Directed <i>cis</i>-hydrosilylation of borylalkynes to borylsilylalkenes.
Stefanowska, Kinga; Sokolnicki, Tomasz; Walkowiak, Jędrzej; Czapik, Agnieszka; Franczyk, Adrian; Chemical communications (Cambridge, England) 58 (2022) 12046–12049; doi:10.1039/d2cc04318a

data_7130861
_publ_section_title
;
 Directed <i>cis</i>-hydrosilylation of borylalkynes to borylsilylalkenes.
;
_journal_issue                   86
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12046
_journal_page_last               12049
_journal_paper_doi               10.1039/d2cc04318a
_journal_volume                  58
_journal_year                    2022
_chemical_formula_moiety         'C32 H40 B2 O4 Si'
_chemical_formula_sum            'C32 H40 B2 O4 Si'
_chemical_formula_weight         538.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-05-13 deposited with the CCDC.	2022-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.3870(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.11404(9)
_cell_length_b                   16.90606(14)
_cell_length_c                   18.29331(16)
_cell_measurement_reflns_used    14066
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      76.2800
_cell_measurement_theta_min      2.4550
_cell_volume                     3055.13(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.94a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.94a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.94a (Rigaku OD, 2021)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17756
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.382
_diffrn_reflns_theta_min         4.950
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.939
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80277
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.94a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.280
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.164
_refine_diff_density_rms         0.030
_refine_ls_abs_structure_details
;
 Flack x determined using 2593 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         5832
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0521P)^2^+0.5346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0762
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_full    0.872
_reflns_Friedel_fraction_max     0.824
_reflns_number_gt                5799
_reflns_number_total             5832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04318a2.cif
_cod_data_source_block           DATA
_cod_depositor_comments
'Adding full bibliography for 7130861--7130865.cif.'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7130861
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.705
_shelx_estimated_absorpt_t_max   0.779
_shelx_res_checksum              2326
_shelx_hkl_checksum              95757