#------------------------------------------------------------------------------ #$Date: 2024-04-16 01:47:36 +0300 (Tue, 16 Apr 2024) $ #$Revision: 291203 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/84/7248414.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_7248414 loop_ _publ_author_name 'Igoa, Fernando' 'L\'opez Cabrera, Agust\'in' 'Gonzalez-Platas, Javier' 'Suescun, Leopoldo' 'Kremer, Carlos' 'Torres, Julia' _publ_section_title ; Extended isomerism in heteronuclear metal-organic frameworks: synthetic strategies and crystal structures of lanthanide-cobalt-oxydiacetate systems ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D4CE00168K _journal_year 2024 _chemical_formula_moiety 'C24 H24 Co2 O30 Tm2, Co H6 O6, 3(O)' _chemical_formula_sum 'C24 H30 Co3 O39 Tm2' _chemical_formula_weight 1457.13 _space_group_crystal_system cubic _space_group_IT_number 228 _space_group_name_Hall '-F 4ud 2vw 3' _space_group_name_H-M_alt 'F d -3 c :2' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2023-08-29 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2023-12-28 deposited with the CCDC. 2024-04-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 16 _cell_length_a 25.4416(9) _cell_length_b 25.4416(9) _cell_length_c 25.4416(9) _cell_measurement_reflns_used 2086 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 31.1760 _cell_measurement_theta_min 3.8720 _cell_volume 16467.7(10) _computing_cell_refinement 'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2019/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 298(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.5953 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.997 _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 -39.00 58.00 1.00 30.00 -- -14.87 38.00 120.00 97 2 \w -19.00 27.00 1.00 30.00 -- -14.87 38.00 30.00 46 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0057294000 _diffrn_orient_matrix_UB_12 0.0227557000 _diffrn_orient_matrix_UB_13 0.0150578000 _diffrn_orient_matrix_UB_21 -0.0266517000 _diffrn_orient_matrix_UB_22 -0.0079796000 _diffrn_orient_matrix_UB_23 0.0018886000 _diffrn_orient_matrix_UB_31 0.0058373000 _diffrn_orient_matrix_UB_32 -0.0139871000 _diffrn_orient_matrix_UB_33 0.0233926000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_unetI/netI 0.0152 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 13427 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.233 _diffrn_reflns_theta_min 