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_7064026
_publ_section_title
;
 Dicobalt tetracarboxylate complexes with labile axial ligands
;
_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         'C96 H94 Co2 O13, C4 H8 O'
_chemical_formula_sum            'C100 H102 Co2 O14'
_chemical_formula_weight         1645.67
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-23
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2025-01-07 deposited with the CCDC.	2025-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.748(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.372(5)
_cell_length_b                   25.215(9)
_cell_length_c                   23.014(9)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    100.02
_cell_measurement_theta_max      72.142
_cell_measurement_theta_min      3.504
_cell_volume                     8330(5)
_computing_cell_refinement       'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 Ver. 2013.2-0 (Bruker-AXS, 2013)'
_computing_data_reduction        'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.02
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.60\% \w and 0.6\% \f scans'
_diffrn_radiation_collimation    '0.5 mm double-pinhole'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'equatorially mounted graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            118030
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.168
_diffrn_reflns_theta_min         2.601
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           32.0
_diffrn_source_power             1.28
_diffrn_source_type              'Siemens, K FFCU 2K 90'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    3.655
_exptl_absorpt_correction_T_max  0.6064
_exptl_absorpt_correction_T_min  0.5298
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0744 before and 0.0614 after correction.
The Ratio of minimum to maximum transmission is 0.8737.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3472
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.906
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1071
_refine_ls_number_reflns         16286
_refine_ls_number_restraints     316
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0522P)^2^+7.4456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1226
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13193
_reflns_number_total             16286
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj02169c2.cif
_cod_data_source_block           berry899
_cod_depositor_comments
'Adding full bibliography for 7064026--7064029.cif.'
_cod_database_code               7064026
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.711
_shelx_estimated_absorpt_t_min   0.711
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H1A-O1 \\sim H1B-O1
 with sigma of 0.01
 C82-C83 \\sim C82A-C83
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C98) = Uanis(C97)
Uanis(O14A) = Uanis(C10A) = Uanis(C97A) = Uanis(C98A) = Uanis(C99A)
Uiso(O12) = Uiso(C89) = Uiso(C90) = Uiso(C91) = Uiso(C92) = Uiso(O12A) =
Uiso(C89A) = Uiso(C90A) = Uiso(C91A) = Uiso(C92A) = Uiso(O12B) = Uiso(C89B) =
Uiso(C90B) = Uiso(C91B) = Uiso(C92B)
Uiso(O13A) = Uiso(C93B) = Uiso(C93A) = Uiso(C94A) = Uiso(C95A) = Uiso(C96A)
Uanis(O13) = Uanis(C93) = Uanis(C94) = Uanis(C95) = Uanis(C96)
Uiso(C82A) = Uiso(C84A)
Uanis(C84) = Uanis(C82)
4. Same fragment restrains
{O12, C89, C90, C91, C92} sigma for 1-2: 0.01, 1-3: 0.02
{O12A, C89A, C90A, C91A, C92A} sigma for 1-2: 0.01, 1-3: 0.02
{O12B, C89B, C90B, C91B, C92B} sigma for 1-2: 0.01, 1-3: 0.02
{O13A, C93B, C94A, C95A, C96A} sigma for 1-2: 0.01, 1-3: 0.02
{O13A, C93A, C94A, C95A, C96A} sigma for 1-2: 0.01, 1-3: 0.02
