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_7064029
_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         'C88 H76 Co2 O10'
_chemical_formula_sum            'C88 H76 Co2 O10'
_chemical_formula_weight         1411.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-12-13
_audit_creation_method
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Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
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_audit_update_record
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2025-01-07 deposited with the CCDC.	2025-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.332(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.931(3)
_cell_length_b                   16.880(2)
_cell_length_c                   20.205(3)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.3286
_cell_measurement_theta_min      4.0065
_cell_volume                     7138.6(17)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            145922
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.536
_diffrn_reflns_theta_min         3.364
_exptl_absorpt_coefficient_mu    4.135
_exptl_absorpt_correction_T_max  0.3875
_exptl_absorpt_correction_T_min  0.2808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0819 before and 0.0637 after correction.
The Ratio of minimum to maximum transmission is 0.7246.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       block
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         7298
_refine_ls_number_restraints     613
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+6.3310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1231
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6177
_reflns_number_total             7298
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj02169c2.cif
_cod_data_source_block           inverted
_cod_depositor_comments
'Adding full bibliography for 7064026--7064029.cif.'
_cod_original_cell_volume        7138.9(17)
_cod_database_code               7064029
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.615
_shelx_estimated_absorpt_t_min   0.463
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C35-C22 \\sim C35A-C22
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
O5 \\sim C41 \\sim C42 \\sim C43 \\sim C44: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 2A
O6 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim O6A \\sim C52 \\sim C51 \\sim
C50 \\sim C49: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C35A \\sim C36A
\\sim C37A \\sim C38A \\sim C39A \\sim C40A \\sim C22: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.03 within 2A
Co1 \\sim O4 \\sim O4A \\sim C2: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) = Uanis(O2A)
Uanis(O1A) = Uanis(O1)
Uanis(C48) = Uanis(C52)
4. Rigid body (RIGU) restrains
 O6, C45, C46, C47, C48, O6A, C52, C51, C50, C49
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O5, C41, C42, C43, C44
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 C35, C36, C37, C38, C39, C40, C35A, C36A, C37A, C38A, C39A, C40A, C22
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 O4, O4A, C2, Co1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O1A)=Sof(O2A)=1-FVAR(1)
 Sof(O1)=Sof(O2)=FVAR(1)
 Sof(O3A)=Sof(O4A)=1-FVAR(2)
 Sof(O3)=Sof(O4)=FVAR(2)
 Sof(C35A)=Sof(C36A)=Sof(H36A)=Sof(C37A)=Sof(H37A)=Sof(C38A)=Sof(H38A)=
 Sof(C39A)=Sof(H39A)=Sof(C40A)=Sof(H40A)=1-FVAR(3)
 Sof(C35)=Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38)=Sof(C39)=
 Sof(H39)=Sof(C40)=Sof(H40)=FVAR(3)
 Sof(O6A)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(C51)=
 Sof(H51A)=Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=0.5*(1-FVAR(5))
 Sof(O6)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C47)=
 Sof(H47A)=Sof(H47B)=Sof(C48)=Sof(H48A)=Sof(H48B)=0.5*FVAR(5)
 Fixed Sof: O5(0.5) C41(0.5) H41A(0.5) H41B(0.5) C42(0.5) H42A(0.5) H42B(0.5)
 C43(0.5) H43A(0.5) H43B(0.5) C44(0.5) H44A(0.5) H44B(0.5)
6.a Free rotating group:
 O5(C41,C42,C43,C44), O6(C45,C46,C47,C48), O6A(C49,C50,C51,C52)
6.b Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,
 H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B),
 C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32),
 C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40),
 C36A(H36A), C37A(H37A), C38A(H38A), C39A(H39A), C40A(H40A)
6.d Fitted hexagon refined as free rotating group:
 C35(C36,C37,C38,C39,C40), C35A(C36A,C37A,C38A,C39A,C40A)
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_shelx_res_checksum              13434
_olex2_submission_special_instructions 'No special instructions were received'