Synthesis and crystal structures of a family of bimetallic complexes with phenyl-substituted bridging tetraoxolene ligands.
Kamin, Ashlyn A.; Le, Phuong H.; Brannan, E. J.; Gannon, Paige M.; Krajewski, Sebastian; Kaminsky, Werner; Xiao, Dianne J.; Acta crystallographica. Section C, Structural chemistry 81 (2025) –; doi:10.1107/S2053229625003584

data_2312841
_publ_section_title
;
 Synthesis and crystal structures of a family of bimetallic complexes with
 phenyl-substituted bridging tetraoxolene ligands.
;
_journal_coeditor_code           QF3068
_journal_issue                   6
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi               10.1107/S2053229625003584
_journal_volume                  81
_journal_year                    2025
_chemical_formula_iupac
'[Co3 (C18 H10 O4)2 (C18 H18 N4)2 (C2 H3 N)2] (B F4)2, 2C2 H3 N'
_chemical_formula_moiety         'C76 H62 Co3 N10 O8 4+, 4(B F4 -), 2(C2 H3 N)'
_chemical_formula_sum            'C80 H68 B4 Co3 F16 N12 O8'
_chemical_formula_weight         1849.49
_chemical_name_systematic
'[{Tris[(pyridin-2-yl)methyl]amine}cobalt(III)]-\m-3,6-dioxo-2,5-diphenylcyclohexa-1,4-diene-1,4-diolato-[diacetonitrilecobalt(II)]-\m-3,6-dioxo-2,5-diphenylcyclohexa-1,4-diene-1,4-diolato-[{tris[(pyridin-2-yl)methyl]amine}cobalt(III)] bis(tetrafluoroborate) acetonitrile disolvate'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
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_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   mixed
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_cell_angle_alpha                80.478(10)
_cell_angle_beta                 80.379(9)
_cell_angle_gamma                85.651(9)
_cell_formula_units_Z            1
_cell_length_a                   10.6863(15)
_cell_length_b                   12.962(2)
_cell_length_c                   15.377(2)
_cell_measurement_reflns_used    1695
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.55
_cell_measurement_theta_min      2.52
_cell_measurement_wavelength     0.71073
_cell_volume                     2068.5(5)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX2 (Bruker, 2016)
;
_computing_data_reduction
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SORTAV (Blessing, 1995)
;
_computing_molecular_graphics
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ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
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WinGX publication routines (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXS2013 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_UB_11      -0.027649
_diffrn_orient_matrix_UB_12      0.075354
_diffrn_orient_matrix_UB_13      -0.015271
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_diffrn_orient_matrix_UB_22      -0.018771
_diffrn_orient_matrix_UB_23      -0.043997
_diffrn_orient_matrix_UB_31      -0.075814
_diffrn_orient_matrix_UB_32      -0.010193
_diffrn_orient_matrix_UB_33      0.04785
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1756
_diffrn_reflns_av_unetI/netI     0.2357
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_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.36
_diffrn_source                   'sealed x-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.693
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       piece
_exptl_crystal_F_000             941
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     547
_refine_ls_number_reflns         7308
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.3061
_refine_ls_R_factor_gt           0.1115
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1391P)^2^+4.3598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2482
_refine_ls_wR_factor_ref         0.3474
_reflns_Friedel_coverage         0
_reflns_number_gt                2394
_reflns_number_total             7308
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            qf3068sup1.cif
_cod_data_source_block           Co3TPA2Ph2dhbq2BF44
_cod_database_code               2312841
_shelx_estimated_absorpt_t_min   0.928
_shelx_estimated_absorpt_t_max   0.953
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              62062
_shelx_hkl_checksum              74725
_cod_database_fobs_code 2312841