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_2312842
_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
'[Zn2 (C18 H10 O4) (C18 H18 N4)2] (B F4)2, 0.892C2 H3 N, 0.108C4 H10 O'
_chemical_formula_moiety
'C54 H46 N8 O4 Zn2 2+, 2(B F4 -), 0.892(C2 H3 N), 0.108(C4 H10 O)'
_chemical_formula_sum            'C56.22 H49.75 B2 F8 N8.89 O4.11 Zn2'
_chemical_formula_weight         1220.02
_chemical_name_systematic
;(\m~2~-3,6-Dioxo-2,5-diphenylcyclohexa-1,4-diene-1,4-diolato)bis[{tris[(pyridin-2-yl)methyl]amine}zinc(II)]
bis(tetrafluoroborate)--acetonitrile--diethyl ether (1/0.9/0.1)
;
_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
_atom_sites_solution_primary     direct
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_audit_creation_date             2022-07-28T14:56:43-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                101.725(3)
_cell_angle_beta                 105.794(3)
_cell_angle_gamma                101.012(3)
_cell_formula_units_Z            1
_cell_length_a                   10.9172(7)
_cell_length_b                   11.0896(7)
_cell_length_c                   12.1795(8)
_cell_measurement_reflns_used    9695
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.42
_cell_measurement_theta_min      2.27
_cell_measurement_wavelength     0.71073
_cell_volume                     1340.94(15)
_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 1
_diffrn_measured_fraction_theta_max 0.994
_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      -0.060362
_diffrn_orient_matrix_UB_12      -0.032097
_diffrn_orient_matrix_UB_13      -0.083839
_diffrn_orient_matrix_UB_21      0.062478
_diffrn_orient_matrix_UB_22      0.059004
_diffrn_orient_matrix_UB_23      -0.024362
_diffrn_orient_matrix_UB_31      0.046684
_diffrn_orient_matrix_UB_32      -0.067767
_diffrn_orient_matrix_UB_33      -0.015218
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 1
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_diffrn_reflns_limit_h_min       -14
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_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
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_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         28.448
_diffrn_reflns_theta_min         1.805
_diffrn_source                   'sealed x-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.979
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.77
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     472
_refine_ls_number_reflns         6735
_refine_ls_number_restraints     172
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0318P)^2^+0.6647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.07
_reflns_Friedel_coverage         0
_reflns_number_gt                6444
_reflns_number_total             6735
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            qf3068sup1.cif
_cod_data_source_block           Zn2TPA2Ph2dhbqBF42
_cod_database_code               2312842
_shelx_estimated_absorpt_t_min   0.519
_shelx_estimated_absorpt_t_max   0.908
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              59324
_shelx_hkl_checksum              57467
_cod_database_fobs_code 2312842