3.924 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 5.576 _exptl_absorpt_correction_T_max 0.679 _exptl_absorpt_correction_T_min 0.600 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.75a (Rigaku Oxford Diffraction, 2020) 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 'light pink' _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary pink _exptl_crystal_density_diffrn 2.351 _exptl_crystal_description block _exptl_crystal_F_000 11280 _exptl_crystal_size_max 0.133 _exptl_crystal_size_mid 0.111 _exptl_crystal_size_min 0.098 _refine_diff_density_max 0.924 _refine_diff_density_min -0.740 _refine_diff_density_rms 0.109 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 58 _refine_ls_number_reflns 856 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.152 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0327 _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^)+(0.0428P)^2^+119.0316P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0905 _refine_ls_wR_factor_ref 0.1090 _reflns_Friedel_coverage 0.000 _reflns_number_gt 522 _reflns_number_total 856 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00168k2.cif _cod_data_source_block cub_tmcooda _cod_original_cell_volume 16467.7(17) _cod_original_sg_symbol_Hall '-F 4cvw 2vw 3' _cod_original_sg_symbol_H-M 'F d -3 c' _cod_database_code 7248414 _shelx_shelxl_version_number 2019/3 _chemical_oxdiff_formula 'Tm2 Co3 C24 H30 O38' _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. ; _reflns_odcompleteness_completeness 99.44 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 28.22 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All O(H) groups 2. Others Fixed Sof: H1W(0.5) O2W(0.25) 3.a Rotating group: O1W(H1W) 3.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B) ; _shelx_res_file ; TITL Cub_TmCoODA in Fd-3c cub_tmcooda.res created by SHELXL-2019/3 at 11:57:27 on 29-Aug-2023 REM Fd-3c (#228 in standard setting) CELL 0.71073 25.441616 25.441616 25.441616 90 90 90 ZERR 16 0.00087 0.00087 0.00087 0 0 0 LATT 4 SYMM 0.25-X,0.75-Y,0.5+Z SYMM 0.75-X,0.5+Y,0.25-Z SYMM 0.5+X,0.25-Y,0.75-Z SYMM +Z,+X,+Y SYMM 0.5+Z,0.25-X,0.75-Y SYMM 0.25-Z,0.75-X,0.5+Y SYMM 0.75-Z,0.5+X,0.25-Y SYMM +Y,+Z,+X SYMM 0.75-Y,0.5+Z,0.25-X SYMM 0.5+Y,0.25-Z,0.75-X SYMM 0.25-Y,0.75-Z,0.5+X SYMM 0.75+Y,0.25+X,-Z SYMM 0.5-Y,0.5-X,0.5-Z SYMM 0.25+Y,-X,0.75+Z SYMM -Y,0.75+X,0.25+Z SYMM 0.75+X,0.25+Z,-Y SYMM -X,0.75+Z,0.25+Y SYMM 0.5-X,0.5-Z,0.5-Y