00684 0.00495 C5 1 0.750125 0.182778 0.532976 11.00000 0.02898 0.02081 = 0.01508 -0.00140 0.00300 0.00392 C6 1 0.647483 0.201370 0.571083 11.00000 0.02238 0.02143 = 0.01580 0.00040 -0.00104 0.00055 C7 1 0.292111 0.409903 0.750226 11.00000 0.02284 0.02172 = 0.02720 0.00136 0.00387 0.00009 C8 1 0.195221 0.469739 0.764466 11.00000 0.02126 0.02875 = 0.03147 0.00424 0.00339 0.00231 AFIX 43 H8 2 0.120283 0.453800 0.745243 11.00000 -1.20000 AFIX 0 C9 1 0.211061 0.552545 0.807133 11.00000 0.02477 0.02450 = 0.02914 0.00435 0.00738 0.00598 AFIX 43 H9 2 0.147818 0.594386 0.815387 11.00000 -1.20000 AFIX 0 C10 1 0.323020 0.572467 0.837595 11.00000 0.02946 0.01795 = 0.02477 0.00201 0.00706 0.00426 AFIX 43 H10 2 0.335590 0.626407 0.868022 11.00000 -1.20000 AFIX 0 C11 1 0.415324 0.510249 0.821630 11.00000 0.02328 0.01932 = 0.01987 0.00216 0.00622 0.00138 C12 1 0.537570 0.524272 0.856092 11.00000 0.02552 0.02269 = 0.02183 -0.00505 0.00410 0.00146 AFIX 23 H12A 2 0.543446 0.589926 0.876941 11.00000 -1.20000 H12B 2 0.549949 0.476641 0.894730 11.00000 -1.20000 AFIX 0 C13 1 0.633327 0.215781 0.836304 11.00000 0.02247 0.02328 = 0.02578 -0.00093 0.00524 0.00255 C14 1 0.699471 0.171166 0.892807 11.00000 0.02974 0.02814 = 0.03121 0.00354 0.00637 0.00700 AFIX 43 H14 2 0.690804 0.104127 0.902334 11.00000 -1.20000 AFIX 0 C15 1 0.777927 0.227985 0.934337 11.00000 0.03112 0.04056 = 0.02851 0.00248 -0.00238 0.01229 AFIX 43 H15 2 0.822222 0.199724 0.972384 11.00000 -1.20000 AFIX 0 C16 1 0.789734 0.327098 0.918674 11.00000 0.02683 0.03643 = 0.02933 -0.00586 -0.00512 0.00552 AFIX 43 H16 2 0.840336 0.367095 0.946719 11.00000 -1.20000 AFIX 0 C17 1 0.724677 0.365827 0.860321 11.00000 0.02077 0.02462 = 0.02454 -0.00535 0.00271 0.00367 C18 1 0.740912 0.471632 0.837793 11.00000 0.02093 0.02448 = 0.02808 -0.00609 -0.00068 -0.00180 AFIX 23 H18A 2 0.763835 0.511148 0.879700 11.00000 -1.20000 H18B 2 0.803961 0.475493 0.804154 11.00000 -1.20000 AFIX 0 C19 1 0.430956 0.573778 0.618294 11.00000 0.03275 0.03642 = 0.02882 0.00941 0.00470 0.00443 C20 1 0.390118 0.670411 0.605614 11.00000 0.04415 0.04069 = 0.04393 0.01641 0.00289 0.01250 AFIX 43 H20 2 0.333997 0.682830 0.568592 11.00000 -1.20000 AFIX 0 C21 1 0.433133 0.746518 0.647932 11.00000 0.05392 0.03187 = 0.05269 0.01694 0.01472 0.01648 AFIX 43 H21 2 0.405759 0.810648 0.640238 11.00000 -1.20000 AFIX 0 C22 1 0.517696 0.726905 0.702201 11.00000 0.04691 0.02281 = 0.04228 0.00478 0.01652 0.00408 AFIX 43 H22 2 0.548106 0.777198 0.731719 11.00000 -1.20000 AFIX 0 C23 1 0.555748 0.630160 0.711288 11.00000 0.03055 0.02093 = 0.02931 0.00390 0.01129 0.00099 C24 1 0.654675 0.604376 0.765329 11.00000 0.03232 0.02017 = 0.03303 -0.00083 0.00480 -0.00773 AFIX 23 H24A 2 0.728024 0.597762 0.740584 11.00000 -1.20000 H24B 2 0.664539 0.657657 0.800026 11.00000 -1.20000 AFIX 0 C25 1 0.276926 0.316767 0.707143 11.00000 0.02254 0.02674 = 0.04542 -0.00944 0.00094 -0.00092 AFIX 137 H25A 2 0.346303 0.305558 0.680302 11.00000 -1.50000 H25B 2 0.209129 0.322982 0.674466 11.00000 -1.50000 H25C 2 0.265615 0.262089 0.739056 11.00000 -1.50000 AFIX 0 C26 1 0.541025 0.158729 0.793410 11.00000 0.03157 0.02190 = 0.03727 0.00186 0.00117 -0.00432 AFIX 137 H26A 2 0.464461 0.172220 0.811514 11.00000 -1.50000 H26B 2 0.557534 0.089297 0.797516 11.00000 -1.50000 H26C 2 0.541947 0.178121 0.743722 11.00000 -1.50000 AFIX 0 C27 1 0.383410 0.488899 0.573726 11.00000 0.04933 0.04482 = 0.03698 0.00526 -0.01080 0.00181 AFIX 137 H27A 2 0.433768 0.432364 0.581275 11.00000 -1.50000 H27B 2 0.381171 0.506894 0.523690 11.00000 -1.50000 H27C 2 0.304882 0.473153 0.587709 11.00000 -1.50000 AFIX 0 HKLF 4 REM 1-Co5-Zn95_a.res in P2(1)/n REM R1 = 0.0237 for 5622 Fo > 4sig(Fo) and 0.0255 for all 5938 data REM 347 parameters refined using 0 restraints END WGHT 0.0342 1.3943 REM Highest difference peak 0.418, deepest hole -0.700, 1-sigma level 0.079 Q1 1 0.9422 0.2572 0.4583 11.00000 0.05 0.42 Q2 1 0.6057 0.6204 0.7362 11.00000 0.05 0.32 Q3 1 0.6026 0.4675 0.7773 11.00000 0.05 0.31 Q4 1 0.7457 0.1562 0.5039 11.00000 0.05 0.31 Q5 1 0.5754 0.0818 0.6030 11.00000 0.05 0.31 ; _shelx_res_checksum 37678 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.581 _oxdiff_exptl_absorpt_empirical_full_min 0.732 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.97076(2) 0.41154(2) 0.60615(2) 0.03321(7) Uani 1 1 d . . . . Br2 Br 0.98446(2) 0.22633(2) 0.49037(2) 0.03392(7) Uani 1 1 d . . . . Br3 Br 0.75580(2) 0.07531(2) 0.46785(2) 0.02869(6) Uani 1 1 d . . . . Br4 Br 0.51474(2) 0.11602(2) 0.56111(2) 0.02547(6) Uani 1 1 d . . . . Zn1 Zn 0.57313(2) 0.40469(2) 0.72515(2) 0.02088(12) Uani 0.939(10) 1 d . P A 1 Co Co 0.57313(2) 0.40469(2) 0.72515(2) 