Salts of boronium (+3) ions with unprecedented hydrolytic stability. Design, synthesis, single-crystal X-ray structures, electrochemistry, and thermophysical properties
Crowley, Margaret E.; Stachurski, Christopher D.; Davis, James H.; Zeller, Matthias; Merchant, Gabriel A.; Salter, E. A.; Wierzbicki, A.; O'Brien, Richard A.; Trulove, Paul C.; Durkin, David P.; RSC Advances 15 (2025) 19947–19953; doi:10.1039/D5RA02301G

data_7250555
_publ_section_title
;
 Salts of boronium (+3) ions with unprecedented hydrolytic stability.
 Design, synthesis, single-crystal X-ray structures, electrochemistry, and
 thermophysical properties
;
_journal_issue                   25
_journal_name_full               'RSC Advances'
_journal_page_first              19947
_journal_page_last               19953
_journal_paper_doi               10.1039/D5RA02301G
_journal_volume                  15
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C44 H56 B N8, 3(C2 F6 N O4 S2)'
_chemical_formula_sum            'C50 H56 B F18 N11 O12 S6'
_chemical_formula_weight         1548.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-10-30 deposited with the CCDC.	2025-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.9250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3318(5)
_cell_length_b                   29.6715(11)
_cell_length_c                   17.2747(7)
_cell_measurement_reflns_used    9781
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.1303
_cell_measurement_theta_min      2.5638
_cell_volume                     6382.8(4)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2020)'
_computing_data_collection       'Apex4 v2022.10-0 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2020)'
_computing_structure_refinement
;  
SHELXL-2019/2 (Sheldrick, 2015a, 2019), 
SHELXLE Rev1541 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXT (Sheldrick, 2015b)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type
'PhotonII charge-integrating pixel array (CPAD)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS D8 Quest'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            156871
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.186
_diffrn_reflns_theta_min         2.493
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    0.335
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_description       block
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.510
_exptl_crystal_size_mid          0.480
_exptl_crystal_size_min          0.370
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 9452 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1273
_refine_ls_number_reflns         23201
_refine_ls_number_restraints     1963
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+2.0056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0896
_reflns_Friedel_coverage         0.902
_reflns_Friedel_fraction_full    0.947
_reflns_Friedel_fraction_max     0.903
_reflns_number_gt                21354
_reflns_number_total             23201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra02301g2.cif
_cod_data_source_block           JD_09_28_23_0m
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7250555
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.848
_shelx_estimated_absorpt_t_max   0.886
_shelx_res_checksum              39599
_shelx_hkl_checksum              57882