Strong Magnetic Exchange Coupling in a Radical-Bridged Trinuclear Nickel Complex
Yang, Luming; Oppenheim, Julius; Dinca, Mircea; Dalton Transactions  (2022) –; doi:10.1039/D2DT01337A

data_7710285
_publ_section_title
;
 Strong Magnetic Exchange Coupling in a Radical-Bridged Trinuclear Nickel
 Complex
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01337A
_journal_year                    2022
_chemical_formula_moiety         'C167 H145 B3 Cl4 N24 Ni3'
_chemical_formula_sum            'C167 H145 B3 Cl4 N24 Ni3'
_chemical_formula_weight         2838.42
_chemical_name_common
'Trinickel 2,3,6,7,10,11-hexaiminotriphenylene cluster'
_chemical_name_systematic
'Trinickel 2,3,6,7,10,11-hexaiminotriphenylene cluster'
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-09-10 deposited with the CCDC.	2022-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                103.088(2)
_cell_angle_beta                 99.793(2)
_cell_angle_gamma                91.711(2)
_cell_formula_units_Z            2
_cell_length_a                   13.9935(6)
_cell_length_b                   18.2318(8)
_cell_length_c                   30.6238(13)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.06
_cell_measurement_theta_min      2.28
_cell_volume                     7480.1(6)
_computing_cell_refinement       'SAINT 8.38A (Bruker-AXS, 2017)'
_computing_data_collection       'APEX3 v2017.3.0 (Bruker-AXS, 2017)'
_computing_data_reduction        'SAINT 8.38A (Bruker-AXS, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.4
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Photon3 CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            397208
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.068
_diffrn_reflns_theta_min         1.388
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Herbst-Irmer et al., 2015)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2964
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane-hexane'
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.494
_refine_diff_density_min         -1.244
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1851
_refine_ls_number_reflns         47922
_refine_ls_number_restraints     2976
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0571P)^2^+6.7072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1373
_reflns_Friedel_coverage         0.000
_reflns_number_gt                36576
_reflns_number_total             47922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01337a2.cif
_cod_data_source_block           Ni3HITP
_cod_database_code               7710285
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.897
_shelx_estimated_absorpt_t_max   0.995
_shelx_res_checksum              5688
_shelx_fab_checksum              17533