0.02088(12) Uani 0.061(10) 1 d . P A 2 O1 O 0.54266(12) 0.29960(11) 0.65295(8) 0.0223(3) Uani 1 1 d . . . . O2 O 0.73458(13) 0.41469(11) 0.67769(8) 0.0251(3) Uani 1 1 d . . . . N1 N 0.63075(14) 0.51186(13) 0.80355(9) 0.0209(3) Uani 1 1 d . . . . N2 N 0.40149(15) 0.43183(13) 0.77727(9) 0.0207(3) Uani 1 1 d . . . . N3 N 0.64790(14) 0.31144(13) 0.81949(9) 0.0214(3) Uani 1 1 d . . . . N4 N 0.51304(16) 0.55433(14) 0.67092(10) 0.0260(4) Uani 1 1 d . . . . C1 C 0.63852(17) 0.28059(15) 0.61815(10) 0.0194(4) Uani 1 1 d . . . . C2 C 0.74083(17) 0.34436(15) 0.63061(10) 0.0204(4) Uani 1 1 d . . . . C3 C 0.84042(17) 0.32467(15) 0.59101(11) 0.0217(4) Uani 1 1 d . . . . C4 C 0.84615(18) 0.24561(16) 0.54253(11) 0.0227(4) Uani 1 1 d . . . . C5 C 0.75012(18) 0.18278(15) 0.53298(10) 0.0216(4) Uani 1 1 d . . . . C6 C 0.64748(17) 0.20137(15) 0.57108(10) 0.0199(4) Uani 1 1 d . . . . C7 C 0.29211(19) 0.40990(15) 0.75023(12) 0.0238(4) Uani 1 1 d . . . . C8 C 0.19522(18) 0.46974(17) 0.76447(12) 0.0271(4) Uani 1 1 d . . . . H8 H 0.1203 0.4538 0.7452 0.033 Uiso 1 1 calc R . . . C9 C 0.21106(19) 0.55254(16) 0.80713(12) 0.0260(4) Uani 1 1 d . . . . H9 H 0.1478 0.5944 0.8154 0.031 Uiso 1 1 calc R . . . C10 C 0.32302(19) 0.57247(15) 0.83759(11) 0.0239(4) Uani 1 1 d . . . . H10 H 0.3356 0.6264 0.8680 0.029 Uiso 1 1 calc R . . . C11 C 0.41532(17) 0.51025(15) 0.82163(10) 0.0207(4) Uani 1 1 d . . . . C12 C 0.53757(18) 0.52427(16) 0.85609(11) 0.0233(4) Uani 1 1 d . . . . H12A H 0.5434 0.5899 0.8769 0.028 Uiso 1 1 calc R . . . H12B H 0.5499 0.4766 0.8947 0.028 Uiso 1 1 calc R . . . C13 C 0.63333(18) 0.21578(16) 0.83630(11) 0.0237(4) Uani 1 1 d . . . . C14 C 0.6995(2) 0.17117(18) 0.89281(12) 0.0295(4) Uani 1 1 d . . . . H14 H 0.6908 0.1041 0.9023 0.035 Uiso 1 1 calc R . . . C15 C 0.7779(2) 0.2280(2) 0.93434(13) 0.0335(5) Uani 1 1 d . . . . H15 H 0.8222 0.1997 0.9724 0.040 Uiso 1 1 calc R . . . C16 C 0.7897(2) 0.32710(19) 0.91867(13) 0.0311(5) Uani 1 1 d . . . . H16 H 0.8403 0.3671 0.9467 0.037 Uiso 1 1 calc R . . . C17 C 0.72468(18) 0.36583(16) 0.86032(11) 0.0233(4) Uani 1 1 d . . . . C18 C 0.74091(17) 0.47163(16) 0.83779(11) 0.0245(4) Uani 1 1 d . . . . H18A H 0.7638 0.5111 0.8797 0.029 Uiso 1 1 calc R . . . H18B H 0.8040 0.4755 0.8042 0.029 Uiso 1 1 calc R . . . C19 C 0.4310(2) 0.57378(19) 0.61829(13) 0.0326(5) Uani 1 1 d . . . . C20 