The catenation of a singlet diradical dication and modulation of diradical character by metal coordination
Li, Ke; Feng, Zhongtao; Ruan, Huapeng; Sun, Quanchun; Zhao, Yue; Wang, Xinping; Chemical Communications  (2022) –; doi:10.1039/D2CC01539K

data_7130091
_publ_section_title
;
 The catenation of a singlet diradical dication and modulation of
 diradical character by metal coordination
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC01539K
_journal_year                    2022
_chemical_formula_sum            'C46 H38 Ag Cl4 F18 N2 O9 Sb3'
_chemical_formula_weight         1719.70
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-04-19 deposited with the CCDC.	2022-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.257(3)
_cell_angle_beta                 110.805(3)
_cell_angle_gamma                99.213(3)
_cell_formula_units_Z            2
_cell_length_a                   12.0834(14)
_cell_length_b                   14.7801(15)
_cell_length_c                   16.8572(18)
_cell_measurement_reflns_used    7066
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      26.87
_cell_measurement_theta_min      2.49
_cell_volume                     2771.8(5)
_computing_cell_refinement       'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_data_collection       'Bruker BIS V6.2.1'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker D8 VENTURE TXS PHOTON 100'
_diffrn_measurement_method       '\w and \f shutterless scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23416
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_min         1.969
_exptl_absorpt_coefficient_mu    2.103
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0990 before and 0.0547 after correction.
Estimated minimum and maximum transmission were 0.0242 and 0.0468.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    2.060
_exptl_crystal_description       block
_exptl_crystal_F_000             1660
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane'
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         3.375
_refine_diff_density_min         -1.591
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     774
_refine_ls_number_reflns         12621
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1197
_refine_ls_R_factor_gt           0.0779
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0910P)^2^+16.9526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2002
_refine_ls_wR_factor_ref         0.2236
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7912
_reflns_number_total             12621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01539k2.cif
_cod_data_source_block           1_a_CCDC1
_cod_database_code               7130091
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.786
_shelx_estimated_absorpt_t_max   0.817
_shelx_res_checksum              31496
_shelx_hkl_checksum              27597