SYMM 0.25+X,-Z,0.75+Y SYMM 0.75+Z,0.25+Y,-X SYMM 0.25+Z,-Y,0.75+X SYMM -Z,0.75+Y,0.25+X SYMM 0.5-Z,0.5-Y,0.5-X SFAC C H Co O Tm UNIT 384 480 48 624 32 L.S. 50 PLAN 10 TEMP 25(2) CONF BOND $H LIST 4 MORE -1 fmap 2 acta REM REM REM WGHT 0.042800 119.031601 FVAR 0.21167 CO1 3 0.250000 0.250000 0.500000 10.16667 0.01996 0.01996 = 0.01996 0.00109 0.00109 -0.00109 TM 5 0.250000 0.500000 0.500000 10.16667 0.02362 0.02362 = 0.02362 0.00340 -0.00340 -0.00340 O2 4 0.272542 0.328129 0.513394 11.00000 0.03952 0.03127 = 0.03901 -0.00029 -0.00515 0.00120 O1 4 0.280920 0.413936 0.508618 11.00000 0.03094 0.03140 = 0.05336 0.00705 -0.00417 -0.00231 C1 1 0.253309 0.372903 0.508144 11.00000 0.03459 0.03124 = 0.02491 0.00373 0.00127 -0.00265 C2 1 0.195166 0.379387 0.502568 11.00000 0.03296 0.02864 = 0.06615 0.00079 -0.00462 -0.00353 AFIX 23 H2A 2 0.183150 0.361922 0.470879 11.00000 -1.20000 H2B 2 0.177437 0.363592 0.532398 11.00000 -1.20000 AFIX 0 O3 4 0.183248 0.433248 0.500000 10.50000 0.02663 0.02663 = 0.04926 0.00324 -0.00324 0.00092 CO2 3 0.375000 0.375000 0.375000 10.08333 0.04373 0.04373 = 0.04373 0.00000 0.00000 0.00000 O1W 4 0.375000 0.375000 0.456683 10.50000 0.04167 0.08378 = 0.04366 0.00000 0.00000 0.00165 AFIX 7 H1W 2 0.342521 0.376191 0.469823 10.50000 -1.50000 AFIX 0 O2W 4 0.125000 0.417762 0.625000 10.25000 0.07547 0.09455 = 0.11494 0.00000 -0.00231 0.00000 HKLF 4 REM Cub_TmCoODA in Fd-3c REM wR2 = 0.1090, GooF = S = 1.152, Restrained GooF = 1.152 for all data REM R1 = 0.0327 for 522 Fo > 4sig(Fo) and 0.0572 for all 856 data REM 58 parameters refined using 0 restraints END WGHT 0.0428 119.2471 REM Highest difference peak 0.924, deepest hole -0.740, 1-sigma level 0.109 Q1 1 0.1250 0.3750 0.6250 10.25000 0.05 0.80 Q2 1 0.2475 0.3740 0.4998 11.00000 0.05 0.55 Q3 1 0.2500 0.4374 0.5626 10.50000 0.05 0.47 Q4 1 0.2440 0.3299 0.4833 11.00000 0.05 0.44 Q5 1 0.2463 0.4144 0.4692 11.00000 0.05 0.41 Q6 1 0.2510 0.4995 0.4524 11.00000 0.05 0.39 Q7 1 0.1950 0.4372 0.5125 11.00000 0.05 0.34 Q8 1 0.3123 0.4326 0.4979 11.00000 0.05 0.34 Q9 1 0.2569 0.4375 0.4964 11.00000 0.05 0.32 Q10 1 0.2381 0.3196 0.4898 11.00000 0.05 0.29 ; _shelx_res_checksum 48445 _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 2.277 _oxdiff_exptl_absorpt_empirical_full_min 0.526 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/4, -y+3/4, z+1/2' '-x+3/4, y+1/2, -z+1/4' 'x+1/2, -y+1/4, -z+3/4' 'z, x, y' 