Synthesis, structures and catalytic activity of some BINOL based boronates and boronium salts.
Garg, Shipra; Unruh, Daniel K.; Krempner, Clemens; Dalton transactions (Cambridge, England : 2003) 50 (2021) 5044–5049; doi:10.1039/d1dt00842k

data_7706955
_publ_section_title
;
 Synthesis, structures and catalytic activity of some BINOL based
 boronates and boronium salts.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5044
_journal_page_last               5049
_journal_paper_doi               10.1039/d1dt00842k
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         '2(C26 H12 B F5 O2)'
_chemical_formula_sum            'C52 H24 B2 F10 O4'
_chemical_formula_weight         924.33
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-15
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2021-02-01 deposited with the CCDC.	2021-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                98.515(2)
_cell_angle_beta                 97.647(2)
_cell_angle_gamma                92.998(2)
_cell_formula_units_Z            2
_cell_length_a                   7.5800(2)
_cell_length_b                   15.1022(4)
_cell_length_c                   19.1160(4)
_cell_measurement_reflns_used    13270
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.724
_cell_measurement_theta_min      2.348
_cell_volume                     2139.13(9)
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      99.95
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37333
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         77.188
_diffrn_reflns_theta_min         2.361
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.026
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       needle
_exptl_crystal_F_000             936
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Diethyl ether'
_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.039
_exptl_crystal_size_min          0.014
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.0014(3)
_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   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         8671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0508
_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^)+(0.1003P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1461
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6932
_reflns_number_total             8671
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00842k2.cif
_cod_data_source_block           RS-2
_cod_depositor_comments
'Adding full bibliography for 7706949--7706955.cif.'
_cod_database_code               7706955
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.832
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C15(H15), C16(H16), C20(H20),
 C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C36(H36), C37(H37), C38(H38),
  C39(H39), C41(H41), C42(H42), C46(H46), C47(H47), C48(H48), C49(H49),
 C51(H51), C52(H52)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              26645
_shelx_hkl_checksum              58455
_shelx_fab_checksum              94564
_olex2_exptl_crystal_mounting_method 'MiTeGen 50 micron MicroLoop'
_olex2_submission_original_sample_id kre19_42
_olex2_submission_special_instructions 'No special instructions were received'