C 0.3901(3) 0.6704(2) 0.60561(16) 0.0429(6) Uani 1 1 d . . . . H20 H 0.3340 0.6828 0.5686 0.051 Uiso 1 1 calc R . . . C21 C 0.4331(3) 0.7465(2) 0.64793(17) 0.0458(7) Uani 1 1 d . . . . H21 H 0.4058 0.8106 0.6402 0.055 Uiso 1 1 calc R . . . C22 C 0.5177(2) 0.72691(18) 0.70220(15) 0.0369(5) Uani 1 1 d . . . . H22 H 0.5481 0.7772 0.7317 0.044 Uiso 1 1 calc R . . . C23 C 0.5557(2) 0.63016(16) 0.71129(12) 0.0266(4) Uani 1 1 d . . . . C24 C 0.6547(2) 0.60438(16) 0.76533(13) 0.0284(4) Uani 1 1 d . . . . H24A H 0.7280 0.5978 0.7406 0.034 Uiso 1 1 calc R . . . H24B H 0.6645 0.6577 0.8000 0.034 Uiso 1 1 calc R . . . C25 C 0.27693(19) 0.31677(18) 0.70714(14) 0.0316(5) Uani 1 1 d . . . . H25A H 0.3463 0.3056 0.6803 0.047 Uiso 1 1 calc GR . . . H25B H 0.2091 0.3230 0.6745 0.047 Uiso 1 1 calc GR . . . H25C H 0.2656 0.2621 0.7391 0.047 Uiso 1 1 calc GR . . . C26 C 0.5410(2) 0.15873(17) 0.79341(13) 0.0303(4) Uani 1 1 d . . . . H26A H 0.4645 0.1722 0.8115 0.045 Uiso 1 1 calc GR . . . H26B H 0.5575 0.0893 0.7975 0.045 Uiso 1 1 calc GR . . . H26C H 0.5419 0.1781 0.7437 0.045 Uiso 1 1 calc GR . . . C27 C 0.3834(3) 0.4889(2) 0.57373(15) 0.0441(6) Uani 1 1 d . . . . H27A H 0.4338 0.4324 0.5813 0.066 Uiso 1 1 calc GR . . . H27B H 0.3812 0.5069 0.5237 0.066 Uiso 1 1 calc GR . . . H27C H 0.3049 0.4732 0.5877 0.066 Uiso 1 1 calc GR . . . 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 Br1 0.02479(11) 0.03134(13) 0.04428(14) -0.00901(10) 0.01027(9) -0.00614(8) Br2 0.03431(13) 0.03451(13) 0.03453(13) -0.00380(9) 0.01958(10) 0.00088(9) Br3 0.03835(13) 0.02660(12) 0.02154(11) -0.00740(8) 0.00603(8) 0.00261(8) Br4 0.02354(11) 0.02723(12) 0.02535(11) -0.00586(8) -0.00219(8) -0.00227(8) Zn1 0.01977(17) 0.02135(17) 0.02177(17) -0.00566(10) 0.00368(10) 0.00068(10) Co 0.01977(17) 0.02135(17) 0.02177(17) -0.00566(10) 0.00368(10) 0.00068(10) O1 0.0202(6) 0.0246(7) 0.0222(6) -0.0056(6) 0.0032(5) 0.0006(5) O2 0.0218(7) 0.0250(7) 0.0292(7) -0.0085(6) 0.0077(6) -0.0018(5) N1 0.0210(7) 0.0192(8) 0.0229(8) -0.0029(6) 0.0042(6) -0.0018(6) N2 0.0197(7) 0.0192(8) 0.0236(8) -0.0004(6) 0.0048(6) 0.0008(6) N3 0.0188(7) 0.0234(8) 0.0221(8) -0.0033(6) 0.0021(6) 0.0017(6) N4 0.0283(9) 0.0246(9) 0.0257(8) 0.0046(7) 0.0067(7) 0.0029(7) C1 0.0209(9) 0.0208(9) 0.0165(8) 0.0007(7) 0.0005(7) 0.0034(7) C2 0.0218(9) 0.0208(9) 0.0187(8) 0.0000(7) 