Rapid, iterative syntheses of unsymmetrical di- and triarylboranes from crystalline aryldifluoroboranes.
Turnbull, Douglas; Légaré, Marc-André; Chemical science 14 (2023) 14256–14261; doi:10.1039/d3sc05071h

data_1570346
_publ_section_title
;
 Rapid, iterative syntheses of unsymmetrical di- and triarylboranes from
 crystalline aryldifluoroboranes.
;
_journal_issue                   48
_journal_name_full               'Chemical science'
_journal_page_first              14256
_journal_page_last               14261
_journal_paper_doi               10.1039/d3sc05071h
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C52 H48 B2 Fe, 0.5[C6H5F]'
_chemical_formula_sum            'C55 H50.5 B2 F0.5 Fe'
_chemical_formula_weight         798.507
_chemical_name_systematic
'1,1'-bis[5-acenaphthyl(mesityl)boryl]ferrocene - fluorobenzene (1:0.5)'
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-03
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.17 svn.r577a77a9 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-09-03 deposited with the CCDC.	2023-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.668(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.0228(11)
_cell_length_b                   7.5570(3)
_cell_length_c                   18.3028(8)
_cell_measurement_reflns_used    2216
_cell_measurement_temperature    298
_cell_measurement_theta_max      70.771
_cell_measurement_theta_min      2.874
_cell_volume                     4252.5(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.9513
_diffrn_measured_fraction_theta_max 0.9103
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_av_unetI/netI     0.0857
_diffrn_reflns_Laue_measured_fraction_full 0.9513
_diffrn_reflns_Laue_measured_fraction_max 0.9103
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24980
_diffrn_reflns_point_group_measured_fraction_full 0.9513
_diffrn_reflns_point_group_measured_fraction_max 0.9103
_diffrn_reflns_theta_full        67.6786
_diffrn_reflns_theta_max         75.33
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    3.133
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.1720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1571 before and 0.0405 after correction.
The Ratio of minimum to maximum transmission is 0.2282.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'translucent red'
_exptl_crystal_colour_lustre     translucent
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       plate
_exptl_crystal_F_000             1684.665
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.5676
_refine_diff_density_min         -0.6905
_refine_diff_density_rms         0.0912
_refine_ls_d_res_high            0.7969
_refine_ls_d_res_low             15.3727
_refine_ls_extinction_coef       0.00143(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   0.9696
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    80
_refine_ls_number_parameters     503
_refine_ls_number_reflns         8026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9696
_refine_ls_R_factor_all          0.1351
_refine_ls_R_factor_gt           0.0619
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0916P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1979
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              37
_reflns_limit_h_min              -38
_reflns_limit_k_max              9
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                3677
_reflns_number_total             8026
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3sc05071h2.cif
_cod_data_source_block           6_FcBAM2
_cod_depositor_comments
'Adding full bibliography for 1570333--1570346.cif.'
_cod_original_formula_sum        'C55 H50.5 B2 F0.5 Fe1'
_cod_database_code               1570346
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C11(H11a,H11b), C12(H12a,H12b), C37(H37a,H37b), C38(H38a,H38b)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), C9(H9), C15(H15), C17(H17), C23(H23),
 C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C33(H33), C34(H34), C35(H35),
  C41(H41), C43(H43), C49(H49), C50(H50), C51(H51), C52(H52)
2.c Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C21(H21a,H21b,H21c), C45(H45a,H45b,
 H45c), C46(H46a,H46b,H46c), C47(H47a,H47b,H47c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'