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_7706952
_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         'C52 H24 B2 F10 O4'
_chemical_formula_sum            'C52 H24 B2 F10 O4'
_chemical_formula_weight         924.33
_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   geom
_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                90
_cell_angle_beta                 108.241(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.525(3)
_cell_length_b                   11.785(2)
_cell_length_c                   23.532(5)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.254
_cell_measurement_theta_min      2.217
_cell_volume                     4089.1(14)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0900
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            15324
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.446
_diffrn_reflns_theta_min         1.381
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0783 before and 0.0520 after correction.
The Ratio of minimum to maximum transmission is 0.7003.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Benzene'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 3861 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1190
_refine_ls_number_reflns         15324
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0598
_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^)+(0.0538P)^2^+0.6137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1221
_reflns_Friedel_coverage         0.876
_reflns_Friedel_fraction_full    0.975
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                11534
_reflns_number_total             15324
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00842k2.cif
_cod_data_source_block           RR-2
_cod_depositor_comments
'Adding full bibliography for 7706949--7706955.cif.'
_cod_database_code               7706952
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.971
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5964(14)
 0.4036(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Rigid body (RIGU) restrains
 C59, C67, C68, C69, C66, C65, C64
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C53, C54, C58, B3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C11(H11), C12(H12), C13(H13), C14(H14), C19(H19), C20(H20),
 C21(H21), C22(H22), C24(H24), C25(H25), C28(H28), C29(H29), C31(H31), C32(H32),
  C33(H33), C34(H34), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44),
 C45(H45), C60(H60), C61(H61), C63(H63), C64(H64), C65(H65), C66(H66), C71(H71),
  C72(H72), C73(H73), C74(H74), C76(H76), C77(H77), C80(H80), C81(H81),
 C83(H83), C84(H84), C85(H85), C86(H86), C91(H91), C92(H92), C93(H93), C94(H94),
  C96(H96), C97(H97)
4.b Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C53(C54,C55,C56,C57,C58), C99(C100,C101,C102,C103,C104)
;
_shelx_res_checksum              56201
_shelx_hkl_checksum              89680
_olex2_exptl_crystal_mounting_method 'MiTeGen 200 micron MicroLoop'
_olex2_submission_special_instructions 'No special instructions were received'