0.0018(7) 0.0025(7) C3 0.0222(9) 0.0208(9) 0.0223(9) 0.0015(7) 0.0039(7) -0.0002(7) C4 0.0244(9) 0.0257(10) 0.0185(9) 0.0005(8) 0.0068(7) 0.0049(8) C5 0.0290(10) 0.0208(9) 0.0151(8) -0.0014(7) 0.0030(7) 0.0039(7) C6 0.0224(9) 0.0214(9) 0.0158(8) 0.0004(7) -0.0010(7) 0.0006(7) C7 0.0228(9) 0.0217(9) 0.0272(10) 0.0014(8) 0.0039(8) 0.0001(8) C8 0.0213(9) 0.0288(11) 0.0315(10) 0.0042(9) 0.0034(8) 0.0023(8) C9 0.0248(9) 0.0245(10) 0.0291(10) 0.0044(8) 0.0074(8) 0.0060(8) C10 0.0295(10) 0.0180(9) 0.0248(9) 0.0020(7) 0.0071(8) 0.0043(8) C11 0.0233(9) 0.0193(9) 0.0199(8) 0.0022(7) 0.0062(7) 0.0014(7) C12 0.0255(9) 0.0227(10) 0.0218(9) -0.0051(7) 0.0041(7) 0.0015(8) C13 0.0225(9) 0.0233(10) 0.0258(10) -0.0009(8) 0.0052(7) 0.0025(7) C14 0.0297(10) 0.0281(11) 0.0312(11) 0.0035(9) 0.0064(8) 0.0070(8) C15 0.0311(11) 0.0406(13) 0.0285(11) 0.0025(10) -0.0024(9) 0.0123(9) C16 0.0268(10) 0.0364(12) 0.0293(11) -0.0059(9) -0.0051(8) 0.0055(9) C17 0.0208(9) 0.0246(10) 0.0245(9) -0.0053(8) 0.0027(7) 0.0037(8) C18 0.0209(9) 0.0245(10) 0.0281(10) -0.0061(8) -0.0007(7) -0.0018(7) C19 0.0328(11) 0.0364(13) 0.0288(11) 0.0094(9) 0.0047(9) 0.0044(9) C20 0.0441(14) 0.0407(15) 0.0439(14) 0.0164(12) 0.0029(11) 0.0125(11) C21 0.0539(16) 0.0319(13) 0.0527(16) 0.0169(12) 0.0147(13) 0.0165(12) C22 0.0469(14) 0.0228(11) 0.0423(13) 0.0048(10) 0.0165(11) 0.0041(10) C23 0.0305(10) 0.0209(10) 0.0293(10) 0.0039(8) 0.0113(8) 0.0010(8) C24 0.0323(11) 0.0202(10) 0.0330(11) -0.0008(8) 0.0048(9) -0.0077(8) C25 0.0225(10) 0.0267(11) 0.0454(13) -0.0094(10) 0.0009(9) -0.0009(8) C26 0.0316(11) 0.0219(10) 0.0373(11) 0.0019(9) 0.0012(9) -0.0043(8) C27 0.0493(15) 0.0448(15) 0.0370(13) 0.0053(11) -0.0108(11) 0.0018(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _citation_id _citation_doi _citation_year 1 10.1039/C9SC00914K 2019 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 1 0.0620 -1 1 -2 0.0750 0 -1 0 0.1270 0 1 0 0.1270 0 0 -1 0.0702 0 0 1 0.0702 1 -1 2 0.0750 -1 -1 -1 0.0780 1 1 1 0.0780 -1 0 -1 0.0620 -1 0 1 0.0525 1 0 -1 0.0525 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O1 Zn1 O2 83.57(6) O1 Zn1 N1 172.15(6) O1 Zn1 N2 106.48(6) O1 Zn1 N3 99.82(6) O1 Zn1 N4 106.92(7) O2 Zn1 N1 89.88(6) O2 Zn1 N2 166.78(6) O2 Zn1 N3 93.41(6) O2 Zn1 N4 90.27(6) N1 Zn1 N2 80.66(6) N1 Zn1 N3 76.18(7) N1 Zn1 N4 77.35(7) N2 Zn1 N3 