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_1568731
_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 H61 B2, C16 H32 Li O4'
_chemical_formula_sum            'C62 H93 B2 Li O4'
_chemical_formula_weight         930.92
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_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                 91.836(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9232(8)
_cell_length_b                   19.4217(13)
_cell_length_c                   25.512(2)
_cell_measurement_reflns_used    4793
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.6640
_cell_measurement_theta_min      3.7290
_cell_volume                     5904.8(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'image plate'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0970
_diffrn_reflns_av_unetI/netI     0.2732
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            23899
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.419
_diffrn_reflns_theta_min         3.641
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.047
_exptl_crystal_description       block
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.240
_refine_diff_density_max         0.172
_refine_diff_density_min         -0.163
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
 Flack x determined using 2623 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.3(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.749
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1300
_refine_ls_number_reflns         23899
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      0.749
_refine_ls_R_factor_all          0.1579
_refine_ls_R_factor_gt           0.0616
_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^)+(0.0473P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1214
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                9092
_reflns_number_total             23899
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.5760\% 
around [1.00 0.00 -0.06] (reciprocal) or [1.00 -0.00 0.00] (direct)
;
_cod_data_source_file            d3sc01395b3.cif
_cod_data_source_block           wa2777_revised_by_AVirovets
_cod_depositor_comments
'Adding full bibliography for 1568727--1568737.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1568731
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.982
_shelx_estimated_absorpt_t_max   0.985
_oxdiff_twin_items               2
_oxdiff_twin_integration_method  simultaneous
_shelx_res_checksum              6953