'z+1/2, -x+1/4, -y+3/4' '-z+1/4, -x+3/4, y+1/2' '-z+3/4, x+1/2, -y+1/4' 'y, z, x' '-y+3/4, z+1/2, -x+1/4' 'y+1/2, -z+1/4, -x+3/4' '-y+1/4, -z+3/4, x+1/2' 'y+3/4, x+1/4, -z' '-y+1/2, -x+1/2, -z+1/2' 'y+1/4, -x, z+3/4' '-y, x+3/4, z+1/4' 'x+3/4, z+1/4, -y' '-x, z+3/4, y+1/4' '-x+1/2, -z+1/2, -y+1/2' 'x+1/4, -z, y+3/4' 'z+3/4, y+1/4, -x' 'z+1/4, -y, x+3/4' '-z, y+3/4, x+1/4' '-z+1/2, -y+1/2, -x+1/2' 'x, y+1/2, z+1/2' '-x+1/4, -y+5/4, z+1' '-x+3/4, y+1, -z+3/4' 'x+1/2, -y+3/4, -z+5/4' 'z, x+1/2, y+1/2' 'z+1/2, -x+3/4, -y+5/4' '-z+1/4, -x+5/4, y+1' '-z+3/4, x+1, -y+3/4' 'y, z+1/2, x+1/2' '-y+3/4, z+1, -x+3/4' 'y+1/2, -z+3/4, -x+5/4' '-y+1/4, -z+5/4, x+1' 'y+3/4, x+3/4, -z+1/2' '-y+1/2, -x+1, -z+1' 'y+1/4, -x+1/2, z+5/4' '-y, x+5/4, z+3/4' 'x+3/4, z+3/4, -y+1/2' '-x, z+5/4, y+3/4' '-x+1/2, -z+1, -y+1' 'x+1/4, -z+1/2, y+5/4' 'z+3/4, y+3/4, -x+1/2' 'z+1/4, -y+1/2, x+5/4' '-z, y+5/4, x+3/4' '-z+1/2, -y+1, -x+1' 'x+1/2, y, z+1/2' '-x+3/4, -y+3/4, z+1' '-x+5/4, y+1/2, -z+3/4' 'x+1, -y+1/4, -z+5/4' 'z+1/2, x, y+1/2' 'z+1, -x+1/4, -y+5/4' '-z+3/4, -x+3/4, y+1' '-z+5/4, x+1/2, -y+3/4' 'y+1/2, z, x+1/2' '-y+5/4, z+1/2, -x+3/4' 'y+1, -z+1/4, -x+5/4' '-y+3/4, -z+3/4, x+1' 'y+5/4, x+1/4, -z+1/2' '-y+1, -x+1/2, -z+1' 'y+3/4, -x, z+5/4' '-y+1/2, x+3/4, z+3/4' 'x+5/4, z+1/4, -y+1/2' '-x+1/2, z+3/4, y+3/4' '-x+1, -z+1/2, -y+1' 'x+3/4, -z, y+5/4' 'z+5/4, y+1/4, -x+1/2' 'z+3/4, -y, x+5/4' '-z+1/2, y+3/4, x+3/4' '-z+1, -y+1/2, -x+1' 'x+1/2, y+1/2, z' '-x+3/4, -y+5/4, z+1/2' '-x+5/4, y+1, -z+1/4' 'x+1, -y+3/4, -z+3/4' 'z+1/2, x+1/2, y' 'z+1, -x+3/4, -y+3/4' '-z+3/4, -x+5/4, y+1/2' '-z+5/4, x+1, -y+1/4' 'y+1/2, z+1/2, x' '-y+5/4, z+1, -x+1/4' 'y+1, -z+3/4, -x+3/4' '-y+3/4, -z+5/4, x+1/2' 'y+5/4, x+3/4, -z' '-y+1, -x+1, -z+1/2' 'y+3/4, -x+1/2, z+3/4' '-y+1/2, x+5/4, z+1/4' 'x+5/4, z+3/4, -y' '-x+1/2, z+5/4, y+1/4' '-x+1, -z+1, -y+1/2' 'x+3/4, -z+1/2, y+3/4' 'z+5/4, y+3/4, -x' 'z+3/4, -y+1/2, x+3/4' '-z+1/2, y+5/4, x+1/4' '-z+1, -y+1, -x+1/2' '-x, -y, -z' 'x-1/4, y-3/4, -z-1/2' 'x-3/4, -y-1/2, z-1/4' '-x-1/2, y-1/4, z-3/4' '-z, -x, -y' '-z-1/2, x-1/4, y-3/4' 'z-1/4, x-3/4, -y-1/2' 'z-3/4, -x-1/2, y-1/4' '-y, -z, -x' 'y-3/4, -z-1/2, x-1/4' '-y-1/2, z-1/4, x-3/4' 'y-1/4, z-3/4, -x-1/2' '-y-3/4, -x-1/4, z' 'y-1/2, x-1/2, z-1/2' '-y-1/4, x, -z-3/4' 'y, -x-3/4, -z-1/4' '-x-3/4, -z-1/4, y' 'x, -z-3/4, -y-1/4' 'x-1/2, z-1/2, y-1/2' '-x-1/4, z, -y-3/4' '-z-3/4, -y-1/4, x' '-z-1/4, y, -x-3/4' 'z, -y-3/4, -x-1/4' 'z-1/2, y-1/2, x-1/2' '-x, -y+1/2, -z+1/2' 