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_7250552
_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_formula_moiety         'C40 H56 B N8, 3(C2 F6 N O4 S2), 0.29(H2 O)'
_chemical_formula_sum            'C46 H56.58 B F18 N11 O12.29 S6'
_chemical_formula_weight         1505.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_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                 90.267(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2248(8)
_cell_length_b                   13.2729(6)
_cell_length_c                   27.7992(10)
_cell_measurement_reflns_used    9440
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.1609
_cell_measurement_theta_min      2.7909
_cell_volume                     6355.5(5)
_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 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0261
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            117866
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.175
_diffrn_reflns_theta_min         2.122
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    0.334
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6822
_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    1.573
_exptl_crystal_description       plate
_exptl_crystal_F_000             3083.5
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1278
_refine_ls_number_reflns         24204
_refine_ls_number_restraints     2338
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0601P)^2^+3.9110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1461
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19244
_reflns_number_total             24204
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra02301g2.cif
_cod_data_source_block           GM1_56_0m
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7250552
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.875
_shelx_estimated_absorpt_t_max   0.961
_shelx_res_checksum              25914
_shelx_hkl_checksum              90026