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_2312847
_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          'C18 H12 O4, 3C4 H8 O2'
_chemical_formula_moiety         'C18 H12 O4, 3(C4 H8 O2)'
_chemical_formula_sum            'C30 H36 O10'
_chemical_formula_weight         556.59
_chemical_name_systematic
;
2,5-Dihydroxy-3,6-diphenylcyclohexa-2,5-diene-1,4-dione dioxane trisolvate
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.5
_audit_creation_date             2021-11-01T12:22:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                81.071(6)
_cell_angle_beta                 84.938(6)
_cell_angle_gamma                78.087(6)
_cell_formula_units_Z            1
_cell_length_a                   5.4224(5)
_cell_length_b                   8.9702(9)
_cell_length_c                   14.1901(14)
_cell_measurement_reflns_used    1941
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.78
_cell_measurement_theta_min      2.34
_cell_measurement_wavelength     0.71073
_cell_volume                     666.03(11)
_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 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 0.992
_diffrn_measured_fraction_theta_max 0.974
_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      2
_diffrn_orient_matrix_UB_12      0.008419
_diffrn_orient_matrix_UB_13      0.050627
_diffrn_orient_matrix_UB_21      2
_diffrn_orient_matrix_UB_22      -0.022692
_diffrn_orient_matrix_UB_23      -0.096603
_diffrn_orient_matrix_UB_31      2
_diffrn_orient_matrix_UB_32      0.187243
_diffrn_orient_matrix_UB_33      -0.03671
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0858
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6214
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         28.56
_diffrn_reflns_theta_min         1.455
_diffrn_source                   'sealed x-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(TWINABS; Bruker, 2016)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3305
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1074
_refine_ls_R_factor_gt           0.0584
_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^)+(0.0768P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1611
_reflns_Friedel_coverage         0
_reflns_number_gt                1998
_reflns_number_total             3305
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            qf3068sup1.cif
_cod_data_source_block           H2Ph2dhbq-3dioxane
_cod_database_code               2312847
_shelx_estimated_absorpt_t_min   0.931
_shelx_estimated_absorpt_t_max   0.996
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              89361
_shelx_hkl_checksum              99952
_cod_database_fobs_code 2312847