'x-1/4, y-1/4, -z' 'x-3/4, -y, z+1/4' '-x-1/2, y+1/4, z-1/4' '-z, -x+1/2, -y+1/2' '-z-1/2, x+1/4, y-1/4' 'z-1/4, x-1/4, -y' 'z-3/4, -x, y+1/4' '-y, -z+1/2, -x+1/2' 'y-3/4, -z, x+1/4' '-y-1/2, z+1/4, x-1/4' 'y-1/4, z-1/4, -x' '-y-3/4, -x+1/4, z+1/2' 'y-1/2, x, z' '-y-1/4, x+1/2, -z-1/4' 'y, -x-1/4, -z+1/4' '-x-3/4, -z+1/4, y+1/2' 'x, -z-1/4, -y+1/4' 'x-1/2, z, y' '-x-1/4, z+1/2, -y-1/4' '-z-3/4, -y+1/4, x+1/2' '-z-1/4, y+1/2, -x-1/4' 'z, -y-1/4, -x+1/4' 'z-1/2, y, x' '-x+1/2, -y, -z+1/2' 'x+1/4, y-3/4, -z' 'x-1/4, -y-1/2, z+1/4' '-x, y-1/4, z-1/4' '-z+1/2, -x, -y+1/2' '-z, x-1/4, y-1/4' 'z+1/4, x-3/4, -y' 'z-1/4, -x-1/2, y+1/4' '-y+1/2, -z, -x+1/2' 'y-1/4, -z-1/2, x+1/4' '-y, z-1/4, x-1/4' 'y+1/4, z-3/4, -x' '-y-1/4, -x-1/4, z+1/2' 'y, x-1/2, z' '-y+1/4, x, -z-1/4' 'y+1/2, -x-3/4, -z+1/4' '-x-1/4, -z-1/4, y+1/2' 'x+1/2, -z-3/4, -y+1/4' 'x, z-1/2, y' '-x+1/4, z, -y-1/4' '-z-1/4, -y-1/4, x+1/2' '-z+1/4, y, -x-1/4' 'z+1/2, -y-3/4, -x+1/4' 'z, y-1/2, x' '-x+1/2, -y+1/2, -z' 'x+1/4, y-1/4, -z-1/2' 'x-1/4, -y, z-1/4' '-x, y+1/4, z-3/4' '-z+1/2, -x+1/2, -y' '-z, x+1/4, y-3/4' 'z+1/4, x-1/4, -y-1/2' 'z-1/4, -x, y-1/4' '-y+1/2, -z+1/2, -x' 'y-1/4, -z, x-1/4' '-y, z+1/4, x-3/4' 'y+1/4, z-1/4, -x-1/2' '-y-1/4, -x+1/4, z' 'y, x, z-1/2' '-y+1/4, x+1/2, -z-3/4' 'y+1/2, -x-1/4, -z-1/4' '-x-1/4, -z+1/4, y' 'x+1/2, -z-1/4, -y-1/4' 'x, z, y-1/2' '-x+1/4, z+1/2, -y-3/4' '-z-1/4, -y+1/4, x' '-z+1/4, y+1/2, -x-3/4' 'z+1/2, -y-1/4, -x-1/4' 'z, y, x-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 0.250000 0.250000 0.500000 0.0200(4) Uani 1 6 d S T P . . Tm Tm 0.250000 0.500000 0.500000 0.0236(2) Uani 1 6 d S T P . . O2 O 0.27254(13) 0.32813(13) 0.51339(12) 0.0366(8) Uani 1 1 d . . . . . O1 O 0.28092(13) 0.41394(12) 0.50862(13) 0.0386(8) Uani 1 1 d . . . . . C1 C 0.25331(17) 0.3729(2) 0.50814(18) 0.0302(13) Uani 1 1 d . . . . . C2 C 0.19517(19) 0.37939(19) 0.5026(2) 0.0426(12) Uani 1 1 d . . . . . H2A H 0.183150 0.361922 0.470879 0.051 Uiso 1 1 calc R U . . . H2B H 0.177437 0.363592 0.532398 0.051 Uiso 1 1 calc R U . . . O3 O 0.18325(12) 0.43325(12) 0.500000 0.0342(11) Uani 1 2 d S T P . . Co2 Co 0.375000 0.375000 0.375000 0.0437(6) Uani 1 12 d S T P . . O1W O 0.375000 0.375000 0.4567(2) 0.0564(15) Uani 1 2 d S T P . . H1W H 0.342521 0.376191 0.469823 0.085 Uiso 0.5 1 d R U P . . O2W O 0.125000 0.4178(6) 0.625000 0.095(4) Uani 0.5 2 d S T 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 0.0200(4) 0.0200(4) 