Catalyst-free diboration and silaboration of alkenes and alkynes using bis(9-heterofluorenyl)s.
Gilmer, Jannik; Trageser, Timo; Čaić, Luis; Virovets, Alexander; Bolte, Michael; Lerner, Hans-Wolfram; Fantuzzi, Felipe; Wagner, Matthias; Chemical science 14 (2023) 4589–4596; doi:10.1039/d3sc01395b

data_1568733
_publ_section_title
;
 Catalyst-free diboration and silaboration of alkenes and alkynes using
 bis(9-heterofluorenyl)s.
;
_journal_issue                   17
_journal_name_full               'Chemical science'
_journal_page_first              4589
_journal_page_last               4596
_journal_paper_doi               10.1039/d3sc01395b
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C46 H60 B Cl O Si, 1.5(C4 H10 O)'
_chemical_formula_sum            'C52 H75 B Cl O2.5 Si'
_chemical_formula_weight         814.47
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-03-08 deposited with the CCDC.	2023-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.094(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8477(7)
_cell_length_b                   14.9915(7)
_cell_length_c                   22.6511(12)
_cell_measurement_reflns_used    39295
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.18
_cell_measurement_theta_min      1.95
_cell_volume                     4963.9(4)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            30219
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.724
_diffrn_reflns_theta_min         2.094
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_description       block
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.260
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         9272
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0710
_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^)+(0.0694P)^2^+5.0918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1709
_refine_ls_wR_factor_ref         0.1906
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7369
_reflns_number_total             9272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01395b3.cif
_cod_data_source_block           wa3030
_cod_depositor_comments
'Adding full bibliography for 1568727--1568737.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C52 H75 B Cl O2.50 Si'
_cod_database_code               1568733
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.957
_shelx_estimated_absorpt_t_max   0.965
_shelx_res_checksum              25443