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_2312839
_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          '[Fe2 (C18 H10 O4) (C18 H18 N4)2] (B F4)2'
_chemical_formula_moiety         'C54 H46 Fe2 N8 O4 2+, 2(B F4 -)'
_chemical_formula_sum            'C54 H46 B2 F8 Fe2 N8 O4'
_chemical_formula_weight         1156.31
_chemical_name_systematic
'(\m~2~-3,6-Dioxo-2,5-diphenylcyclohexa-1,4-diene-1,4-diolato)bis[{tris[(pyridin-2-yl)methyl]amine}iron(II) bis(tetrafluoroborate)'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
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_symmetry_space_group_name_Hall  '-P 1'
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_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                83.672(7)
_cell_angle_beta                 74.388(7)
_cell_angle_gamma                71.152(7)
_cell_formula_units_Z            2
_cell_length_a                   10.5990(10)
_cell_length_b                   13.9435(15)
_cell_length_c                   18.859(2)
_cell_measurement_reflns_used    2299
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.45
_cell_measurement_theta_min      2.19
_cell_measurement_wavelength     0.71073
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_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX2 (Bruker, 2016)
;
_computing_data_reduction
;
SORTAV (Blessing, 1995)
;
_computing_molecular_graphics
;
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 1
_diffrn_measured_fraction_theta_max 1
_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      0.009264
_diffrn_orient_matrix_UB_12      -0.021198
_diffrn_orient_matrix_UB_13      -0.050582
_diffrn_orient_matrix_UB_21      -0.030376
_diffrn_orient_matrix_UB_22      0.072782
_diffrn_orient_matrix_UB_23      -0.016164
_diffrn_orient_matrix_UB_31      0.097894
_diffrn_orient_matrix_UB_32      0.000163
_diffrn_orient_matrix_UB_33      -0.014603
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1554
_diffrn_reflns_av_unetI/netI     0.2233
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_diffrn_source                   'sealed x-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flake
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
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_refine_diff_density_max         0.417
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     808
_refine_ls_number_reflns         8358
_refine_ls_number_restraints     312
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.1935
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.01
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0476P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1409
_reflns_Friedel_coverage         0
_reflns_number_gt                3574
_reflns_number_total             8358
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            qf3068sup1.cif
_cod_data_source_block           Fe2TPA2Ph2dhbqBF42
_cod_original_cell_volume        2539.6(5)
_cod_database_code               2312839
_shelx_estimated_absorpt_t_min   0.914
_shelx_estimated_absorpt_t_max   0.981
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              38373
_shelx_hkl_checksum              89622
_cod_database_fobs_code 2312839