0.0200(4) 0.0011(3) 0.0011(3) -0.0011(3) Tm 0.0236(2) 0.0236(2) 0.0236(2) 0.00340(10) -0.00340(10) -0.00340(10) O2 0.0395(19) 0.0313(18) 0.0390(18) -0.0003(15) -0.0051(17) 0.0012(16) O1 0.0309(17) 0.0314(18) 0.053(2) 0.0071(15) -0.0042(16) -0.0023(15) C1 0.035(3) 0.031(3) 0.025(2) 0.0037(18) 0.0013(18) -0.003(2) C2 0.033(3) 0.029(3) 0.066(3) 0.001(2) -0.005(2) -0.004(2) O3 0.0266(14) 0.0266(14) 0.049(3) 0.0032(14) -0.0032(14) 0.0009(18) Co2 0.0437(6) 0.0437(6) 0.0437(6) 0.000 0.000 0.000 O1W 0.042(3) 0.084(4) 0.044(3) 0.000 0.000 0.002(3) O2W 0.075(9) 0.095(12) 0.115(12) 0.000 -0.002(9) 0.000 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.0677 1 1 5 0.0651 -1 -1 -5 0.0409 0 1 0 0.0602 0 -1 0 0.0378 0 -3 5 0.0601 0 3 -5 0.0695 -1 0 0 0.0434 1 -1 -4 0.0554 3 -4 0 0.0564 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 O2 Co1 O2 180.0 . 169_556 ? O2 Co1 O2 86.51(12) 152_565 107_656 ? O2 Co1 O2 93.49(12) 152_565 83_455 ? O2 Co1 O2 93.49(12) . 152_565 ? O2 Co1 O2 86.51(12) . 83_455 ? O2 Co1 O2 86.51(12) 169_556 152_565 ? O2 Co1 O2 86.51(12) 169_556 107_656 ? O2 Co1 O2 86.51(12) . 32_545 ? O2 Co1 O2 93.49(12) 32_545 107_656 ? O2 Co1 O2 93.49(12) 169_556 32_545 ? O2 Co1 O2 93.49(12) 169_556 83_455 ? O2 Co1 O2 180.00(6) 152_565 32_545 ? O2 Co1 O2 86.51(12) 32_545 83_455 ? O2 Co1 O2 93.49(12) . 107_656 ? O2 Co1 O2 180.00(18) 107_656 83_455 ? O1 Tm O1 129.76(16) 70_464 55_554 ? O1 Tm O1 78.70(12) 13_456 43 ? O1 Tm O1 129.76(16) 13_456 . ? O1 Tm O1 86.42(16) 70_464 34_545 ? O1 Tm O1 78.70(12) 55_554 . ? O1 Tm O1 78.70(12) 55_554 34_545 ? O1 Tm O1 144.56(16) 55_554 43 ? O1 Tm O1 78.70(12) 70_464 13_456 ? O1 Tm O1 144.56(16) 70_464 . ? O1 Tm O1 86.42(16) 55_554 13_456 ? O1 Tm O1 78.70(12) 34_545 . ? O1 Tm O1 144.56(16) 34_545 13_456 ? O1 Tm O1 86.42(16) 43 . ? O1 Tm O1 78.70(12) 70_464 43 ? O1 Tm O1 129.76(16) 34_545 43 ? O1 Tm O3 72.28(8) 70_464 34_545 ? O1 Tm O3 64.88(8) . . ? O1 Tm O3 72.28(8) 55_554 . ? O1 Tm O3 136.79(8) 55_554 34_545 ? O1 Tm O3 136.79(8) 43 55_554 ? O1 Tm O3 64.88(8) 34_545 34_545 ? O1 Tm O3 64.88(8) 13_456 . ? O1 Tm O3 136.79(8) 13_456 34_545 ? O1 Tm O3 72.28(8) 13_456 55_554 ? O1 Tm O3 64.88(8) 43 34_545 ? O1 Tm O3 136.79(8) 70_464 . ? O1 Tm O3 72.28(8) . 34_545 ? O1 Tm O3 136.79(8) 34_545 . ? O1 Tm O3 64.88(8) 70_464 55_554 ? O1 Tm O3 72.28(8) 43 . ? O1 Tm O3 64.88(8) 55_554 55_554 ? O1 Tm O3 72.28(8) 34_545 55_554 ? O1 Tm O3 136.79(8) . 