Distiboranes based on <i>ortho</i>-phenylene backbones as bidentate Lewis acids for fluoride anion chelation.
You, Di; Zhou, Benyu; Hirai, Masato; Gabbaï, François P; Organic & biomolecular chemistry 19 (2021) 4949–4957; doi:10.1039/d1ob00536g

data_7158048
_publ_section_title
;
 Distiboranes based on <i>ortho</i>-phenylene backbones as bidentate Lewis
 acids for fluoride anion chelation.
;
_journal_issue                   22
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              4949
_journal_page_last               4957
_journal_paper_doi               10.1039/d1ob00536g
_journal_volume                  19
_journal_year                    2021
_chemical_formula_moiety         'C57.951 H24 F16.972 O4 Sb2, C16 H35 N'
_chemical_formula_sum            'C73.95 H59 F16.97 N O4 Sb2'
_chemical_formula_weight         1591.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-03-17 deposited with the CCDC.	2021-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.702(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   43.782(13)
_cell_length_b                   12.384(3)
_cell_length_c                   24.941(7)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.97
_cell_measurement_theta_min      2.16
_cell_volume                     13431(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      110.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            64060
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.394
_diffrn_reflns_theta_min         1.644
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       block
_exptl_crystal_F_000             6371
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.126
_refine_diff_density_max         1.130
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1421
_refine_ls_number_reflns         13691
_refine_ls_number_restraints     4910
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0516P)^2^+60.7717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1228
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9975
_reflns_number_total             13691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ob00536g2.cif
_cod_data_source_block           i_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7158045--7158050.cif.'
_cod_database_code               7158048
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.895
_shelx_estimated_absorpt_t_min   0.852
_olex2_refinement_description
;
1. Shared sites
{C49B, C55D}
{C58A, C58D}
2. Others
 Fixed Uiso: H3(0.052) H4(0.066) H5(0.073) H6(0.055) H8(0.061) H9(0.079)
 H10(0.086) H11(0.08) H12(0.059) H14(0.076) H15(0.096) H16(0.105) H17(0.093)
 H18(0.07) H34(0.047) H35(0.065) H36(0.073) H37(0.075) H38(0.051) H40(0.056)
 H41(0.078) H42(0.081) H43(0.077) H44(0.059) H59A(0.103) H59B(0.103)
 H60A(0.125) H60B(0.125) H61(0.138) H62A(0.257) H62B(0.257) H62C(0.257)
 H63A(0.077) H63B(0.077) H64A(0.123) H64B(0.123) H65A(0.128) H65B(0.128)
 H66A(0.192) H66B(0.192) H66C(0.192) H67A(0.103) H67B(0.103) H68A(0.156)
 H68B(0.156) H69A(0.15) H69B(0.15) H70A(0.167) H70B(0.167) H70C(0.167)
 H71C(0.076) H71D(0.076) H71A(0.076) H71B(0.076) H72A(0.088) H72B(0.088)
 H72C(0.088) H72D(0.088) H73C(0.093) H73D(0.093) H73A(0.096) H73B(0.096)
 H74D(0.171) H74E(0.171) H74F(0.171) H74A(0.233) H74B(0.233) H74C(0.233)