93.27(6) N2 Zn1 N4 78.71(6) N3 Zn1 N4 153.25(7) O1 Co O2 83.57(6) O1 Co N1 172.15(6) O1 Co N2 106.48(6) O1 Co N3 99.82(6) O1 Co N4 106.92(7) O2 Co N1 89.88(6) O2 Co N2 166.78(6) O2 Co N3 93.41(6) O2 Co N4 90.27(6) N1 Co N2 80.66(6) N1 Co N3 76.18(7) N1 Co N4 77.35(7) N2 Co N3 93.27(6) N2 Co N4 78.71(6) N3 Co N4 153.25(7) C1 O1 Zn1 110.66(12) C1 O1 Co 110.66(12) C2 O2 Zn1 108.39(12) C2 O2 Co 108.39(12) C12 N1 Zn1 108.83(12) C12 N1 Co 108.83(12) C18 N1 Zn1 105.62(12) C18 N1 Co 105.62(12) C18 N1 C12 111.71(16) C24 N1 Zn1 107.80(13) C24 N1 Co 107.80(13) C24 N1 C12 111.98(17) C24 N1 C18 110.61(16) C7 N2 Zn1 127.02(14) C7 N2 Co 127.02(14) C7 N2 C11 118.74(17) C11 N2 Zn1 108.32(13) C11 N2 Co 108.32(13) C13 N3 Zn1 131.58(14) C13 N3 Co 131.58(14) C13 N3 C17 118.58(18) C17 N3 Zn1 109.69(14) C17 N3 Co 109.69(14) C19 N4 Zn1 131.16(17) C19 N4 Co 131.16(17) C19 N4 C23 118.3(2) C23 N4 Zn1 109.15(14) C23 N4 Co 109.15(14) O1 C1 C2 118.32(18) O1 C1 C6 123.10(18) C6 C1 C2 118.56(18) O2 C2 C1 118.44(17) O2 C2 C3 124.35(19) C3 C2 C1 117.21(18) C2 C3 Br1 116.29(15) C2 C3 C4 123.02(19) C4 C3 Br1 120.70(15) C3 C4 Br2 119.78(16) C5 C4 Br2 120.71(15) C5 C4 C3 119.52(18) C4 C5 Br3 120.30(15) C4 C5 C6 119.01(18) C6 C5 Br3 120.67(16) C1 C6 Br4 116.84(15) C1 C6 C5 122.59(19) C5 C6 Br4 120.56(15) N2 C7 C8 121.1(2) N2 C7 C25 117.76(18) C8 C7 C25 121.1(2) C7 C8 H8 120.1 C9 C8 C7 119.8(2) C9 C8 H8 120.1 C8 C9 H9 120.5 C8 C9 C10 118.95(19) C10 C9 H9 120.5 C9 C10 H10 120.8 C11 C10 C9 118.5(2) C11 C10 H10 120.8 N2 C11 C10 122.81(19) N2 C11 C12 115.93(17) C10 C11 C12 121.21(19) N1 C12 C11 111.85(16) N1 C12 H12A 109.2 N1 C12 H12B 109.2 C11 C12 H12A 109.2 C11 C12 H12B 109.2 H12A C12 H12B 107.9 N3 C13 C14 121.6(2) N3 C13 C26 117.54(19) C14 C13 C26 120.9(2) C13 C14 H14 120.4 C15 C14 C13 119.2(2) C15 C14 H14 120.4 C14 C15 H15 120.4 C16 C15 C14 119.2(2) C16 C15 H15 120.4 C15 C16 H16 120.7 C15 C16 C17 118.7(2) C17 C16 H16 120.7 N3 C17 C16 122.7(2) N3 C17 C18 116.54(18) C16 C17 C18 120.7(2) N1 C18 C17 111.06(16) N1 C18 H18A 109.4 N1 C18 H18B 109.4 C17 C18 H18A 109.4 C17 C18 H18B 109.4 H18A C18 H18B 108.0 N4 C19 C20 121.1(3) N4 C19 C27 118.1(2) C20 C19 C27 120.9(2) C19 C20 H20 120.1 C21 C20 C19 119.9(3) C21 C20 H20 120.1 C20 C21 H21 120.3 C20 C21 C22 119.3(2) C22 C21 H21 120.3 C21 C22 H22 121.0 C21 C22 C23 118.1(3) C23 C22 H22 121.0 N4 C23 C22 