Dicobalt tetracarboxylate complexes with labile axial ligands
Pankratz, Trey C.; Harris, Caleb F.; Hyland, Ethan E.; Sailer, Joshua K.; Wheaton, Amelia M.; Davies, Huw M. L.; Berry, John F.; New Journal of Chemistry 49 (2025) 18292–18302; doi:10.1039/D5NJ02169C

data_7064027
_publ_section_title
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 Dicobalt tetracarboxylate complexes with labile axial ligands
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_journal_issue                   42
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18292
_journal_page_last               18302
_journal_paper_doi               10.1039/D5NJ02169C
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C44 H46 Co O8, 2(C20 H16 O2), 2(C H4 O)'
_chemical_formula_sum            'C86 H86 Co O14'
_chemical_formula_weight         1402.47
_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     dual
_audit_creation_date             2018-11-13
_audit_creation_method
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Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-01-07 deposited with the CCDC.	2025-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                109.773(11)
_cell_angle_beta                 98.611(10)
_cell_angle_gamma                104.368(13)
_cell_formula_units_Z            1
_cell_length_a                   12.130(3)
_cell_length_b                   12.137(3)
_cell_length_c                   13.833(4)
_cell_measurement_reflns_used    9752
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.239
_cell_measurement_theta_min      2.512
_cell_volume                     1794.5(8)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015b)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5\ \w and 0.5\ \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            56944
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.252
_diffrn_reflns_theta_min         1.618
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.307
_exptl_absorpt_correction_T_max  0.8750
_exptl_absorpt_correction_T_min  0.8459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0638 before and 0.0400 after correction. The Ratio of minimum to maximum transmission is 0.9667. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             741
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         12574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0419P)^2^+0.8230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0889
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11602
_reflns_number_total             12574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj02169c2.cif
_cod_data_source_block           berry896
_cod_depositor_comments
'Adding full bibliography for 7064026--7064029.cif.'
_cod_original_cell_volume        1794.6(8)
_cod_database_code               7064027
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.938
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4A), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34),
 C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C43(H43A,H43B,H43C)
2.c Idealised tetrahedral OH refined as rotating group:
 O7(H7A)
;
_shelx_res_checksum              90270
_olex2_submission_special_instructions 'No special instructions were received'