 Fixed X: H3(0.174291) H4(0.213282) H5(0.231665) H6(0.211822) H8(0.151982)
 H9(0.176379) H10(0.225988) H11(0.250238) H12(0.225008) H14(0.166853)
 H15(0.204996) H16(0.252768) H17(0.263475) H18(0.227374) H34(0.178837)
 H35(0.177261) H36(0.133387) H37(0.09189) H38(0.092792) H40(0.068295)
 H41(0.022871) H42(0.02115) H43(0.064278) H44(0.110769) H59A(-0.131489) H59B(-
 0.098564) H60A(-0.155238) H60B(-0.121909) H61(-0.124784) H62A(-0.147051) H62B(-
 0.155121) H62C(-0.175644) H63A(-0.146863) H63B(-0.156879) H64A(-0.171222)
 H64B(-0.168222) H65A(-0.206094) H65B(-0.220401) H66A(-0.236737) H66B(-
 0.201848) H66C(-0.215005) H67A(-0.10925) H67B(-0.096154) H68A(-0.06766) H68B(-
 0.055031) H69A(-0.058236) H69B(-0.027131) H70A(-0.033607) H70B(-0.059578)
 H70C(-0.024721) H71C(-0.08861) H71D(-0.123551) H71A(-0.10701) H71B(-0.077811)
 H72A(-0.069707) H72B(-0.105382) H72C(-0.100975) H72D(-0.135051) H73C(-
 0.109459) H73D(-0.109068) H73A(-0.069975) H73B(-0.101563) H74D(-0.059781)
 H74E(-0.057425) H74F(-0.05938) H74A(-0.075899) H74B(-0.059122) H74C(-0.044413)
 Fixed Y: H3(0.992126) H4(1.087589) H5(1.025761) H6(0.870671) H8(0.799787)
 H9(0.819531) H10(0.755154) H11(0.663701) H12(0.631617) H14(0.440906)
 H15(0.311111) H16(0.366147) H17(0.544881) H18(0.674657) H34(0.840497)
 H35(0.938992) H36(1.035394) H37(1.038545) H38(0.94227) H40(0.710292)
 H41(0.773733) H42(0.9454) H43(1.052891) H44(0.98755) H59A(0.623219)
 H59B(0.677512) H60A(0.784371) H60B(0.838786) H61(0.783943) H62A(0.96887)
 H62B(0.929787) H62C(0.890062) H63A(0.606992) H63B(0.700557) H64A(0.555151)
 H64B(0.475386) H65A(0.606568) H65B(0.521022) H66A(0.691039) H66B(0.731261)
 H66C(0.64601) H67A(0.768054) H67B(0.665354) H68A(0.760271) H68B(0.652709)
 H69A(0.857168) H69B(0.811498) H70A(0.772989) H70B(0.688402) H70C(0.670726)
 H71C(0.497318) H71D(0.472177) H71A(0.478956) H71B(0.557125) H72A(0.509299)
 H72B(0.481122) H72C(0.469995) H72D(0.43585) H73C(0.289473) H73D(0.26881)
 H73A(0.351453) H73B(0.3169) H74D(0.374292) H74E(0.254069) H74F(0.354499)
 H74A(0.304025) H74B(0.227319) H74C(0.341789)
 Fixed Z: H3(0.322918) H4(0.374544) H5(0.460823) H6(0.494347) H8(0.576419)
 H9(0.664926) H10(0.686569) H11(0.623896) H12(0.537132) H14(0.453268)
 H15(0.437849) H16(0.419013) H17(0.411177) H18(0.426258) H34(0.235503)
 H35(0.155035) H36(0.123113) H37(0.171242) H38(0.252151) H40(0.328777)
 H41(0.357327) H42(0.393377) H43(0.404821) H44(0.37869) H59A(0.467317)
 H59B(0.466015) H60A(0.429726) H60B(0.431266) H61(0.539233) H62A(0.491376)
 H62B(0.549242) H62C(0.495561) H63A(0.321685) H63B(0.359952) H64A(0.419704)
 H64B(0.369976) H65A(0.31629) H65B(0.354986) H66A(0.372661) H66B(0.384103)
 H66C(0.423823) H67A(0.352434) H67B(0.323781) H68A(0.422649) H68B(0.39719)
 H69A(0.341728) H69B(0.374295) H70A(0.276711) H70B(0.288799) H70C(0.314571)
 H71C(0.41345) H71D(0.421157) H71A(0.426682) H71B(0.426681) H72A(0.34084)
 H72B(0.323536) H72C(0.31804) H72D(0.328694) H73C(0.389929) H73D(0.326236)
 H73A(0.405008) H73B(0.370059) H74D(0.336428) H74E(0.36008) H74F(0.399914)
 H74A(0.291613) H74B(0.337606) H74C(0.32549)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              46714
_shelx_fab_checksum              78224
_olex2_submission_special_instructions 'No special instructions were received'