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_2312848
_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
;
[Mn (C18 H10 O4) (C18 H18 N4)2 (C3 H7 N O)2], 0.5C4 H10 O, 0.5C3 H7 N O
;
_chemical_formula_moiety
;
C60 H60 Mn2 N10 O6 2+, 2(C24 H20 B -), 0.5(C4 H10 O), 0.5(C3 H7 N O)
;
_chemical_formula_sum            'C111.5 H108.5 B2 Mn2 N10.5 O7'
_chemical_formula_weight         1839.08
_chemical_name_systematic
;(\m~2~-3,6-Dioxo-2,5-diphenylcyclohexa-1,4-diene-1,4-diolato)bis[(dimethylformamide){tris[(pyridin-2-yl)methyl]amine}manganese(II)]
bis(tetraphenylborate)--diethyl ether--dimethylformamide (1/0.5/0.5)
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
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_audit_creation_date             2023-06-28T10:15:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 101.261(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.5401(12)
_cell_length_b                   38.071(3)
_cell_length_c                   31.818(2)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.83
_cell_measurement_theta_min      2.25
_cell_measurement_wavelength     0.71073
_cell_volume                     20838(3)
_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
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2019 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.995
_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      0.02266
_diffrn_orient_matrix_UB_12      0.024105
_diffrn_orient_matrix_UB_13      0.000023
_diffrn_orient_matrix_UB_21      -0.017235
_diffrn_orient_matrix_UB_22      0.001209
_diffrn_orient_matrix_UB_23      -0.031836
_diffrn_orient_matrix_UB_31      -0.050683
_diffrn_orient_matrix_UB_32      0.010366
_diffrn_orient_matrix_UB_33      0.003658
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0866
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            824783
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.696
_diffrn_reflns_theta_min         0.844
_diffrn_source                   'sealed x-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.301
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7736
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.984
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     2722
_refine_ls_number_reflns         58856
_refine_ls_number_restraints     2055
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1282
_refine_ls_R_factor_gt           0.0786
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+45.8699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1706
_refine_ls_wR_factor_ref         0.1949
_reflns_Friedel_coverage         0
_reflns_number_gt                38201
_reflns_number_total             58856
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            qf3068sup1.cif
_cod_data_source_block           Mn2TPA2Ph2dhbqDMF2BPh42
_cod_original_cell_volume        20838(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2312848
_shelx_estimated_absorpt_t_min   0.872
_shelx_estimated_absorpt_t_max   0.976
_shelx_shelxl_version_number     2019/3
_shelx_fab_checksum              44650
_shelx_res_checksum              43006
_shelx_hkl_checksum              42308
_cod_database_fobs_code 2312848