{O13, C93, C94, C95, C96} sigma for 1-2: 0.01, 1-3: 0.02
{O14A, C97A, C98A, C99A, C10A} sigma for 1-2: 0.01, 1-3: 0.02
{O14, C100, C99, C98, C97} sigma for 1-2: 0.01, 1-3: 0.02
as in
{O11, C85, C86, C87, C88}
5. Others
 1*[Sof(O12)+Sof(C89)+Sof(H89A)+Sof(H89B)+Sof(C90)+Sof(H90A)+Sof(H90B)+
 Sof(C91)+Sof(H91A)+Sof(H91B)+Sof(C92)+Sof(H92A)+Sof(H92B)]+1*[Sof(O12A)+
 Sof(C89A)+Sof(H89C)+Sof(H89D)+Sof(C90A)+Sof(H90C)+Sof(H90D)+Sof(C91A)+
 Sof(H91C)+Sof(H91D)+Sof(C92A)+Sof(H92C)+Sof(H92D)]+1*[Sof(O12B)+Sof(C89B)+
 Sof(H89E)+Sof(H89F)+Sof(C90B)+Sof(H90E)+Sof(H90F)+Sof(C91B)+Sof(H91E)+
 Sof(H91F)+Sof(C92B)+Sof(H92E)+Sof(H92F)]=1 with esd of 0
 -1*[Sof(O13)+Sof(C93)+Sof(H93A)+Sof(H93B)+Sof(C94)+Sof(H94A)+Sof(H94B)+
 Sof(C95)+Sof(H95A)+Sof(H95B)+Sof(C96)+Sof(H96A)+Sof(H96B)+Sof(O13A)+Sof(C94A)+
 Sof(C95A)+Sof(H95C)+Sof(H95D)+Sof(C96A)+Sof(H96C)+Sof(H96D)]+1*[Sof(C93A)+
 Sof(H93C)+Sof(H93D)+Sof(H94C)+Sof(H94D)]+1*[Sof(H94E)+Sof(H94F)+Sof(C93B)+
 Sof(H93E)+Sof(H93F)]=0 with esd of 0
 Sof(H81C)=Sof(H81D)=Sof(H83C)=Sof(H83D)=Sof(C82A)=Sof(H82C)=Sof(H82D)=
 Sof(C84A)=Sof(H84C)=Sof(H84D)=1-FVAR(1)
 Sof(H81A)=Sof(H81B)=Sof(H83A)=Sof(H83B)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(C84)=
 Sof(H84A)=Sof(H84B)=FVAR(1)
 Sof(O12)=Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(C91)=
 Sof(H91A)=Sof(H91B)=Sof(C92)=Sof(H92A)=Sof(H92B)=FVAR(2)
 Sof(O12A)=Sof(C89A)=Sof(H89C)=Sof(H89D)=Sof(C90A)=Sof(H90C)=Sof(H90D)=
 Sof(C91A)=Sof(H91C)=Sof(H91D)=Sof(C92A)=Sof(H92C)=Sof(H92D)=FVAR(3)
 Sof(O12B)=Sof(C89B)=Sof(H89E)=Sof(H89F)=Sof(C90B)=Sof(H90E)=Sof(H90F)=
 Sof(C91B)=Sof(H91E)=Sof(H91F)=Sof(C92B)=Sof(H92E)=Sof(H92F)=FVAR(4)
 Sof(O13)=Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(C94)=Sof(H94A)=Sof(H94B)=Sof(C95)=
 Sof(H95A)=Sof(H95B)=Sof(C96)=Sof(H96A)=Sof(H96B)=1-FVAR(5)
 Sof(O13A)=Sof(C94A)=Sof(C95A)=Sof(H95C)=Sof(H95D)=Sof(C96A)=Sof(H96C)=
 Sof(H96D)=FVAR(5)
 Sof(C93A)=Sof(H93C)=Sof(H93D)=Sof(H94C)=Sof(H94D)=FVAR(6)
 Sof(H94E)=Sof(H94F)=Sof(C93B)=Sof(H93E)=Sof(H93F)=FVAR(7)
 Sof(O14A)=Sof(C97A)=Sof(H97C)=Sof(H97D)=Sof(C98A)=Sof(H98C)=Sof(H98D)=
 Sof(C99A)=Sof(H99C)=Sof(H99D)=Sof(C10A)=Sof(H10C)=Sof(H10D)=1-FVAR(8)
 Sof(O14)=Sof(C100)=Sof(H10A)=Sof(H10B)=Sof(C99)=Sof(H99A)=Sof(H99B)=Sof(C98)=
 Sof(H98A)=Sof(H98B)=Sof(C97)=Sof(H97A)=Sof(H97B)=FVAR(8)
6.a Secondary CH2 refined with riding coordinates:
 C81(H81A,H81B), C81(H81C,H81D), C83(H83A,H83B), C83(H83C,H83D), C82(H82A,
 H82B), C84(H84A,H84B), C82A(H82C,H82D), C84A(H84C,H84D), C85(H85A,H85B),
 C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B),
  C91(H91A,H91B), C92(H92A,H92B), C89A(H89C,H89D), C90A(H90C,H90D), C91A(H91C,
 H91D), C92A(H92C,H92D), C89B(H89E,H89F), C90B(H90E,H90F), C91B(H91E,H91F),
 C92B(H92E,H92F), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B), C96(H96A,
 H96B), C93A(H93C,H93D), C94A(H94E,H94F), C94A(H94C,H94D), C95A(H95C,H95D),
 C96A(H96C,H96D), C93B(H93E,H93F), C100(H10A,H10B), C99(H99A,H99B), C98(H98A,
 H98B), C97(H97A,H97B), C97A(H97C,H97D), C98A(H98C,H98D), C99A(H99C,H99D),
 C10A(H10C,H10D)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), 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), 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), C44(H44),
  C45(H45), C46(H46), C47(H47), C48(H48), C50(H50), C51(H51), C52(H52),
 C53(H53), C54(H54), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C64(H64),
  C65(H65), C66(H66), C67(H67), C68(H68), C70(H70), C71(H71), C72(H72),
 C73(H73), C74(H74), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80)
;
_shelx_res_checksum              23558
_olex2_submission_special_instructions 'No special instructions were received'