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_7130090
_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            'C39 H18 Al Cl2 F36 N O8'
_chemical_formula_weight         1410.42
_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   geom
_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                95.559(4)
_cell_angle_beta                 101.930(4)
_cell_angle_gamma                111.307(4)
_cell_formula_units_Z            2
_cell_length_a                   10.9911(15)
_cell_length_b                   14.4696(18)
_cell_length_c                   17.114(2)
_cell_measurement_reflns_used    9442
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.66
_cell_volume                     2436.4(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      120(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21988
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.527
_diffrn_reflns_theta_min         2.060
_exptl_absorpt_coefficient_mu    0.343
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0979 before and 0.0541 after correction.
The Ratio of minimum to maximum transmission is 0.9266.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.923
_exptl_crystal_description       block
_exptl_crystal_F_000             1388
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane'
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         11097
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.316
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0600
_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^)+(0.0567P)^2^+3.2432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1539
_refine_ls_wR_factor_ref         0.1654
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8623
_reflns_number_total             11097
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01539k2.cif
_cod_data_source_block           1_a
_cod_original_cell_volume        2436.3(6)
_cod_database_code               7130090
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.941
_shelx_estimated_absorpt_t_max   0.950
_shelx_res_checksum              53980
_shelx_hkl_checksum              4297