Synthesis and crystal structures of boryl <i>ortho</i>-silylaryl tri-fluoro-methane-sulfonates.
Barnå, Fredrik; Hribersek, Matic; Orthaber, Andreas; Pilarski, Lukasz T.; Acta crystallographica. Section E, Crystallographic communications 80 (2024) 143–147; doi:10.1107/S2056989024000264

data_2023007
_publ_section_title
;
 Synthesis and crystal structures of boryl <i>ortho</i>-silylaryl
 tri-fluoro-methane-sulfonates.
;
_journal_coeditor_code           DJ2074
_journal_issue                   'Pt 2'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              143
_journal_page_last               147
_journal_paper_doi               10.1107/S2056989024000264
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          'C16 H24 B F3 O5 S Si'
_chemical_formula_moiety         'C16 H24 B F3 O5 S Si'
_chemical_formula_sum            'C16 H24 B F3 O5 S Si'
_chemical_formula_weight         424.31
_chemical_name_systematic
;
5-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)-2-(trimethylsilyl)phenyl
trifluoromethanesulfonate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4316(7)
_cell_length_b                   25.1732(17)
_cell_length_c                   7.7756(5)
_cell_measurement_reflns_used    3068
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.566
_cell_measurement_theta_min      2.536
_cell_volume                     2041.8(2)
_computing_cell_refinement
;
SAINT v8.34A (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT v8.34A (Bruker, 2013)
;
_computing_molecular_graphics
;
Olex2 1.5 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
Olex2 1.5 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/4</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            13726
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.749
_diffrn_reflns_theta_min         1.618
_exptl_absorpt_coefficient_mu    0.267
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.249
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1809 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.11(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         5205
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0416P)^2^+0.1163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0912
_reflns_number_gt                4654
_reflns_number_total             5205
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            dj2074sup1.cif
_cod_data_source_block           1_a
_cod_depositor_comments
'Adding full bibliography for 2023007--2023009.cif.'
_cod_database_code               2023007
_cod_database_fobs_code          2023007
_shelx_estimated_absorpt_t_min   0.924
_shelx_estimated_absorpt_t_max   0.953
_shelx_hkl_checksum              34553
_shelx_res_checksum              47402