Single electron reduction of NHC-CO<sub>2</sub>-borane compounds.
Morales, Agustín; Gonçalves, Caroline; Sournia-Saquet, Alix; Vendier, Laure; Lledós, Agustí; Baslé, Olivier; Bontemps, Sébastien; Chemical science 15 (2024) 3165–3173; doi:10.1039/d3sc06325a

data_1570814
_publ_section_title
;
 Single electron reduction of NHC-CO<sub>2</sub>-borane compounds.
;
_journal_issue                   9
_journal_name_full               'Chemical science'
_journal_page_first              3165
_journal_page_last               3173
_journal_paper_doi               10.1039/d3sc06325a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C42 H32 B F15 N2 O2'
_chemical_formula_sum            'C42 H32 B F15 N2 O2'
_chemical_formula_weight         892.50
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-11-09 deposited with the CCDC.	2024-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.130(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4874(2)
_cell_length_b                   20.6397(4)
_cell_length_c                   15.6705(3)
_cell_measurement_reflns_used    14591
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.4170
_cell_measurement_theta_min      4.2880
_cell_volume                     3712.85(12)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18464
_diffrn_reflns_point_group_measured_fraction_full 0.811
_diffrn_reflns_point_group_measured_fraction_max 0.763
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.522
_diffrn_reflns_theta_min         4.284
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.321
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       plate
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.179
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.04(8)
_refine_ls_extinction_coef       0.00033(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         6206
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+1.8608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0687
_reflns_Friedel_coverage         0.556
_reflns_Friedel_fraction_full    0.622
_reflns_Friedel_fraction_max     0.546
_reflns_number_gt                6074
_reflns_number_total             6206
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06325a3.cif
_cod_data_source_block           AMA173
_cod_depositor_comments
'Adding full bibliography for 1570813--1570816.cif.'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               1570814
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              12034
_shelx_hkl_checksum              24300