123.3(2) N4 C23 C24 115.50(19) C22 C23 C24 121.1(2) N1 C24 C23 111.78(17) N1 C24 H24A 109.3 N1 C24 H24B 109.3 C23 C24 H24A 109.3 C23 C24 H24B 109.3 H24A C24 H24B 107.9 C7 C25 H25A 109.5 C7 C25 H25B 109.5 C7 C25 H25C 109.5 H25A C25 H25B 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 C13 C26 H26A 109.5 C13 C26 H26B 109.5 C13 C26 H26C 109.5 H26A C26 H26B 109.5 H26A C26 H26C 109.5 H26B C26 H26C 109.5 C19 C27 H27A 109.5 C19 C27 H27B 109.5 C19 C27 H27C 109.5 H27A C27 H27B 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br1 C3 1.896(2) Br2 C4 1.894(2) Br3 C5 1.894(2) Br4 C6 1.896(2) Zn1 O1 1.9741(14) Zn1 O2 2.0665(15) Zn1 N1 2.1361(17) Zn1 N2 2.2371(17) Zn1 N3 2.2902(18) Zn1 N4 2.3480(19) Co O1 1.9741(14) Co O2 2.0665(15) Co N1 2.1361(17) Co N2 2.2371(17) Co N3 2.2902(18) Co N4 2.3480(19) O1 C1 1.312(2) O2 C2 1.296(3) N1 C12 1.477(2) N1 C18 1.477(3) N1 C24 1.470(3) N2 C7 1.347(3) N2 C11 1.348(3) N3 C13 1.343(3) N3 C17 1.346(3) N4 C19 1.344(3) N4 C23 1.347(3) C1 C2 1.453(3) C1 C6 1.390(3) C2 C3 1.398(3) C3 C4 1.401(3) C4 C5 1.384(3) C5 C6 1.409(3) C7 C8 1.397(3) C7 C25 1.498(3) C8 H8 0.9300 C8 C9 1.379(3) C9 H9 0.9300 C9 C10 1.390(3) C10 H10 0.9300 C10 C11 1.383(3) C11 C12 1.509(3) C12 H12A 0.9700 C12 H12B 0.9700 C13 C14 1.398(3) C13 C26 1.498(3) C14 H14 0.9300 C14 C15 1.383(4) C15 H15 0.9300 C15 C16 1.380(4) C16 H16 0.9300 C16 C17 1.385(3) C17 C18 1.505(3) C18 H18A 0.9700 C18 H18B 0.9700 C19 C20 1.403(4) C19 C27 1.501(4) C20 H20 0.9300 C20 C21 1.371(5) C21 H21 0.9300 C21 C22 1.384(4) C22 H22 0.9300 C22 C23 1.386(3) C23 C24 1.510(3) C24 H24A 0.9700 C24 H24B 0.9700 C25 H25A 0.9600 C25 H25B 0.9600 C25 H25C 0.9600 C26 H26A 0.9600 C26 H26B 0.9600 C26 H26C 0.9600 C27 H27A 0.9600 C27 H27B 0.9600 C27 H27C 0.9600 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0.9961 0.0243 1.0001 0.0328 -0.0073 0.1588 -1.0022 0.9702 -2.0059 -0.1147 0.1194 -0.1823 0.0080 -1.0001 0.0071 0.1012 -0.0467 -0.0237 -0.0080 1.0001 -0.0071 -0.1012 0.0467 0.0237 0.0020 -0.0056 -0.9988 0.0193 0.0654 -0.0472 -0.0020 0.0056 0.9988 -0.0193 -0.0654 0.0472 1.0022 -0.9702 2.0059 0.1147 -0.1194 0.1823 -0.9881 -1.0244 -0.9930 0.0684 -0.0393 -0.1825 0.9881 1.0244 0.9930 -0.0684 0.0393 0.1825 -0.9961 -0.0243 -1.0001 -0.0328 0.0073 -0.1588 -1.0001 -0.0130 0.9975 -0.0713 -0.1234 -0.0643 1.0001 0.0130 -0.9975 0.0713 0.1234 0.0643