55_554 ? O3 Tm O3 120.0 34_545 55_554 ? O3 Tm O3 120.0 55_554 . ? O3 Tm O3 120.0 34_545 . ? C1 O2 Co1 137.8(3) . . ? C1 O1 Tm 126.1(3) . . ? O2 C1 O1 122.5(4) . . ? O2 C1 C2 119.9(4) . . ? O1 C1 C2 117.5(4) . . ? C1 C2 H2A 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? O3 C2 C1 109.0(4) . . ? O3 C2 H2A 109.9 . . ? O3 C2 H2B 109.9 . . ? C2 O3 Tm 122.5(2) 13_456 . ? C2 O3 Tm 122.5(2) . . ? C2 O3 C2 115.0(5) . 13_456 ? O1W Co2 O1W 90.000(1) 27_545 55_554 ? O1W Co2 O1W 90.0 27_545 9 ? O1W Co2 O1W 180.0 . 27_545 ? O1W Co2 O1W 90.0 . 9 ? O1W Co2 O1W 90.0 83_455 27_545 ? O1W Co2 O1W 90.0 55_554 9 ? O1W Co2 O1W 90.000(1) . 5 ? O1W Co2 O1W 180.0 5 55_554 ? O1W Co2 O1W 90.0 83_455 5 ? O1W Co2 O1W 180.0 83_455 9 ? O1W Co2 O1W 90.0 27_545 5 ? O1W Co2 O1W 90.0 5 9 ? O1W Co2 O1W 90.0 . 55_554 ? O1W Co2 O1W 90.000(1) 83_455 55_554 ? O1W Co2 O1W 90.0 . 83_455 ? Co2 O1W H1W 112.0 . . ? Co2 O1W H1W 112.01(3) . 50_554 ? H1W O1W H1W 136.0 . 50_554 ? 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 O2 2.097(3) . ? Co1 O2 2.097(3) 107_656 ? Co1 O2 2.097(3) 32_545 ? Co1 O2 2.097(3) 169_556 ? Co1 O2 2.097(3) 152_565 ? Co1 O2 2.097(3) 83_455 ? Tm O1 2.337(3) 55_554 ? Tm O1 2.337(3) . ? Tm O1 2.337(3) 43 ? Tm O1 2.337(3) 34_545 ? Tm O1 2.337(3) 13_456 ? Tm O1 2.337(3) 70_464 ? Tm O3 2.402(4) 34_545 ? Tm O3 2.402(4) 55_554 ? Tm O3 2.402(4) . ? O2 C1 1.247(6) . ? O1 C1 1.258(6) . ? C1 C2 1.495(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 O3 1.405(5) . ? Co2 O1W 2.078(5) 9 ? Co2 O1W 2.078(5) 5 ? Co2 O1W 2.078(5) 55_554 ? Co2 O1W 2.078(5) 83_455 ? Co2 O1W 2.078(5) 27_545 ? Co2 O1W 2.078(5) . ? O1W H1W 0.8919 . ? O1W H1W 0.8918 50_554 ? 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 Co1 O2 C1 O1 -163.3(3) . . . . ? Co1 O2 C1 C2 18.5(7) . . . . ? Tm O1 C1 O2 -179.4(3) . . . . ? Tm O1 C1 C2 -1.2(6) . . . . ? O2 C1 C2 O3 177.0(4) . . . . ? O1 C1 C2 O3 -1.3(6) . . . . ? C1 C2 O3 Tm 3.1(5) . . . . ? C1 C2 O3 C2 -176.9(5) . . . 13_456 ? 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 1.0000 -0.0001 -0.0002 -0.0057 -0.0267 0.0058 1.0004 1.0008 4.9997 0.0923 -0.0252 0.1088 -1.0004 -1.0008 -4.9997 -0.0923 0.0252 -0.1088 0.0004 1.0001 0.0002 0.0228 -0.0080 -0.0140 -0.0004 -1.0001 -0.0002 -0.0228 0.0080 0.0140 -0.0012 -2.9996 4.9992 0.0070 0.0334 0.1589 0.0012 2.9996 -4.9992 -0.0070 -0.0334 -0.1589 -1.0000 0.0001 0.0002 0.0057 0.0267 -0.0058 1.0000 -0.9999 -3.9999 -0.0887 -0.0262 -0.0737 3.0000 -3.9998 0.0001 -0.1082 -0.0480 0.0735